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Sample records for mas nmr spin-lattice

  1. Interaction study of polyisobutylene with paraffins by NMR using the evaluation of spin-lattice relaxation times for hydrogen nuclei

    International Nuclear Information System (INIS)

    Marques, Rosana G.G.; Tavares, Maria I.B.

    2001-01-01

    The evaluation of spin-lattice relaxation times of 1 H for polyisobutylene/paraffin systems, were obtained using the classic inversion recovery technique, and also through Cross Polarization Magic Angle Spinning (CP/MAS) techniques varying the contact time and also by the delayed contact time pulse sequence. NMR results showed that the polyisobutylene/paraffin systems in which high molecular weight paraffins were used, is heterogeneous. However, for paraffins with low molecular weight, the system presents good homogeneity. (author)

  2. Magnetization and 13C NMR spin-lattice relaxation of nanodiamond powder

    Energy Technology Data Exchange (ETDEWEB)

    Levin, E.M.; Fang, X.W.; Bud' ko, S.L.; Straszheim, W.E.; McCallum, R.W.; Schmidt-Rohr, K.

    2008-02-15

    The bulk magnetization at temperatures of 1.8-400 K and in magnetic fields up to 70 kOe, the ambient temperature {sup 13}C NMR spin-lattice relaxation, T{sub 1,c}, and the elemental composition of three nanodiamond powder samples have been studied. The total magnetization of nanodiamond can be explained in terms of contributions from (1) the diamagnetic effect of carbon, (2) the paramagnetic effect of unpaired electrons present in nanodiamond grains, and (3) ferromagnetic-like and (4) superparamagnetic contributions from Fe-containing particles detected in spatially resolved energy-dispersive spectroscopy. Contributions (1) and (2) are intrinsic to nanodiamond, while contributions (3) and (4) arise from impurities naturally present in detonation nanodiamond samples. {sup 13}C NMR T{sub 1,c} relaxation would be unaffected by the presence of the ferromagnetic particles with the bulk magnetization of {approx} 0.01 emu/g at 300 K. Thus, a reduction of T{sub 1,c} by 3 orders of magnitude compared to natural and synthetic microdiamonds confirms the presence of unpaired electrons in the nanodiamond grains. The spin concentration in nanodiamond powder corresponds to {approx}30 unpaired electrons per {approx}4.6 nm diameter nanodiamond grain.

  3. Interaction study of polyisobutylene with paraffins by NMR using the evaluation of spin-lattice relaxation times for hydrogen nuclei; Estudo da interacao do poliisobutileno com parafinas por RMN no estado solido

    Energy Technology Data Exchange (ETDEWEB)

    Marques, Rosana G.G. [PETROBRAS S.A., Rio de Janeiro, RJ (Brazil). Centro de Pesquisas - CENPES]. E-mail: garrido@cenpes.petrobras.com.br; Tavares, Maria I.B. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Macromoleculas]. E-mail: mibt@ima.ufrj.br

    2001-07-01

    The evaluation of spin-lattice relaxation times of {sup 1}H for polyisobutylene/paraffin systems, were obtained using the classic inversion recovery technique, and also through Cross Polarization Magic Angle Spinning (CP/MAS) techniques varying the contact time and also by the delayed contact time pulse sequence. NMR results showed that the polyisobutylene/paraffin systems in which high molecular weight paraffins were used, is heterogeneous. However, for paraffins with low molecular weight, the system presents good homogeneity. (author)

  4. An NMR thermometer for cryogenic magic-angle spinning NMR: The spin-lattice relaxation of 127I in cesium iodide

    Science.gov (United States)

    Sarkar, Riddhiman; Concistrè, Maria; Johannessen, Ole G.; Beckett, Peter; Denning, Mark; Carravetta, Marina; al-Mosawi, Maitham; Beduz, Carlo; Yang, Yifeng; Levitt, Malcolm H.

    2011-10-01

    The accurate temperature measurement of solid samples under magic-angle spinning (MAS) is difficult in the cryogenic regime. It has been demonstrated by Thurber et al. (J. Magn. Reson., 196 (2009) 84-87) [10] that the temperature dependent spin-lattice relaxation time constant of 79Br in KBr powder can be useful for measuring sample temperature under MAS over a wide temperature range (20-296 K). However the value of T1 exceeds 3 min at temperatures below 20 K, which is inconveniently long. In this communication, we show that the spin-lattice relaxation time constant of 127I in CsI powder can be used to accurately measure sample temperature under MAS within a reasonable experimental time down to 10 K.

  5. A study of spin-lattice relaxation rates of glucose, fructose, sucrose and cherries using high-T c SQUID-based NMR in ultralow magnetic fields

    Science.gov (United States)

    Liao, Shu-Hsien; Wu, Pei-Che

    2017-08-01

    We study the concentration dependence of spin-lattice relaxation rates, T 1 -1, of glucose, fructose, sucrose and cherries by using high-T c SQUID-based NMR at magnetic fields of ˜97 μT. The detected NMR signal, Sy (T Bp), is fitted to [1 - exp(-T Bp/T 1)] to derive T 1 -1, where Sy (T Bp) is the strength of the NMR signal, T Bp is the duration of pre-polarization and T 1 -1 is the spin-lattice relaxation rate. It was found that T 1 -1 increases as the sugar concentrations increase. The increased T 1 -1 is due to the presence of more molecules in the surroundings, which increases the spin-lattice interaction and in turn enhances T 1 -1. The T 1 -1 versus degrees Brix curve provides a basis for determining unknown Brix values for cherries as well as other fruits.

  6. 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.

  7. NMR water-proton spin-lattice relaxation time of human red blood cells and red blood cell suspensions

    International Nuclear Information System (INIS)

    Sullivan, S.G.; Rosenthal, J.S.; Winston, A.; Stern, A.

    1988-01-01

    NMR water-proton spin-lattice relaxation times were studied as probes of water structure in human red blood cells and red blood cell suspensions. Normal saline had a relaxation time of about 3000 ms while packed red blood cells had a relaxation time of about 500 ms. The relaxation time of a red blood cell suspension at 50% hematocrit was about 750 ms showing that surface charges and polar groups of the red cell membrane effectively structure extracellular water. Incubation of red cells in hypotonic saline increases relaxation time whereas hypertonic saline decreases relaxation time. Relaxation times varied independently of mean corpuscular volume and mean corpuscular hemoglobin concentration in a sample population. Studies with lysates and resealed membrane ghosts show that hemoglobin is very effective in lowering water-proton relaxation time whereas resealed membrane ghosts in the absence of hemoglobin are less effective than intact red cells. 9 refs.; 3 figs.; 1 table

  8. Quartz Crystal Temperature Sensor for MAS NMR

    Science.gov (United States)

    Simon, Gerald

    1997-10-01

    Quartz crystal temperature sensors (QCTS) were tested for the first time as wireless thermometers in NMR MAS rotors utilizing the NMR RF technique itself for exiting and receiving electro-mechanical quartz resonances. This new tool in MAS NMR has a high sensitivity, linearity, and precision. When compared to the frequently used calibration of the variable temperature in the NMR system by a solid state NMR chemical shift thermometer (CST), such as lead nitrate, QCTS shows a number of advantages. It is an inert thermometer in close contact with solid samples operating parallel to the NMR experiment. QCTS can be manufactured for any frequency to be near a NMR frequency of interest (typically 1 to 2 MHz below or above). Due to the strong response of the crystal, signal detection is possible without changing the tuning of the MAS probe. The NMR signal is not influenced due to the relative sharp crystal resonance, restricted excitation by finite pulses, high probeQvalues, and commonly used audio filters. The quadratic dependence of the temperature increase on spinning speed is the same for the QCTS and for the CST lead nitrate and is discussed in terms of frictional heat in accordance with the literature about lead nitrate and with the results of a simple rotor speed jump experiment with differently radial located lead nitrate in the rotor.

  9. Enhanced 29Si spin-lattice relaxation and observation of three-dimensional lattice connectivity in zeolites by two-dimensional 29Si MASS NMR

    International Nuclear Information System (INIS)

    Sivadinarayana, C.; Choudhary, V.R.; Ganapathy, S.

    1994-01-01

    It is shown that considerable sensitivity enhancement is achieved in the 29 Si magic angle sample spinning (MASS) NMR spectra of highly siliceous zeolites by pre treating the material with oxygen. The presence of adsorbed molecular oxygen in zeolite channels promotes an efficient 29 Si spin-lattice relaxation via a paramagnetic interaction between the lattice 29 Si T-site and the adsorbed oxygen on zeolite channels. This affords an efficient 2-D data collection and leads to increased sensitivity. The utility of this method is demonstrated in a two-dimensional COSY-45 NMR experiment of a high silica zeolite ZSM-5. (author). 20 refs., 3 figs., 1 tab

  10. Nuclear spin-lattice relaxation in carbon nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Panich, A.M., E-mail: pan@bgu.ac.i [Department of Physics, Ben-Gurion University of the Negev, P.O. Box 653, Beer Sheva 84105 (Israel); Sergeev, N.A. [Institute of Physics, University of Szczecin, 70-451 Szczecin (Poland)

    2010-04-15

    Interpretation of nuclear spin-lattice relaxation data in the carbon nanostructures is usually based on the analysis of fluctuations of dipole-dipole interactions of nuclear spins and anisotropic electron-nuclear interactions responsible for chemical shielding, which are caused by molecular dynamics. However, many nanocarbon systems such as fullerene and nanotube derivatives, nanodiamonds and carbon onions reveal noticeable amount of paramagnetic defects with unpaired electrons originating from dangling bonds. The interaction between nuclear and electron spins strongly influences the nuclear spin-lattice relaxation, but usually is not taken into account, thus the relaxation data are not correctly interpreted. Here we report on the temperature dependent NMR spectra and spin-lattice relaxation measurements of intercalated fullerenes C{sub 60}(MF{sub 6}){sub 2} (M=As and Sb), where nuclear relaxation is caused by both molecular rotation and interaction between nuclei and unpaired electron spins. We present a detailed theoretical analysis of the spin-lattice relaxation data taking into account both these contributions. Good agreement between the experimental data and calculations is obtained. The developed approach would be useful in interpreting the NMR relaxation data in different nanostructures and their intercalation compounds.

  11. $^{11}$B and $^{27}$Al NMR spin-lattice relaxation and Knight shift study of Mg$_{1-x}$Al$_x$B$_2$. Evidence for anisotropic Fermi surface

    OpenAIRE

    Papavassiliou, G.; Pissas, M.; Karayanni, M.; Fardis, M.; Koutandos, S.; Prassides, K.

    2002-01-01

    We report a detailed study of $^{11}$B and $^{27}$Al NMR spin-lattice relaxation rates ($1/T_1$), as well as of $^{27}$Al Knight shift (K) of Mg$_{1-x}$Al$_x$B$_2$, $0\\leq x\\leq 1$. The obtained ($1/T_1T$) and K vs. x plots are in excellent agreement with ab initio calculations. This asserts experimentally the prediction that the Fermi surface is highly anisotropic, consisting mainly of hole-type 2-D cylindrical sheets from bonding $2p_{x,y}$ boron orbitals. It is also shown that the density ...

  12. Phase separation, clustering, and fractal characteristics in glass: A magic-angle-spinning NMR spin-lattice relaxation study

    Science.gov (United States)

    Sen, S.; Stebbins, J. F.

    1994-07-01

    A comparative study of the 29Si spin-lattice relaxation behavior (induced by trace amounts of paramagnetic dopants in the glass) in phase-separated Li2Si4O9 and monophasic Li2Si2O5 and Na2Si2O5 glasses has been made in order to understand the nature of clustering and the resulting intermediate-range ordering. Optically clear tetrasilicate and disilicate glasses were prepared with 500 to 2000 ppm of Gd2O3, a paramagnetic dopant. The constituent structural units (Q3 and Q4 species) in all tetrasilicate glasses show strong differential relaxation following a power-law behavior. This is due to preferential partitioning of Gd3+ into the lower silica (Q3-rich) regions of these glasses, indicating the presence of Q species clusters too small to produce optical opalescence (a few nm to perhaps tens of nm). Preliminary results on 6Li spin-lattice relaxation in these glasses support this hypothesis. Differential relaxation becomes more pronounced on annealing due to growth of such clusters. No such differential relaxation was observed in the monophase disilicate glasses. For spin-lattice relaxation induced by direct dipolar coupling to paramagnetic ions, the recovery of magnetization is proportional to time as M(t)~tα where α is a function of the dimensionality D of mass distribution of the constituent Q species around the Gd3+ paramagnetic centers in the glass. For tetrasilicate glasses D~=2.62+/-0.22 and the system behaves as a mass fractal up to a length scale of 2 to 3 nm. D is thus equal to, within error, the theoretical value of 2.6 for an infinite percolation cluster of one type of Q species in another. For disilicate glasses, D~=3.06+/-0.18 which indicates a three-dimensional (and thus nonfractal) mass distribution of the constituent Q species over the same length scale.

  13. Novel spin dynamics in ferrimagnetic molecular chains from 1H NMR and μSR spin-lattice relaxation measurements

    International Nuclear Information System (INIS)

    Micotti, E.; Lascialfari, A.; Rigamonti, A.; Aldrovandi, S.; Caneschi, A.; Gatteschi, D.; Bogani, L.

    2004-01-01

    The spin dynamics in the helical chain Co(hfac) 2 NITPhOMe has been investigated by 1 H NMR and μSR relaxation. In the temperature range 15< T<60 K, the results are consistent with the relaxation of the homogeneous magnetization. For T≤15 K, NMR and μSR evidence a second spin relaxation mechanism, undetected by the magnetization measurements. From the analysis of these data, insights on this novel relaxation process are derived

  14. Novel spin dynamics in ferrimagnetic molecular chains from 1H NMR and μSR spin-lattice relaxation measurements

    Science.gov (United States)

    Micotti, E.; Lascialfari, A.; Rigamonti, A.; Aldrovandi, S.; Caneschi, A.; Gatteschi, D.; Bogani, L.

    2004-05-01

    The spin dynamics in the helical chain Co(hfac) 2NITPhOMe has been investigated by 1H NMR and μSR relaxation. In the temperature range 15NMR and μSR evidence a second spin relaxation mechanism, undetected by the magnetization measurements. From the analysis of these data, insights on this novel relaxation process are derived.

  15. 31P Solid-state MAS NMR spectra

    International Nuclear Information System (INIS)

    Grobet, P.J.; Geerts, H.; Martens, J.A.; Jacobs, P.A.

    1989-01-01

    The structures of the silicoaluminiophosphates MCM-1 and MCM9 were characterized by 27 Al and 31 P MAS NMR. The structural identity of MCM-1 and its silicon-free homologue AlPO 4 -H 3 is demonstrated. The presence of a structural mixture in MCM-9 is confirmed. 31 P MAS NMR spectra of MCM-9 could be interpreted as a superposition of spectra of VPI-5, AlPO 4 -H 3 and SAPO-11 phases. (author). 12 refs.; 3 figs.; 1 tab

  16. Anomalous H/D isotope effect on 35Cl NQR frequencies and H/D isotope effect on 1H MAS NMR spectra in pyrrolidinium p-chlorobenzoate

    International Nuclear Information System (INIS)

    Nakano, Ryo; Honda, Hisashi; Nakata, Eiichi; Takamizawa, Satoshi; Noro, Sumiko; Kimura, Taiki; Kyo, Shin-shin; Ishimaru, Shin'ichi; Miyake, Ryosuke

    2010-01-01

    An anomalous isotope effect was observed in the 35 Cl NQR frequency of pyrrolidinium p-chlorobenzoate (C 4 H 8 NH 2 + ·ClC 6 H 4 COO - ) by deuterium substitution of hydrogen atoms which form two kinds of N-H...O type hydrogen bonds. Large negative frequency shifts of the 35 Cl resonance lines, reaching 309 kHz at 77 K and 267 kHz at 293 K, were obtained upon deuteration, although the Cl atom in the molecule formed no hydrogen bonds in the crystal. 1 H MAS NMR lines showed significant changes by the deuterium substitution, while in contrast, small shifts of 13 C CP/MAS NMR signals were obtained. Our measurements of 1 H NMR spin-lattice relaxation times (T 1 ) suggested that the H/D isotope shifts detected from the 35 Cl NQR frequencies and 1 H NMR spectra are due to structural changes rather than molecular dynamics. Single-crystal X-ray diffraction measurements showed two remarkable H/D isotope differences in the molecular arrangements, (1) the N-H length along the crystallographic a axis became 1 pm shorter, and (2) the dihedral angle between benzene and the pyrrolidine ring changed by 1.1(2)deg upon deuteration. Using density functional theory estimations, the anomalous 35 Cl NQR frequency shifts and 1 H MAS NMR line-shape changes could be explained by the dihedral angle change rather than the N-H length difference. (author)

  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. A General Protocol for Temperature Calibration of MAS NMR Probes at Arbitrary Spinning Speeds

    Science.gov (United States)

    Guan, Xudong; Stark, Ruth E.

    2010-01-01

    A protocol using 207Pb NMR of solid lead nitrate was developed to determine the temperature of magic-angle spinning (MAS) NMR probes over a range of nominal set temperatures and spinning speeds. Using BioMAS and fastMAS probes with typical sample spinning rates of 8 and 35 kHz, respectively, empirical equations were devised to predict the respective sample temperatures. These procedures provide a straightforward recipe for temperature calibration of any MAS probe. PMID:21036557

  19. 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

  20. Novel spin dynamics in ferrimagnetic molecular chains from {sup 1}H NMR and {mu}SR spin-lattice relaxation measurements

    Energy Technology Data Exchange (ETDEWEB)

    Micotti, E. E-mail: micotti@fisicavolta.unipv.it; Lascialfari, A.; Rigamonti, A.; Aldrovandi, S.; Caneschi, A.; Gatteschi, D.; Bogani, L

    2004-05-01

    The spin dynamics in the helical chain Co(hfac){sub 2}NITPhOMe has been investigated by {sup 1}H NMR and {mu}SR relaxation. In the temperature range 15NMR and {mu}SR evidence a second spin relaxation mechanism, undetected by the magnetization measurements. From the analysis of these data, insights on this novel relaxation process are derived.

  1. Multinuclear MAS NMR studies on coked zeolites H-ZSM-5

    International Nuclear Information System (INIS)

    Ernst, H.; Freude, D.; Hunger, M.; Pfeifer, H.

    1991-01-01

    During the cracking process carbonaceous materials are deposited on the outer or inner surface of the catalyst. These deposits are in many cases the main cause of catalyst deactivation. Magic angle spinning (MAS) NMR investigations and catalytic n-hexane cracking were carried out on H-ZSM-5 zeolites after a mild hydrothermal de-alumination. By 13 C CP MAS NMR it could be shown that the enhanced catalytic activity does not enhance the coke formation and that the chemical nature of these deposits is essentially aromatic. From 1 H MAS NMR studies performed on shallow-bed activated sealed samples and 27 Al and 29 Si MAS NMR on rehydrated samples it follows that for high coke concentrations the catalyst deactivation is caused mainly by blocking of Broensted acid sites. (author). 27 refs.; 3 figs.; 2 tabs

  2. A software framework for analysing solid-state MAS NMR data

    International Nuclear Information System (INIS)

    Stevens, Tim J.; Fogh, Rasmus H.; Boucher, Wayne; Higman, Victoria A.; Eisenmenger, Frank; Bardiaux, Benjamin; Rossum, Barth-Jan van; Oschkinat, Hartmut; Laue, Ernest D.

    2011-01-01

    Solid-state magic-angle-spinning (MAS) NMR of proteins has undergone many rapid methodological developments in recent years, enabling detailed studies of protein structure, function and dynamics. Software development, however, has not kept pace with these advances and data analysis is mostly performed using tools developed for solution NMR which do not directly address solid-state specific issues. Here we present additions to the CcpNmr Analysis software package which enable easier identification of spinning side bands, straightforward analysis of double quantum spectra, automatic consideration of non-uniform labelling schemes, as well as extension of other existing features to the needs of solid-state MAS data. To underpin this, we have updated and extended the CCPN data model and experiment descriptions to include transfer types and nomenclature appropriate for solid-state NMR experiments, as well as a set of experiment prototypes covering the experiments commonly employed by solid-sate MAS protein NMR spectroscopists. This work not only improves solid-state MAS NMR data analysis but provides a platform for anyone who uses the CCPN data model for programming, data transfer, or data archival involving solid-state MAS NMR data.

  3. Advances in 27Al MAS NMR studies of geopolymers

    Czech Academy of Sciences Publication Activity Database

    Brus, Jiří; Abbrent, Sabina; Kobera, Libor; Urbanová, Martina; Cuba, P.

    2016-01-01

    Roč. 88, č. 2016 (2016), s. 79-147 ISSN 0066-4103 R&D Projects: GA ČR(CZ) GA13-24155S; GA MŠk(CZ) LO1507 Institutional support: RVO:61389013 Keywords : geopolymers * aluminosilicates * solid-state NMR Subject RIV: CD - Macromolecular Chemistry Impact factor: 2.600, year: 2016

  4. Measuring proton shift tensors with ultrafast MAS NMR.

    Science.gov (United States)

    Miah, Habeeba K; Bennett, David A; Iuga, Dinu; Titman, Jeremy J

    2013-10-01

    A new proton anisotropic-isotropic shift correlation experiment is described which operates with ultrafast MAS, resulting in good resolution of isotropic proton shifts in the detection dimension. The new experiment makes use of a recoupling sequence designed using symmetry principles which reintroduces the proton chemical shift anisotropy in the indirect dimension. The experiment has been used to measure the proton shift tensor parameters for the OH hydrogen-bonded protons in tyrosine·HCl and citric acid at Larmor frequencies of up to 850 MHz. Copyright © 2013 Elsevier Inc. All rights reserved.

  5. Measurement of sample temperatures under magic-angle spinning from the chemical shift and spin-lattice relaxation rate of 79Br in KBr powder.

    Science.gov (United States)

    Thurber, Kent R; Tycko, Robert

    2009-01-01

    Accurate determination of sample temperatures in solid state nuclear magnetic resonance (NMR) with magic-angle spinning (MAS) can be problematic, particularly because frictional heating and heating by radio-frequency irradiation can make the internal sample temperature significantly different from the temperature outside the MAS rotor. This paper demonstrates the use of (79)Br chemical shifts and spin-lattice relaxation rates in KBr powder as temperature-dependent parameters for the determination of internal sample temperatures. Advantages of this method include high signal-to-noise, proximity of the (79)Br NMR frequency to that of (13)C, applicability from 20 K to 320 K or higher, and simultaneity with adjustment of the MAS axis direction. We show that spin-lattice relaxation in KBr is driven by a quadrupolar mechanism. We demonstrate a simple approach to including KBr powder in hydrated samples, such as biological membrane samples, hydrated amyloid fibrils, and hydrated microcrystalline proteins, that allows direct assessment of the effects of frictional and radio-frequency heating under experimentally relevant conditions.

  6. Radiofrequency fields in MAS solid state NMR probes

    Science.gov (United States)

    Tošner, Zdeněk; Purea, Armin; Struppe, Jochem O.; Wegner, Sebastian; Engelke, Frank; Glaser, Steffen J.; Reif, Bernd

    2017-11-01

    We present a detailed analysis of the radiofrequency (RF) field over full volume of a rotor that is generated in a solenoid coil. On top of the usually considered static distribution of amplitudes along the coil axis we describe dynamic radial RF inhomogeneities induced by sample rotation. During magic angle spinning (MAS), the mechanical rotation of the sample about the magic angle, a spin packet travels through areas of different RF fields and experiences periodical modulations of both the RF amplitude and the phase. These modulations become particularly severe at the end regions of the coil where the relative RF amplitude varies up to ±25% and the RF phase changes within ±30°. Using extensive numerical simulations we demonstrate effects of RF inhomogeneity on pulse calibration and for the ramped CP experiment performed at a wide range of MAS rates. In addition, we review various methods to map RF fields using a B0 gradient along the sample (rotor axis) for imaging purposes. Under such a gradient, a nutation experiment provides directly the RF amplitude distribution, a cross polarization experiment images the correlation of the RF fields on the two channels according to the Hartmann-Hahn matching condition, while a spin-lock experiment allows to calibrate the RF amplitude employing the rotary resonance recoupling condition. Knowledge of the RF field distribution in a coil provides key to understand its effects on performance of a pulse sequence at the spectrometer and enables to set robustness requirements in the experimental design.

  7. Solid state CP/MAS 13C n.m.r. analysis of particle size and density fractions of soil incubated with uniformly labelled 13C-glucose

    International Nuclear Information System (INIS)

    Baldock, J.A.; Oades, J.M.

    1990-01-01

    A soil incubated for 34 days in the absence (control) and presence (treated) of uniformly labelled 13 C-glucose was dispersed using an ultrasonic probe and fractionated by sedimentation in water and a polytungstate solution of density 2.0 Mg m -3 . Solid state CP/MAS 13 C n.m.r. (cross polarization/magic angle spinning 13 C nuclear magnetic resonance) spectroscopy was used to characterize the chemical structure of the native soil organic carbon and the residual substrate carbon in the fractions of the control and treated soils. To obtain quantitative results it was essential to determine the spin lattice relaxation time in a rotating frame of the individual carbon types in the spectra as the relaxation behaviour of the native organic material in the clay fraction was different from that of the residual substrate carbon. The residual substrate carbon was found to accumulate in predominantly alkyl and O-alkyl structures in both fractions. However, significant amounts of acetal and carboxyl carbon were also observed in the clay fraction. Little if any aromatic or phenolic carbon was synthesized by the soil microorganisms utilizing substrate carbon. Dipolar dephasing CP/MAS 13 C n.m.r. experiments were also performed and allowed the proportion of each type of carbon which was protonated and nonprotonated to be estimated. Essentially all of the O-alkyl and acetal carbon, 25-40% of the aromatic carbon and 66-80% of the alkyl carbon was protonated in the fractions isolated from the treated soil. 24 refs., 4 figs., 2 tabs

  8. Spin lattices of walking droplets

    Science.gov (United States)

    Saenz, Pedro; Pucci, Giuseppe; Goujon, Alexis; Dunkel, Jorn; Bush, John

    2017-11-01

    We present the results of an experimental investigation of the spontaneous emergence of collective behavior in spin lattice of droplets walking on a vibrating fluid bath. The bottom topography consists of relatively deep circular wells that encourage the walking droplets to follow circular trajectories centered at the lattice sites, in one direction or the other. Wave-mediated interactions between neighboring drops are enabled through a thin fluid layer between the wells. The sense of rotation of the walking droplets may thus become globally coupled. When the coupling is sufficiently strong, interactions with neighboring droplets may result in switches in spin that lead to preferred global arrangements, including correlated (all drops rotating in the same direction) or anti-correlated (neighboring drops rotating in opposite directions) states. Analogies with ferromagnetism and anti-ferromagnetism are drawn. Different spatial arrangements are presented in 1D and 2D lattices to illustrate the effects of topological frustration. This work was supported by the US National Science Foundation through Grants CMMI-1333242 and DMS-1614043.

  9. {sup 1}H HR-MAS NMR and S180 cells: metabolite assignment and evaluation of pulse sequence

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Aline L. de; Martinelli, Bruno César B.; Lião, Luciano M. [Universidade Federal de Goiás (UFG), Goiânia, GO (Brazil). Instituto de Química. Lab. de RMN; Pereira, Flávia C.; Silveira-Lacerda, Elisangela P. [Universidade Federal de Goiás (UFG), Goiânia, GO (Brazil). Instituto de Ciências Biológicas. Laboratório Genética Molecular e Citogenética; Alcantara, Glaucia B., E-mail: glaucia.alcantara@ufms.br [Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil). Inst. de Química

    2014-07-01

    High resolution magic angle spinning {sup 1}H 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. (author)

  10. 1H HR-MAS NMR and S180 cells: metabolite assignment and evaluation of pulse sequence

    International Nuclear Information System (INIS)

    Oliveira, Aline L. de; 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 1 H 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. (author)

  11. 29Si MAS NMR for the zeolite Y - gallium oxide system

    International Nuclear Information System (INIS)

    Sulikowski, B.; Derewinski, M.; Olejniczak, Z.; Segnowski, S.

    1994-01-01

    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 29 Si has been described and discussed

  12. Deuterium and lithium-6 MAS NMR studies of manganese oxide electrode materials

    Science.gov (United States)

    Paik, Younkee

    Electrolytic manganese dioxide (EMD) is used world wide as the cathode materials in both lithium and alkaline primary (non-rechargeable) batteries. We have developed deuterium and lithium MAS NMR techniques to study EMD and related manganese oxides and hydroxides, where diffraction techniques are of limited value due to a highly defective nature of the structures. Deuterons in EMD, manganite, groutite, and deuterium-intercalated pyrolusite and ramsdellite were detected by NMR, for the first time, and their locations and motions in the structures were analyzed by applying variable temperature NMR techniques. Discharge mechanisms of EMD in alkaline (aqueous) electrolytes were studied, in conjunction with step potential electrochemical spectroscopic (SPECS) method, and five distinctive discharge processes were proposed. EMD is usually heat-treated at about 300--400°C to remove water to be used in lithium batteries. Details of the effects of heat-treatment, such as structural and compositional changes as a function of heat-treatment temperature, were studied by a combination of MAS NMR, XRD, and thermogravimetric analysis. Lithium local environments in heat-treated EMD (HEMD) that were discharged in lithium cells, were described in terms of related environments found in model compounds pyrolusite and ramsdellite where specific Li + sites were detected by MAS NMR and the hyperfine shift scale method of Grey et al. Acid-leaching of Li2MnO3 represents an approach for synthesizing new or modified manganese oxide electrode materials for lithium rechargeable batteries. Progressive removal of lithium from specific crystallographic sites, followed by a gradual change of the crystal structure, was monitored by a combination of NMR and XRD techniques.

  13. HR-MAS NMR allied to chemometric on Hancornia speciosa varieties differentiation

    Energy Technology Data Exchange (ETDEWEB)

    Flores, Igor S. [Instituto Federal de Goiás (IFG), Luziânia, GO (Brazil); Silva, Andressa K.; Chaves, Lazaro J.; Collevatti, Rosane G.; Lião, Luciano M., E-mail: lucianoliao@ufg.br [Universidade Federal de Goiás (UFG), Goiânia, GO (Brazil); Furquim, Leonnardo C. [Faculdade Objetivo, GO (Brazil); Castro, Carlos F.S. [Instituto Federal de Educação, Ciência e Tecnologia Goiano (IFGoiano), GO (Brazil)

    2018-05-01

    This work describes the potential of chemometric analyses applied to {sup 1}H high-resolution magic angle spinning nuclear magnetic resonance ({sup 1}H HR-MAS NMR) data for the chemotaxonomic investigation of Hancornia speciosa (Apocynaceae) varieties. This plant, popularly known as mangaba, has a complex morphological differentiation and thus chemical analyses can be used for their taxonomic classification. In comparison to traditional techniques, {sup 1}H HR-MAS NMR allied with chemometrics provided a simple and low cost method for chemotaxonomy. Leaves of four varieties of H. speciosa from a common garden experiment was studied and demonstrated that H. speciosa var. speciosa differs from others due to its specific metabolic profile, and var. pubescens was discriminated based on its high phenolic compound content. The distinction between the latter variety and gardineri is important once it allows for the selection of samples with greater commercial value, once they produce the largest and heaviest fruits. (author)

  14. Improved background suppression in 1H MAS NMR using composite pulses

    Science.gov (United States)

    Odedra, Smita; Wimperis, Stephen

    2012-08-01

    A well known feature of 1H MAS NMR spectroscopy, particularly of solids where the concentration of 1H nuclei is low, is the presence in the spectrum of a significant broad "background" signal arising from 1H nuclei that are outside the MAS rotor and radiofrequency coil, probably located on the surfaces of the static components of the probehead. A popular method of suppressing this unwanted signal is the "depth pulse" method, consisting of a 90° pulse followed by one or two 180° pulses that are phase cycled according to the "Exorcycle" scheme, which removes signal associated with imperfect 180° pulses. Consequently, only spins in the centre of the radiofrequency coil contribute to the 1H MAS spectrum, while those experiencing a low B1 field outside the coil are suppressed. Although very effective at removing background signal from the spectrum, one drawback with this approach is that significant loss of the desired signal from the sample also occurs. Here we investigate the 1H background suppression problem and, in particular, the use of novel antisymmetric passband composite pulses to replace the simple pulses in a depth pulse experiment. We show that it is possible to improve the intensity of the 1H signals of interest while still maintaining effective background suppression. We expect that these results will be relevant to 1H MAS NMR studies of, for example, nominally perdeuterated biological samples or nominally anhydrous inorganic materials.

  15. Improved background suppression in ¹H MAS NMR using composite pulses.

    Science.gov (United States)

    Odedra, Smita; Wimperis, Stephen

    2012-08-01

    A well known feature of ¹H MAS NMR spectroscopy, particularly of solids where the concentration of ¹H nuclei is low, is the presence in the spectrum of a significant broad "background" signal arising from ¹H nuclei that are outside the MAS rotor and radiofrequency coil, probably located on the surfaces of the static components of the probehead. A popular method of suppressing this unwanted signal is the "depth pulse" method, consisting of a 90° pulse followed by one or two 180° pulses that are phase cycled according to the "Exorcycle" scheme, which removes signal associated with imperfect 180° pulses. Consequently, only spins in the centre of the radiofrequency coil contribute to the ¹H MAS spectrum, while those experiencing a low B₁ field outside the coil are suppressed. Although very effective at removing background signal from the spectrum, one drawback with this approach is that significant loss of the desired signal from the sample also occurs. Here we investigate the ¹H background suppression problem and, in particular, the use of novel antisymmetric passband composite pulses to replace the simple pulses in a depth pulse experiment. We show that it is possible to improve the intensity of the ¹H signals of interest while still maintaining effective background suppression. We expect that these results will be relevant to ¹H MAS NMR studies of, for example, nominally perdeuterated biological samples or nominally anhydrous inorganic materials. Copyright © 2012 Elsevier Inc. All rights reserved.

  16. In situ high temperature MAS NMR study of the mechanisms of catalysis. Ethane aromatization on Zn-modified zeolite BEA.

    Science.gov (United States)

    Arzumanov, Sergei S; Gabrienko, Anton A; Freude, Dieter; Stepanov, Alexander G

    2009-04-01

    Ethane conversion into aromatic hydrocarbons over Zn-modified zeolite BEA has been analyzed by high-temperature MAS NMR spectroscopy. Information about intermediates (Zn-ethyl species) and reaction products (mainly toluene and methane), which were formed under the conditions of a batch reactor, was obtained by (13)C MAS NMR. Kinetics of the reaction, which was monitored by (1)H MAS NMR in situ at the temperature of 573K, provided information about the reaction mechanism. Simulation of the experimental kinetics within the frames of the possible kinetic schemes of the reaction demonstrates that a large amount of methane evolved under ethane aromatization arises from the stage of direct ethane hydrogenolysis.

  17. 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 Hofmann; Chrestensen, Inge Byg; 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...... hydrate more readily than the galactan side chains and suggests that the overall hydration properties can be controlled by modifying the ratio of these side chains. Enzymatic modification of native (NA) RG-I provided samples with reduced content of arabinan (sample DA), galactan (sample DG), or both side...... chains (sample DB). Results of these samples suggested that hydration properties were determined by the length and character of the side chains. NA and DA exhibited similar hydration characteristics, whereas DG and DB were difficult to hydrate because of the less hydrophilic properties of the rhamnose...

  18. Quantum mechanical alternative to Arrhenius equation in the interpretation of proton spin-lattice relaxation data for the methyl groups in solids

    KAUST Repository

    Bernatowicz, Piotr; Shkurenko, Aleksander; Osior, Agnieszka; Kamieński, Bohdan; Szymański, Sławomir

    2015-01-01

    Theory of nuclear spin-lattice relaxation in methyl groups in solids has been a recurring problem in nuclear magnetic resonance (NMR) spectroscopy. The current view is that, except for extreme cases of low torsional barriers where special quantum

  19. Variable temperature 127I MAS NMR of β-AgI

    International Nuclear Information System (INIS)

    Wagner, G.W.

    1991-01-01

    Variable temperature 127 I MAS NMR of β-AgI powder, measured from 123 to 413 K is sensitive to Ag + diffusion through the iodine lattice. In low temperature spectra, the iodine ions appear to be in nearly static environments in agreement with the low temperature crystal structure. However, at higher temperatures, substantial broadening of the central transition linewidth is consistent with the presence of two types of Ag + diffusion with activation energies of 0.17 and 0.0080 eV. (author). 15 refs.; 5 figs.; 1 tab

  20. 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.

  1. 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.

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

    International Nuclear Information System (INIS)

    Eddy, Matthew T.; Su, Yongchao; Silvers, Robert; Andreas, Loren; Clark, Lindsay; Wagner, Gerhard; Pintacuda, Guido; Emsley, Lyndon; Griffin, Robert G.

    2015-01-01

    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 13 C line widths and <0.5 ppm 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 reported

  3. Exploring high-resolution magic angle spinning (HR-MAS) NMR spectroscopy for metabonomic analysis of apples.

    Science.gov (United States)

    Vermathen, Martina; Marzorati, Mattia; Vermathen, Peter

    2012-01-01

    Classical liquid-state high-resolution (HR) NMR spectroscopy has proved a powerful tool in the metabonomic analysis of liquid food samples like fruit juices. In this paper the application of (1)H high-resolution magic angle spinning (HR-MAS) NMR spectroscopy to apple tissue is presented probing its potential for metabonomic studies. The (1)H HR-MAS NMR spectra are discussed in terms of the chemical composition of apple tissue and compared to liquid-state NMR spectra of apple juice. Differences indicate that specific metabolic changes are induced by juice preparation. The feasibility of HR-MAS NMR-based multivariate analysis is demonstrated by a study distinguishing three different apple cultivars by principal component analysis (PCA). Preliminary results are shown from subsequent studies comparing three different cultivation methods by means of PCA and partial least squares discriminant analysis (PLS-DA) of the HR-MAS NMR data. The compounds responsible for discriminating organically grown apples are discussed. Finally, an outlook of our ongoing work is given including a longitudinal study on apples.

  4. 1H CSA parameters by ultrafast MAS NMR: Measurement and applications to structure refinement.

    Science.gov (United States)

    Miah, Habeeba K; Cresswell, Rosalie; Iuga, Dinu; Titman, Jeremy J

    2017-10-01

    A 1 H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν 1 and ultrafast MAS to resolve 1 H sites in ν 2 is described. This experiment is used to measure 1 H shift parameters for L-ascorbic acid, a compound with a relatively complex hydrogen-bonding network in the solid. The 1 H CSAs of hydrogen-bonded sites with resolved isotropic shifts can be extracted directly from the recoupled lineshapes. In combination with DFT calculations, hydrogen positions in crystal structures obtained from X-ray and neutron diffraction are refined by comparison with simulations of the full two-dimensional NMR spectrum. The improved resolution afforded by the second dimension allows even unresolved hydrogen-bonded sites 1 H to be assigned and their shift parameters to be obtained. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. 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.

  6. The water proton spin-lattice relaxation times in virus-infected cells

    International Nuclear Information System (INIS)

    Valensin, G.; Gaggelli, E.; Tiezzi, E.; Valensin, P.E.; Bianchi Bandinelli, M.L.

    1979-01-01

    The water proton spin-lattice relaxation times in HEp-2 cell cultures were determined immediately after 1 h of polio-virus adsorption. The shortening of the water T 1 was closely related to the multiplicity of infection, allowing direct inspections of the virus-cell interaction since the first steps of the infectious cycle. Virus-induced structural and conformational changes of cell constituents were suggested to be detectable by NMR investigation of cell water. (Auth.)

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

    Czech Academy of Sciences Publication Activity Database

    Urbanová, Martina; Brus, Jiří; Šeděnková, Ivana; Policianová, Olivia; Kobera, Libor

    2013-01-01

    Roč. 100, 1 January (2013), s. 59-66 ISSN 1386-1425 R&D Projects: GA ČR GPP106/11/P426; GA MŠk 2B08021 Institutional research plan: CEZ:AV0Z40500505 Institutional support: RVO:61389013 Keywords : solid-state NMR * factor analysis * 19F MAS NMR Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 2.129, year: 2013

  8. A preliminary study of the relation between adsorption and CP-MAS-NMR characteristics of fused silica model substrates

    NARCIS (Netherlands)

    Scholten, A.B.; Janssen, J.G.M.; Haan, de J.W.; Cramers, C.A.M.G.; Sandra, P.J.F.; Devos, G.; Sandra, P.

    1993-01-01

    The fumed silica model substrate Aerosil was trimethylsilylated to different extents and studied by the combination of IGC and 29Si CP-MAS-NMR. Dihydroxydisiloxane groups were shown to be chemically more reactive than monohydroxytrisiloxane groups. Chromatographic experiments showed that these

  9. 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...

  10. New perspectives of 19F MAS NMR in the characterization of amorphous forms of atorvastatin in dosage formulations

    Czech Academy of Sciences Publication Activity Database

    Brus, Jiří; Urbanová, Martina; Šeděnková, Ivana; Brusová, H.

    2011-01-01

    Roč. 409, 1/2 (2011), s. 62-74 ISSN 0378-5173 R&D Projects: GA MŠk 2B08021 Institutional research plan: CEZ:AV0Z40500505 Keywords : 19F MAS NMR * factor analysis * polymorphism Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.350, year: 2011

  11. Gamma-radiation induced cross-links in ethylene-propylene rubber studied by CP-MAS NMR

    International Nuclear Information System (INIS)

    Sohma, J.; Shiotani, M.; Murakami, S.

    1983-01-01

    A new technique of 13 C-NMR, the CP-MAS method, was applied to study a chemistry of cross-links induced by #betta#-irradiation of ethylene-propylene rubber. The chemical species of cross-linking points were specified with their relative concentrations by the analysis of the CP-MAS spectra obtained before and after the irradiation. It was found that the short branches were also formed by the irradiation. A comparison was made between the cross-links detected by the CP-MAS method and those obtained by the Charlesby-Pinner analysis of the gelation caused by the #betta#-irradiation. The conventional 13 C-NMR of the cross-linked and swollen EPR provided us an information on the sol parts of the sample but little information on the cross-links in the gel parts. (author)

  12. Parallel computer calculation of quantum spin lattices

    International Nuclear Information System (INIS)

    Lamarcq, J.

    1998-01-01

    Numerical simulation allows the theorists to convince themselves about the validity of the models they use. Particularly by simulating the spin lattices one can judge about the validity of a conjecture. Simulating a system defined by a large number of degrees of freedom requires highly sophisticated machines. This study deals with modelling the magnetic interactions between the ions of a crystal. Many exact results have been found for spin 1/2 systems but not for systems of other spins for which many simulation have been carried out. The interest for simulations has been renewed by the Haldane's conjecture stipulating the existence of a energy gap between the ground state and the first excited states of a spin 1 lattice. The existence of this gap has been experimentally demonstrated. This report contains the following four chapters: 1. Spin systems; 2. Calculation of eigenvalues; 3. Programming; 4. Parallel calculation

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

    International Nuclear Information System (INIS)

    Zhang, Rongchun; Mroue, Kamal H.; Ramamoorthy, Ayyalusamy

    2015-01-01

    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), 1 H MAS NMR spectra of rigid solids still suffer from poor resolution and severe peak overlap caused by the strong 1 H– 1 H homonuclear dipolar couplings and narrow 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) 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 1 H– 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-level structural and dynamical

  14. Size dependence of 13C nuclear spin-lattice relaxation in micro- and nanodiamonds

    Science.gov (United States)

    Panich, A. M.; Sergeev, N. A.; Shames, A. I.; Osipov, V. Yu; Boudou, J.-P.; Goren, S. D.

    2015-02-01

    Size dependence of physical properties of nanodiamond particles is of crucial importance for various applications in which defect density and location as well as relaxation processes play a significant role. In this work, the impact of defects induced by milling of micron-sized synthetic diamonds was studied by magnetic resonance techniques as a function of the particle size. EPR and 13C NMR studies of highly purified commercial synthetic micro- and nanodiamonds were done for various fractions separated by sizes. Noticeable acceleration of 13C nuclear spin-lattice relaxation with decreasing particle size was found. We showed that this effect is caused by the contribution to relaxation coming from the surface paramagnetic centers induced by sample milling. The developed theory of the spin-lattice relaxation for such a case shows good compliance with the experiment.

  15. Characterization of coal structure by CP/MAS carbon-13 NMR spectrometry

    International Nuclear Information System (INIS)

    Yoshida, T.; Maekawa, Y.

    1987-01-01

    Cross-polarization (CP)/magic angle spinning (MAS) carbon-13 nuclear magnetic resonance (n.m.r.) spectrometry has been applied to the analysis of the whole structures of different ranks of coal. Three basic structural parameters, namely carbon aromaticity fa, new carbon aromaticity fa', and atomic H/C ratio for the hypothetical unsubstituted aromatic nuclei Haru/Car, were derived from the combined data of ultimate analysis, the distributions of carbon and oxygen functional groups obtained from the spectrum and the distribution of four types of methylene carbon groups in coal. Both fa and fa' values generally increased with coal rank and ranged from 0.51 to 0.71 and from 0.62 to 0.76, respectively. Haru/Car value tended to decrease with coal rank although the value was greatly affected by the types of hydroaromatic methylene carbons to aromatic rings. The values indicated that lower-rank coals consisted mainly of 1-3 aromatic rings, and higher-rank coals, 3-5 aromatic rings. 24 refs.; 5 figs.; 4 tabs

  16. Molybdenum modified phosphate glasses studied by 31P MAS NMR and Raman spectroscopy.

    Science.gov (United States)

    Szumera, Magdalena

    2015-02-25

    Glasses have been synthesized in the system P2O5-SiO2-K2O-MgO-CaO modified by addition of MoO3. Glasses were prepared by conventional fusion method from 40 g batches. The influence of Mo-cations on the analysed glass structure was investigated by means of Raman and (31)P MAS-NMR techniques. It has been found that molybdate units can form Mo[MoO4/MoO6]-O-P and/or Mo[MoO4/MoO6]-O-Si bonds with non-bridging oxygens atoms of Q2 methaphosphate units, resulting in the transformation of chain methaphosphate structure into pyrophosphate and finally into orthophosphate structure. It has been also found that increasing amount of MoO3 in the structure of investigated glasses causes their gradual depolymerization and molybdenum ions in the analysed glass matrix act as modifying cations. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Theory of spin-lattice relaxation of diffusing light nuclei in glasses

    International Nuclear Information System (INIS)

    Schirmer, A.; Schirmacher, W.

    1988-01-01

    NMR data of diffusion-induced spin-lattice relaxation in glasses cannot generally be interpreted in the framework of the classical theory of Bloembergen, Purcell and Pound (BPP). Since it is based on exponential density relaxation, generally bnot found in glasses, the BPP formula must be generalized. Here a combination of standard relaxation theory with a hopping model for diffusion in glasses is present. It is shown that the observed anomaties in the NMR data can be explained as a result of anomalous diffusion. 25 refs.; 1 figure

  18. Complex methyl groups dynamics in [(CH3)4P]3Sb2Br9 (PBA) from low to high temperatures by proton spin-lattice relaxation and narrowing of proton NMR spectrum.

    Science.gov (United States)

    Latanowicz, L; Medycki, W; Jakubas, R

    2009-11-01

    Molecular dynamics of a polycrystalline sample of [(CH(3))(4)P](3)Sb(2)Br(9) (PBA) has been studied on the basis of the T(1) (24.7 MHz) relaxation time measurement, the proton second moment of NMR and the earlier published T(1) (90 MHz) relaxation times. The study was performed in a wide range of temperatures (30-337 K). The tunnel splitting omega(T) of the methyl groups was estimated as of low frequency (from kHz to few MHz). The proton spin pairs of the methyl group are known to perform a complex internal motion being a resultant of four components. Three of them involve mass transportation over and through the potential barrier and are characterized by the correlation times tau(3) and tau(T)of the jumps over the barrier and tunnel jumps in the threefold potential of the methyl group and tau(iso) the correlation time of isotropic rotation of the whole TMP cation. For tau(3) and tau(iso) the Arrhenius temperature dependence was assumed, while for tau(T)--the Schrödinger one. The fourth motion causes fluctuations of the tunnel splitting frequency, omega(T), and it is related to the lifetime of the methyl spin at the energy level. The correlation function for this fourth motion (tau(omega) correlation time) has been proposed by Müller-Warmuth et al. In this paper a formula for the correlation function and spectral density of the complex motion made of the above-mentioned four components was derived and used in interpretation of the T(1) relaxation time. The second moment of proton NMR line at temperatures below 50K is four times lower than its value for the rigid structure. The three components of the internal motion characterized by tau(T), tau(H), and tau(iso) were proved to reduce the second moment of the NMR line. The tunnel jumps of the methyl group reduce M(2) at almost 0K, the classical jumps over the barrier reduce M(2) in the vicinity of 50K, while the isotropic motion near 150K. Results of the study on the dynamics of CH(3) groups of TMP cation based on

  19. 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. Copyright © 2013 Wiley Periodicals, Inc.

  20. 1 H MAS NMR study of structure of hybrid siloxane-based networks and the interaction with quartz filler

    Czech Academy of Sciences Publication Activity Database

    Brus, Jiří; Škrdlantová, M.

    2001-01-01

    Roč. 281, 1-3 (2001), s. 61-71 ISSN 0022-3093 R&D Projects: GA ČR GA203/98/P290; GA AV ČR KSK2050602 Institutional research plan: CEZ:AV0Z4050913 Keywords : hybrid siloxane networks * 1 H MAS NMR spectroscopy * hydrogen bonds Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.363, year: 2001

  1. HR-MAS NMR for rapid identification of illicit substances in tablets and Blotter papers seized by Police Department

    Energy Technology Data Exchange (ETDEWEB)

    Souza, Luciano F.; Vieira, Tarcísio S.; Lião, Luciano M., E-mail: lucianoliao@ufg.br [Universidade Federal de Goiás (UFG), Goiânia, GO (Brazil). Instituto de Química; Alcantara, Glaucia B. [Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil). Instituto de Química

    2016-07-01

    Illicit substances found in blotter papers and tablets seized by police are traditionally identified and characterized from extracts of these materials. However, the procedures involved in extraction stages can result in artifacts and even contamination of the samples to be analyzed. On the other hand, high-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR) is a technique that requires no pretreatment steps, enabling direct analysis of the material, including the analysis of new illegal synthetic psychoactive substances. This study presents and discusses applications of the HR-MAS NMR in the analysis of tablets and blotter papers seized. Additional analysis in solution of the extracts of these materials was performed to compare the obtained spectral resolution signals. The results demonstrated that the HR-MAS NMR allowed the rapid identification of 3,4-methylenedioxy-N-methylcathinone (methylone), 4-methylmethcathinone (mephedrone), 2,5-dimethoxy-4-bromoamphetamine (DOB) and 2-(4-bromo-2,5-dimethoxyphenyl)-N-[(2- methoxyphenyl)methyl]ethanamine (25B-NBOMe) in samples of tablets and blotter papers seized in Goiás State, Brazil. (author)

  2. HR-MAS NMR for rapid identification of illicit substances in tablets and Blotter papers seized by Police Department

    International Nuclear Information System (INIS)

    Souza, Luciano F.; Vieira, Tarcísio S.; Lião, Luciano M.; Alcantara, Glaucia B.

    2016-01-01

    Illicit substances found in blotter papers and tablets seized by police are traditionally identified and characterized from extracts of these materials. However, the procedures involved in extraction stages can result in artifacts and even contamination of the samples to be analyzed. On the other hand, high-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR) is a technique that requires no pretreatment steps, enabling direct analysis of the material, including the analysis of new illegal synthetic psychoactive substances. This study presents and discusses applications of the HR-MAS NMR in the analysis of tablets and blotter papers seized. Additional analysis in solution of the extracts of these materials was performed to compare the obtained spectral resolution signals. The results demonstrated that the HR-MAS NMR allowed the rapid identification of 3,4-methylenedioxy-N-methylcathinone (methylone), 4-methylmethcathinone (mephedrone), 2,5-dimethoxy-4-bromoamphetamine (DOB) and 2-(4-bromo-2,5-dimethoxyphenyl)-N-[(2- methoxyphenyl)methyl]ethanamine (25B-NBOMe) in samples of tablets and blotter papers seized in Goiás State, Brazil. (author)

  3. 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...... on the goethite surface. Even larger Li hyperfine shifts (289 ppm) were observed for Li+-exchanged goethite, which contains lithium ions in the tunnels of the goethite structure, confirming the Li assignment of the 145 ppm Li resonance to the surface sites. Udgivelsesdato: 2005-Oct-6...

  4. 27Al MAS NMR spectroscopic identification of reaction intermediates in the carbothermal reduction and nitridation of alumina

    International Nuclear Information System (INIS)

    Jung, Woo-Sik; Chae, Seen-Ae

    2010-01-01

    The reaction intermediates in the carbothermal reduction and nitridation (CRN) reaction of γ-Al 2 O 3 were identified by 27 Al magic-angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy. This identification ruled out the possibility of a reaction mechanism involving the gaseous reaction intermediates. In the CRN reaction of γ-Al 2 O 3 , AlO 4 units were converted to AlN stepwise via AlN x O 4-x (x = 1, 2, 3) intermediates, while AlO 6 units were more slowly converted to AlN than AlO 4 units and the NMR peaks of partially nitridated AlO 6 units were not detected. The NMR peak intensities of partially nitridated AlO 4 units became weaker with increasing reaction temperature.

  5. Spin-lattice relaxation times and knight shift in InSb and InAs

    International Nuclear Information System (INIS)

    Braun, P.; Grande, S.

    1976-01-01

    For a dominant contact interaction between nuclei and conduction electrons the relaxation rate is deduced. The extreme cases of degenerate and non-degenerate semiconductors are separately discussed. At strong degeneracy the product of the Knight shift and relaxation time gives the Korringa relation for metals. Measurements of the NMR spin-lattice relaxation times of 115 InSb and 115 InAs were made between 4.2 and 300 K for strongly degenerated samples. The different relaxation mechanisms are discussed and the experimental and theoretical results are compared. (author)

  6. A new aluminium-hydrate species in hydrated Portland cements characterized by 27Al and 29Si MAS NMR spectroscopy

    International Nuclear Information System (INIS)

    Andersen, Morten Daugaard; Jakobsen, Hans J.; Skibsted, Jorgen

    2006-01-01

    Recent 27 Al MAS NMR studies of hydrated Portland cements and calcium-silicate-hydrate (C-S-H) phases have shown a resonance from Al in octahedral coordination, which cannot be assigned to the well-known aluminate species in hydrated Portland cements. This resonance, which exhibits the isotropic chemical shift δ iso = 5.0 ppm and the quadrupole product parameter P Q = 1.2 MHz, has been characterized in detail by 27 Al MAS and 27 Al{ 1 H} CP/MAS NMR for different hydrated white Portland cements and C-S-H phases. These experiments demonstrate that the resonance originates from an amorphous or disordered aluminate hydrate which contains Al(OH) 6 3- or O x Al(OH) 6-x (3+x)- units. The formation of the new aluminate hydrate is related to the formation of C-S-H at ambient temperatures, however, it decomposes by thermal treatment at temperatures of 70-90 o C. From the experiments in this work it is proposed that the new aluminate hydrate is either an amorphous/disordered aluminate hydroxide or a calcium aluminate hydrate, produced as a separate phase or as a nanostructured surface precipitate on the C-S-H phase. Finally, the possibilities of Al 3+ for Ca 2+ substitution in the principal layers and interlayers of the C-S-H structure are discussed

  7. 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.

  8. 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.

  9. 27Al Magic Angle Spinning–Nuclear Magnetic Resonance (MAS-NMR) Analyses Applied to Historical Mortars

    Czech Academy of Sciences Publication Activity Database

    Hanzlíček, Tomáš; Perná, Ivana; Brus, Jiří

    2013-01-01

    Roč. 7, č. 2 (2013), s. 153-164 ISSN 1558-3058 R&D Projects: GA AV ČR IAA300460702 Institutional research plan: CEZ:AV0Z30460519; CEZ:AV0Z40500505 Keywords : mortars * magic angle spinning –nuclear magnetic resonance (MAS-NMR) in solid state * alumina-silicates Subject RIV: DM - Solid Waste and Recycling Impact factor: 0.714, year: 2013 http://www.tandfonline.com/doi/abs/10.1080/15583058.2011.624253

  10. Chemical profile of beans cultivars (Phaseolus vulgaris) by 1H NMR - high resolution magic angle spinning (HR-MAS);Perfil quimico de cultivares de feijao (Phaseolus vulgaris) pela tecnica de high resolution magic angle spinning (HR-MAS)

    Energy Technology Data Exchange (ETDEWEB)

    Liao, Luciano Morais; Choze, Rafael; Cavalcante, Pedro Paulo Araujo; Santos, Suzana da Costa; Ferri, Pedro Henrique, E-mail: luciano@quimica.ufg.b [Universidade Federal de Goias (UFG), Goiania, GO (Brazil). Inst. de Quimica; Ferreira, Antonio Gilberto [Universidade Federal de Sao Carlos (UFScar), SP (Brazil). Dept. de Quimica

    2010-07-01

    The application of one-dimensional proton high-resolution magic angle spinning ({sup 1}H 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 Feijao were analyzed by {sup 1}H 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. (author)

  11. Lightweight hydrogen-storage material Mg0.65Sc0.35D2 studied with 2H and 2H–{45Sc} MAS NMR exchange spectroscopy

    NARCIS (Netherlands)

    Srinivasan, S.; Magusin, P.C.M.M.

    2011-01-01

    Using double-quantum 2H MAS NMR with 45Sc recoupling and Bloch–Siegert compensated 2H–{45Sc} TRAPDOR we have identified the overlapping NMR signals of deuterium with and without scandium neighbors in Mg0.65Sc0.35D2, a candidate lightweight material for hydrogen storage. At room temperature we also

  12. 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.

  13. 6Li MAS NMR Study of Lithium Insertion into Hydrothermally Prepared Li-Ti-O Spinel

    Czech Academy of Sciences Publication Activity Database

    Krtil, Petr; Dědeček, Jiří; Kostlánová, Tereza; Brus, Jiří

    2004-01-01

    Roč. 7, č. 7 (2004), A163-A166 ISSN 1099-0062 R&D Projects: GA ČR GA203/03/0823 Institutional research plan: CEZ:AV0Z4040901 Keywords : lithium insertion * spinel * NMR Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.271, year: 2004

  14. Glycerin-Induced Conformational Changes in Bombyx mori Silk Fibroin Film Monitored by (13)C CP/MAS NMR and ¹H DQMAS NMR.

    Science.gov (United States)

    Asakura, Tetsuo; Endo, Masanori; Hirayama, Misaki; Arai, Hiroki; Aoki, Akihiro; Tasei, Yugo

    2016-09-09

    In order to improve the stiff and brittle characteristics of pure Bombyx mori (B. mori) silk fibroin (SF) film in the dry state, glycerin (Glyc) has been used as a plasticizer. However, there have been very limited studies on the structural characterization of the Glyc-blended SF film. In this study, (13)C Cross Polarization/Magic Angle Spinning nuclear magnetic resonance (CP/MAS NMR) was used to monitor the conformational changes in the films by changing the Glyc concentration. The presence of only 5 wt % Glyc in the film induced a significant conformational change in SF where Silk I* (repeated type II β-turn and no α-helix) newly appeared. Upon further increase in Glyc concentration, the percentage of Silk I* increased linearly up to 9 wt % Glyc and then tended to be almost constant (30%). This value (30%) was the same as the fraction of Ala residue within the Silk I* form out of all Ala residues of SF present in B. mori mature silkworm. The ¹H DQMAS NMR spectra of Glyc-blended SF films confirmed the appearance of Silk I* in the Glyc-blended SF film. A structural model of Glyc-SF complex including the Silk I* form was proposed with the guidance of the Molecular Dynamics (MD) simulation using ¹H-¹H distance constraints obtained from the ¹H Double-Quantum Magic Angle Spinning (DQMAS) NMR spectra.

  15. Spin-echo based diagonal peak suppression in solid-state MAS NMR homonuclear chemical shift correlation spectra

    Science.gov (United States)

    Wang, Kaiyu; Zhang, Zhiyong; Ding, Xiaoyan; Tian, Fang; Huang, Yuqing; Chen, Zhong; Fu, Riqiang

    2018-02-01

    The feasibility of using the spin-echo based diagonal peak suppression method in solid-state MAS NMR homonuclear chemical shift correlation experiments is demonstrated. A complete phase cycling is designed in such a way that in the indirect dimension only the spin diffused signals are evolved, while all signals not involved in polarization transfer are refocused for cancellation. A data processing procedure is further introduced to reconstruct this acquired spectrum into a conventional two-dimensional homonuclear chemical shift correlation spectrum. A uniformly 13C, 15N labeled Fmoc-valine sample and the transmembrane domain of a human protein, LR11 (sorLA), in native Escherichia coli membranes have been used to illustrate the capability of the proposed method in comparison with standard 13C-13C chemical shift correlation experiments.

  16. 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...... regions was only observed in NA starch. Moreover phosphorous was observed in a minor pH-insensitive form and as major phosphate in hydrated GEL and BE starches....

  17. Studies using 27Al MAS NMR of AFm and AFt phases and the formation of Friedel's salt

    International Nuclear Information System (INIS)

    Jones, M.R.; Macphee, D.E.; Chudek, J.A.; Hunter, G.; Lannegrand, R.; Talero, R.; Scrimgeour, S.N.

    2003-01-01

    This paper describes the application of the magic angle spinning (MAS) NMR spectroscopy to study the chemical environment of 27 Al-bearing phases in Portland cement-based concrete. A specific methodology is described that allows reliable spectra to be determined for combinations of different types of cements and fillers (in this case, Portland cement, fly ash, slag, silica fume, metakaolin and limestone filler). As well as the study of 'molecular structure' of cement matrix, the paper reviews the mechanism of Friedel's salt formation in cement systems. Mechanisms based on ion exchange of chloride for hydroxide in hydroxy-AF m and on chloride absorption on formation are discussed. Finally, the nature of the chloride/hydrate binding phenomena are described to provide a reasonable robust and fundamental picture of the role different cements can play in the provision of overall concrete durability to chloride ingress from a chemical perspective

  18. 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.

  19. 1H MAS NMR (magic-angle spinning nuclear magnetic resonance) techniques for the quantitative determination of hydrogen types in solid catalysts and supports.

    Science.gov (United States)

    Kennedy, Gordon J; Afeworki, Mobae; Calabro, David C; Chase, Clarence E; Smiley, Randolph J

    2004-06-01

    Distinct hydrogen species are present in important inorganic solids such as zeolites, silicoaluminophosphates (SAPOs), mesoporous materials, amorphous silicas, and aluminas. These H species include hydrogens associated with acidic sites such as Al(OH)Si, non-framework aluminum sites, silanols, and surface functionalities. Direct and quantitative methodology to identify, measure, and monitor these hydrogen species are key to monitoring catalyst activity, optimizing synthesis conditions, tracking post-synthesis structural modifications, and in the preparation of novel catalytic materials. Many workers have developed several techniques to address these issues, including 1H MAS NMR (magic-angle spinning nuclear magnetic resonance). 1H MAS NMR offers many potential advantages over other techniques, but care is needed in recognizing experimental limitations and developing sample handling and NMR methodology to obtain quantitatively reliable data. A simplified approach is described that permits vacuum dehydration of multiple samples simultaneously and directly in the MAS rotor without the need for epoxy, flame sealing, or extensive glovebox use. We have found that careful optimization of important NMR conditions, such as magnetic field homogeneity and magic angle setting are necessary to acquire quantitative, high-resolution spectra that accurately measure the concentrations of the different hydrogen species present. Details of this 1H MAS NMR methodology with representative applications to zeolites, SAPOs, M41S, and silicas as a function of synthesis conditions and post-synthesis treatments (i.e., steaming, thermal dehydroxylation, and functionalization) are presented.

  20. Quality of spelt pasta enriched with eggs and identification of eggs using 13C MAS NMR spectroscopy

    Directory of Open Access Journals (Sweden)

    Filipović Jelena S.

    2015-01-01

    Full Text Available This paper deals with the characteristics of spelt pasta enriched with eggs. Eggs were added to spelt farina in the quantity of 0, 124 or 248 g/kg (equivalent to 0, 3 or 6 eggs, respectively. Post-hoc Tukey’s HSD test at 95% confidence limit showed significant differences between various samples. Relatively low coefficients of variation have been obtained for each applied assay (1.25-12.42%, which confirmed the high accuracy measurements and statistically significant results. Standard score analysis is applied for accessing the contribution of eggs content to spelt pasta quality. Maximum scores regarding quality (0.89 and chemical characteristics (0.70, have been obtained for 6 eggs spelt pasta formulation. It is also shown that the presence of eggs in pasta can be clearly confirmed by 13C MAS NMR spectroscopy. Simultaneous increase in area of peak positioned at 29.5 and 176 ppm is directly associated with the increase in the content of added eggs in the corresponding samples. Pertinent data point at positive contribution of eggs to the spelt pasta and also that NMR spectrum can be used in the egg quantity control. [Projekat Ministarstva nauke Republike Srbije, br. TRI 46005 i br. TR 31029

  1. Analysis of Hydroperoxides in Solid Polyethylene by MAS (13)C NMR and EPR

    International Nuclear Information System (INIS)

    ASSINK, ROGER A.; CELINA, MATHIAS C.; DUNBAR, TIMOTHY D.; ALAM, TODD M.; CLOUGH, ROGER LEE; GILLEN, KENNETH T.

    1999-01-01

    13 C-enriched polyethylene was subjected to γ-irradiation in the presence of air at 25 and 80 C for total doses ranging from 71 to 355 kGy. Significant quantities of hydroperoxides were detected in the 25 C irradiated sample by 13 C magic angle spinning NMR spectroscopy. This method of detection was performed on the solid polymer and required no chemical derivatization or addition of solvent. The chemical stability and subsequent products of the hydroperoxide species were studied by annealing the irradiated samples in air at temperatures ranging from 22 to 110 C. A time-temperature superposition analysis provided an activation energy of 108 kJ/mol for the hydroperoxide decomposition process. The primary products of hydroperoxide decomposition were ketones and secondary alcohols with lesser amounts of acids and esters. EPR measurements suggest that the reactive hydroperoxide species reside in the amorphous phase of polyethylene, consistent with degradation occurring in the amorphous phase

  2. Spin-Lattice Coupling and Superconductivity in Fe Pnictides

    Directory of Open Access Journals (Sweden)

    T. Egami

    2010-01-01

    Full Text Available We consider strong spin-lattice and spin-phonon coupling in iron pnictides and discuss its implications on superconductivity. Strong magneto-volume effect in iron compounds has long been known as the Invar effect. Fe pnictides also exhibit this effect, reflected in particular on the dependence of the magnetic moment on the atomic volume of Fe defined by the positions of the nearest neighbor atoms. Through the phenomenological Landau theory, developed on the basis of the calculations by the density functional theory (DFT and the experimental results, we quantify the strength of the spin-lattice interaction as it relates to the Stoner criterion for the onset of magnetism. We suggest that the coupling between electrons and phonons through the spin channel may be sufficiently strong to be an important part of the superconductivity mechanism in Fe pnictides.

  3. Spin-lattice relaxation of individual solid-state spins

    Science.gov (United States)

    Norambuena, A.; Muñoz, E.; Dinani, H. T.; Jarmola, A.; Maletinsky, P.; Budker, D.; Maze, J. R.

    2018-03-01

    Understanding the effect of vibrations on the relaxation process of individual spins is crucial for implementing nanosystems for quantum information and quantum metrology applications. In this work, we present a theoretical microscopic model to describe the spin-lattice relaxation of individual electronic spins associated to negatively charged nitrogen-vacancy centers in diamond, although our results can be extended to other spin-boson systems. Starting from a general spin-lattice interaction Hamiltonian, we provide a detailed description and solution of the quantum master equation of an electronic spin-one system coupled to a phononic bath in thermal equilibrium. Special attention is given to the dynamics of one-phonon processes below 1 K where our results agree with recent experimental findings and analytically describe the temperature and magnetic-field scaling. At higher temperatures, linear and second-order terms in the interaction Hamiltonian are considered and the temperature scaling is discussed for acoustic and quasilocalized phonons when appropriate. Our results, in addition to confirming a T5 temperature dependence of the longitudinal relaxation rate at higher temperatures, in agreement with experimental observations, provide a theoretical background for modeling the spin-lattice relaxation at a wide range of temperatures where different temperature scalings might be expected.

  4. A MAS NMR and DRIFT study of the Ga species in Ga/H-ZSM5 catalysts and their effect on propane ammoxidation

    NARCIS (Netherlands)

    Pal, P.; Quartararo, J.; Hamid, abd S.B.; Derouane, E.G.; Védrine, J.C.; Magusin, P.C.M.M.; Anderson, B.G.

    2005-01-01

    71Ga, 27Al and 29Si MAS-NMR and DRIFT spectroscopies were used to characterize the state of gallium in Ga/H-ZSM5 catalysts tested for their ability to catalyse the ammoxidation of propane. Ga-species were observed in two different possible environments: octahedrally-coordinated gallium in small

  5. 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...

  6. Structural investigations of borosilicate glasses containing MoO{sub 3} by MAS NMR and Raman spectroscopies

    Energy Technology Data Exchange (ETDEWEB)

    Caurant, D., E-mail: daniel-caurant@enscp.f [Laboratoire de Chimie de la Matiere Condensee de Paris, UMR-CNRS 7574, Ecole Nationale Superieure de Chimie de Paris (ENSCP, ParisTech), 11 rue Pierre et Marie Curie, 75231 Paris (France); Majerus, O.; Fadel, E.; Quintas, A. [Laboratoire de Chimie de la Matiere Condensee de Paris, UMR-CNRS 7574, Ecole Nationale Superieure de Chimie de Paris (ENSCP, ParisTech), 11 rue Pierre et Marie Curie, 75231 Paris (France); Gervais, C. [Laboratoire de Chimie de la Matiere Condensee de Paris, UMR-CNRS 7574, Universite Pierre et Marie Curie, 75252 Paris (France); Charpentier, T. [CEA, IRAMIS, Service Interdisciplinaire sur les Systemes Moleculaires et Materiaux, CEA Saclay, 91191 Gif-sur-Yvette (France); Neuville, D. [Physique des Mineraux et des Magmas, UMR-CNRS 7047, Institut de Physique du Globe, place Jussieu, 75252 Paris (France)

    2010-01-01

    High molybdenum concentration in glass compositions may lead to alkali and alkaline-earth molybdates crystallization during melt cooling that must be controlled particularly during the preparation of highly radioactive nuclear glassy waste forms. To understand the effect of molybdenum addition on the structure of a simplified nuclear glass and to know how composition changes can affect molybdates crystallization tendency, the structure of two glass series belonging to the SiO{sub 2}-B{sub 2}O{sub 3}-Na{sub 2}O-CaO-MoO{sub 3} system was studied by {sup 29}Si, {sup 11}B, {sup 23}Na MAS NMR and Raman spectroscopies by increasing MoO{sub 3} or B{sub 2}O{sub 3} concentrations. Increasing MoO{sub 3} amount induced an increase of the silicate network reticulation but no significant effect was observed on the proportion of BO{sub 4}{sup -} units and on the distribution of Na{sup +} cations in glass structure. By increasing B{sub 2}O{sub 3} concentration, a strong evolution of the distribution of Na{sup +} cations was observed that could explain the evolution of the nature of molybdate crystals (CaMoO{sub 4} or Na{sub 2}MoO{sub 4}) formed during melt cooling.

  7. Structure of Selected Derivates of p-Hydroxy Cynamonic Acid According to 13C CP MAS NMR and DFT Calculation

    International Nuclear Information System (INIS)

    Pisklak, D.M.; Wawer, I.; Tkaczyk, M.

    2005-01-01

    Derivatives of p-hydroxy cynamonic acid are widely occurring in fruits, vegetables, tea and coffee. They exhibit strong antioxidant activity due to the presence of phenolic group. Epidemiological, biological and biochemical data support health beneficial role of this group of compounds and anticarcinogenic, antimutagenic and antiinflamatory effects have been reported. The most common caffeic acid contributes significantly to the total polyphenol intake and has been suggested to play a role in the apparent association between the regular consumption of polyphenol-rich food and beverages, and the prevetion of inflammatory and proliferative diseases. 13 C MAS NMR spectra were recorded on a BRUKER DSX 400 spectrometer at 400,13. Powder samples were spun in a 4 mm rotor at 10 kHz ( 13 C). Signals were assigned:- By comparison with solution spectra; - Using dipolar dephasing and variable contact time experiments; - Confirmed by DFT calculations of shielding constants. The differences in chemical shifts between solution and solid state spectra are due to the formation of intramolecular and intermolecular hydrogen bonds, including C-OH...OC within cyclic dimers. (author)

  8. 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.

  9. Spin-lattice relaxation in phosphorescent triplet state molecules

    International Nuclear Information System (INIS)

    Verbeek, P.J.F.

    1979-01-01

    The present thesis contains the results of a study of spin-lattice relaxation (SLR) in the photo-excited triplet state of aromatic molecules, dissolved in a molecular host crystal. It appears that SLR in phosphorescent triplet state molecules often is related to the presence of so-called (pseudo) localized phonons in the molecular mixed crystals. These local phonons can be thought to correspond with vibrations (librations) of the guest molecule in the force field of the surrounding host molecules. Since the intermolecular forces are relatively weak, the frequencies corresponding with these vibrations are relatively low and usually are of the order of 10-30 cm -1 . (Auth.)

  10. Measurement of solute proton spin-lattice relaxation times in water using the 1,3,3,1 sequence

    International Nuclear Information System (INIS)

    Sankar, S.S.; Mole, P.A.; Coulson, R.L.

    1986-01-01

    1 H NMR spin-lattice relaxation times (T1) of the N-CH3 proton resonances of phosphocreatine (PCr) and creatine (Cr) in water solutions were obtained using the 1,3,3,1 pulse sequence. These T1 values were equivalent to those obtained in D 2 O and water using either the conventional inversion-recovery experiment or the 1,3,3,1 pulse sequence. Thus, the 1,3,3,1 sequence of proton NMR can provide an independent means along with phosphorous NMR for assess PCr and for the study of the creatine kinase reaction (PCr + ADP in equilibrium ATP + Cr) in aqueous solutions and perhaps in biological preparations

  11. 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

    International Nuclear Information System (INIS)

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

    2012-01-01

    The location of extraframework cations in Sr 2+ and Ba 2+ ion-exchanged SAPO-34 was estimated by means of 1 H and 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 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 2 adsorption performance. Highlights: ► Location of extraframework Sr 2+ or Ba 2+ cations was estimated by means of 1 H and 23 Na MAS NMR. ► Level of Sr 2+ or Ba 2+ ion exchange was limited by the presence of protons and sodium cations. ► Presence of ammonium cations in the supercages facilitated the exchange. ► Sr 2+ and Ba 2+ ion exchanged SAPOs are outstanding CO 2 adsorbents.

  12. 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......, even at temperatures above the Neel temperature, TN, 77 K. The formation of a Li+ inner-sphere complex on the surface of lepiclocrocite was confirmed by the observation of a signal with a large 7Li hyperfine shift in the 7Li  MAS NMR spectrum. The effect of pH and relative humidity (RH...

  13. Evaluation of PHB/Clay nanocomposite by spin-lattice relaxation time

    Directory of Open Access Journals (Sweden)

    Mariana Bruno

    2008-12-01

    Full Text Available Poly(3-hydroxybutyrate (PHB based on nanocomposites containing different amounts of a commercial organically modified clay (viscogel B7 were prepared employing solution intercalation method. Three solvents, such as: CHCl3, dimethylchloride (DMC and tetrahydrofuran (THF were used. The relationship among the processing conditions; molecular structure and intermolecular interaction, between both nanocomposite components, were investigated using a nuclear magnetic resonance (NMR, as a part of characterization methodology, which has been used by Tavares et al. It involves the hydrogen spin-lattice relaxation time, T1H, by solid state nuclear magnetic resonance, employing low field NMR. X ray diffraction was also employed because it is a conventional technique, generally used to obtain the first information on nanocomposite formation. Changes in PHB crystallinity were observed after the organophilic nanoclay had been incorporated in the polymer matrix. These changes, in the microstructure, were detected by the variation of hydrogen nuclear relaxation time values and by X ray, which showed an increase in the clay interlamelar space due to the intercalation of the polymer in the clay between lamellae. It was also observed, for both techniques, that the solvents affect directly the organization of the crystalline region, promoting a better intercalation, considering that they behave like a plasticizer.

  14. Localized-magnon states in strongly frustrated quantum spin lattices

    International Nuclear Information System (INIS)

    Richter, J.

    2005-01-01

    Recent developments concerning localized-magnon eigenstates in strongly frustrated spin lattices and their effect on the low-temperature physics of these systems in high magnetic fields are reviewed. After illustrating the construction and the properties of localized-magnon states we describe the plateau and the jump in the magnetization process caused by these states. Considering appropriate lattice deformations fitting to the localized magnons we discuss a spin-Peierls instability in high magnetic fields related to these states. Last but not least we consider the degeneracy of the localized-magnon eigenstates and the related thermodynamics in high magnetic fields. In particular, we discuss the low-temperature maximum in the isothermal entropy versus field curve and the resulting enhanced magnetocaloric effect, which allows efficient magnetic cooling from quite large temperatures down to very low ones

  15. Evidence for radiation induced crosslinking in polytetrafluoroethylene by means of high-resolution solid-state 19F high-speed MAS NMR

    International Nuclear Information System (INIS)

    Katoh, Etsuko; Sugisawa, Hisashi; Oshima, Akihiro; Tabata, Yoneho; Seguchi, Tadao; Yamazaki, Toshimasa

    1999-01-01

    Radiation effects on molecular structure of polytetrafluoroethylene (PTFE) were studied by high-resolution solid-state 19 F high speed magic angle spinning (HS MAS) NMR spectroscopy. Samples used for the NMR studies were prepared by electron beam irradiation of PTFE with a wide range of irradiation doses from 0.5-10 MGy in the molten state at 340 deg. C under oxygen-free atmosphere. While the non-irradiated PTFE displayed only an intense peak of the internal CF 2 , several new signals corresponding to CF 3 , CF 2 and CF groups were observed for the PTFE which was high temperature irradiated at 340 deg. C in oxygen-free atmosphere (hti-PTFE). Intensities of these new signals increased with an increase of irradiation dose. The present solid-state 19 F HS MAS NMR studies provide not only the first experimental evidence regarding the existence of crosslinking structure in hti-PTFE, directly detected as the CF signal, but also the crosslinking density which can be estimated from a proportion of the CF versus total fluorine signal intensities. The higher the irradiation dose, the higher the crosslinking density; hti-PTFE with 10 MGy contains one crosslinking site per approximately 24 CF 2 groups, while the hti-PTFE with 5 MGy contains one crosslinking site per approximately 36 CF 2 groups. Further, G value of crosslinking (G(x)) was estimated from the signal intensities of 19 F HS MAS NMR spectra. The highest G(x)-value, 1.85, was observed for the 2MGy hti-PTFE sample, suggesting that crosslinking of PTFE is formed most efficaciously with 2 MGy irradiation in the molten state at 340 deg. C under oxygen-free atmosphere

  16. 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.

  17. Obtaining aluminas from the thermal decomposition of their different precursors: An {sup 27}Al MAS NMR and X-ray powder diffraction studies

    Energy Technology Data Exchange (ETDEWEB)

    Chagas, L.H.; De Carvalho, G.S.G. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); San Gil, R.A.S. [Universidade Federal do Rio de Janeiro, Instituto de Química, 21949-900 Rio de Janeiro, RJ (Brazil); Chiaro, S.S.X. [PETROBRAS-CENPES, 21941-915 Rio de Janeiro, RJ (Brazil); Leitão, A.A. [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil); Diniz, R., E-mail: renata.diniz@ufjf.edu.br [Universidade Federal de Juiz de Fora, Departamento de Química, Grupo de Físico-Química de Sólidos e Interfaces, 36036-330 Juiz de Fora, MG (Brazil)

    2014-01-01

    Graphical abstract: - Highlights: • We synthesized three precursors of alumina from different methods. • The calcination of the precursors generated several alumina polymorphs. • XRD and NMR were used for structural investigation of the polymorphs. • The synthesis route determines the structural and textural properties of the solids. - Abstract: A commercial sample of Boehmite was used as precursor of alumina polymorphs. For comparison, three other precursors were synthesized from different methods. Particularly, the use of excess of urea promoted a very crystalline form of basic aluminum carbonate. The characteristics of the four precursors were investigated by thermal, vibrational and X-ray powder diffraction (XRD) analysis. Additionally, the nuclear magnetic resonance, with magic angle spinning ({sup 27}Al MAS NMR), was used to verify the coordination of aluminum cations. Each precursor was calcined at various temperatures generating alumina polymorphs, which were structurally analyzed by XRD and {sup 27}Al MAS NMR. Due to interest in catalysis supports, special attention was given to the γ-Al{sub 2}O{sub 3} phase, which in addition to structural investigation was subjected to textural analysis. The results showed that, from different synthesis procedures and common route of calcination, one can obtain materials with the same composition but with different structural and textural properties, which in turn can significantly influence the performance of a supported catalyst.

  18. 1H-detected MAS solid-state NMR experiments enable the simultaneous mapping of rigid and dynamic domains of membrane proteins

    Science.gov (United States)

    Gopinath, T.; Nelson, Sarah E. D.; Veglia, Gianluigi

    2017-12-01

    Magic angle spinning (MAS) solid-state NMR (ssNMR) spectroscopy is emerging as a unique method for the atomic resolution structure determination of native membrane proteins in lipid bilayers. Although 13C-detected ssNMR experiments continue to play a major role, recent technological developments have made it possible to carry out 1H-detected experiments, boosting both sensitivity and resolution. Here, we describe a new set of 1H-detected hybrid pulse sequences that combine through-bond and through-space correlation elements into single experiments, enabling the simultaneous detection of rigid and dynamic domains of membrane proteins. As proof-of-principle, we applied these new pulse sequences to the membrane protein phospholamban (PLN) reconstituted in lipid bilayers under moderate MAS conditions. The cross-polarization (CP) based elements enabled the detection of the relatively immobile residues of PLN in the transmembrane domain using through-space correlations; whereas the most dynamic region, which is in equilibrium between folded and unfolded states, was mapped by through-bond INEPT-based elements. These new 1H-detected experiments will enable one to detect not only the most populated (ground) states of biomacromolecules, but also sparsely populated high-energy (excited) states for a complete characterization of protein free energy landscapes.

  19. 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...... physical and chemical treatments to natural rubber it is shown that mastication, gamma-irradiation, and increasing the temperature, slightly above the ambient, reduce the amount of immobile regions. (C) 1999 Elsevier Science Ltd. All rights reserved....

  20. Nuclear spin-lattice relaxation in nitroxide spin-label EPR

    DEFF Research Database (Denmark)

    Marsh, Derek

    2016-01-01

    that the definition of nitrogen nuclear relaxation rate Wn commonly used in the CW-EPR literature for 14N-nitroxyl spin labels is inconsistent with that currently adopted in time-resolved EPR measurements of saturation recovery. Redefinition of the normalised 14N spin-lattice relaxation rate, b = Wn/(2We), preserves...... of spin-lattice relaxation in this three-level system. Expressions for CW-saturation EPR with the revised definitions are summarised. Data on nitrogen nuclear spin-lattice relaxation times are compiled according to the three-level scheme for 14N-relaxation: T1 n = 1/Wn. Results are compared and contrasted...

  1. Fate of [15N]glycine in peat as determined by 13C and 15N CP-MAS NMR spectroscopy

    International Nuclear Information System (INIS)

    Benzing-Purdie, L.M.; Cheshire, M.V.; Williams, B.L.; Sparling, G.P.; Ratcliffe, C.I.; Ripmeester, J.A.

    1986-01-01

    Peat samples, nonsterile, sterilized by γ irradiation or autoclaving, were incubated with [ 15 N]glycine for a period of 6 months. The 13 C NMR data showed the established trend of increased humification with decreasing particle size and that autoclaving had significantly disturbed the humification-particle size distribution. The 15 N CP-MAS NMR spectra showed the presence of [ 15 N]glycine in all fractions after incubation. 15 NH 4 + , a result of either biological or chemical deamination, was one of the main products in the nonsterile peat series. The 15 N spectra also showed resonances corresponding to amine, secondary amide, and pyrrole-type nitrogen and the presence of glycine derivatives and melanoidins. The results presented give the first spectroscopic evidence of the possible involvement of the Maillard reaction in the humification process

  2. 1H line width dependence on MAS speed in solid state NMR - Comparison of experiment and simulation

    Science.gov (United States)

    Sternberg, Ulrich; Witter, Raiker; Kuprov, Ilya; Lamley, Jonathan M.; Oss, Andres; Lewandowski, Józef R.; Samoson, Ago

    2018-06-01

    Recent developments in magic angle spinning (MAS) technology permit spinning frequencies of ≥100 kHz. We examine the effect of such fast MAS rates upon nuclear magnetic resonance proton line widths in the multi-spin system of β-Asp-Ala crystal. We perform powder pattern simulations employing Fokker-Plank approach with periodic boundary conditions and 1H-chemical shift tensors calculated using the bond polarization theory. The theoretical predictions mirror well the experimental results. Both approaches demonstrate that homogeneous broadening has a linear-quadratic dependency on the inverse of the MAS spinning frequency and that, at the faster end of the spinning frequencies, the residual spectral line broadening becomes dominated by chemical shift distributions and susceptibility effects even for crystalline systems.

  3. Solid state proton spin-lattice relaxation in four structurally related organic molecules

    International Nuclear Information System (INIS)

    Beckmann, Peter A.; Burbank, Kendra S.; Lau, Matty M.W.; Ree, Jessica N.; Weber, Tracy L.

    2003-01-01

    We report and interpret the temperature dependence of the proton spin-lattice relaxation rate at 8.50 and 22.5 MHz in four polycrystalline solids composed of structurally related molecules: 2-ethylanthracene, 2-t-butylanthracene, 2-ethylanthraquinone, and 2-t-butylanthraquinone. We have been unable to grow single crystals and therefore do not know the crystal structures. Hence, we use the NMR relaxometry data to make predictions about the solid state structures. As expected, we are able to conclude that the ethyl groups do not reorient in the solid state but that the t-butyl groups do. The anthraquinones have a ''simpler'' structure than the anthracenes. The best dynamical models suggest that there is a unique crystallographic site for the t-butyl groups in 2-t-butylanthraquinone and two sites, each with half the molecules, for the ethyl groups in 2-ethylanthraquinone. There are also two sites in 2-ethylanthracene, but with unequal weights, suggesting four sites in the unit cell with lower symmetry than the two anthraquinones. Finally, the observed relaxation rate data in 2-t-butylanthracene is very complex and its interpretation demonstrates the uniqueness problem that arises in interpreting relaxometry data without the knowledge of the crystal structure

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

    International Nuclear Information System (INIS)

    Emami, Sanaz; Fan Ying; Munro, Rachel; Ladizhansky, Vladimir; Brown, Leonid S.

    2013-01-01

    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 ( 13 C/ 15 N) isotopically labeled in this system and functionally reconstituted into phospholipids, giving excellent resolution of solid-state magic angle spinning NMR spectra.

  5. 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.

  6. CP/MAS 13C NMR characterization of the isomeric states and intermolecular packing in tris(8-hydroxyquinoline) aluminum(III) (Alq3).

    Science.gov (United States)

    Kaji, Hironori; Kusaka, Yasunari; Onoyama, Goro; Horii, Fumitaka

    2006-04-05

    The isomeric states and intermolecular packing of tris(8-hydroxyquinoline) aluminum(III) (Alq(3)) in the alpha-, gamma-, and delta-crystalline forms and in the amorphous state, which are important for understanding the light-emitting and electron-transport properties, have been analyzed by CP/MAS (13)C NMR. This simple NMR experiment shows that the isomeric state of alpha- and amorphous Alq(3) is meridional, whereas that of gamma- and delta-Alq(3) is facial. In the amorphous Alq(3), the inclusion of facial isomers has been under debate. Our experiments show that meridional isomers are dominant in the amorphous Alq(3), although the existence of facial isomers cannot be completely denied. The local structure of amorphous Alq(3) is similar to that of alpha-Alq(3) and is significantly different from those of gamma- and delta-Alq(3). Among these Alq(3) samples, the effect of intermolecular interaction is not found only for gamma-Alq(3). This finding can explain the good solvent solubility of gamma-Alq(3), compared with the other crystalline forms. It is also shown that the structures are locally disordered not only for amorphous Alq(3) but also for alpha-Alq(3), although clear X-ray diffraction peaks are observed for alpha-Alq(3). In contrast, the local structures of gamma- and delta-Alq(3) are well defined. A clear relation is found between the spectral patterns of CP/MAS (13)C NMR and the fluorescence wavelengths; the samples, which consist of facial isomers, show blue-shifted fluorescence compared with those of meridionals.

  7. Solid state NMR study of cumbaru flour

    International Nuclear Information System (INIS)

    Nogueira, Jose S.; Bathista, Andre L.B.S.; Silva, Emerson O.; Priante Filho, Nicolau; Tavares, Maria I.B.

    2001-01-01

    The polysaccharide obtained by seed of Dipteryx alata Vog, has been characterised by 13 C solid state, using the basic routine techniques, like MAS and CPMAS and by the proton spin-lattice relaxation time in the rotating frame parameter (T 1 H ρ). Knowing that the chemical structure and molecular dynamic are extremely necessary route to obtain information on the polysaccharides, this work contributes to the classification of the seed containing in the cumbaru fruit to get response on its application. To obtain the initial responses for our purposes some solid state NMR techniques were chosen. The CPMAS 13 C NMR spectrum of the polysaccharide was investigated to know if it has some crystallinity. The MAS 13 C NMR spectrum showed the presence of domains with distinct molecular mobility, because these domains will differ basically in the distribution size and chain packing. The variable contact time experiment was used to analyse the distribution form of 13 C decays, which give us more information about sample heterogeneity. The T 1 H ρHr values were obtained from the variable contact time and by delayed contact time experiment, because these parameter indicate the order of polysaccharides. From the values of this parameter, we found that this polysaccharide is completely non-ordered. (author)

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

    Czech Academy of Sciences Publication Activity Database

    Urbanová, Martina; Šturcová, Adriana; Brus, Jiří; Beneš, Hynek; Skořepová, E.; Kratochvíl, B.; Čejka, J.; Šeděnková, Ivana; Kobera, Libor; Policianová, Olivia; Šturc, A.

    2013-01-01

    Roč. 102, č. 4 (2013), s. 1235-1248 ISSN 0022-3549 R&D Projects: GA ČR GPP106/11/P426 Institutional support: RVO:61389013 Keywords : trospium chloride * solid state NMR * factor analysis Subject RIV: FR - Pharmacology ; Medidal Chemistry Impact factor: 3.007, year: 2013

  9. CP/MAS ¹³C NMR study of pulp hornification using nanocrystalline cellulose as a model system.

    Science.gov (United States)

    Idström, Alexander; Brelid, Harald; Nydén, Magnus; Nordstierna, Lars

    2013-01-30

    The hornification process of paper pulp was investigated using solid-state (13)C NMR spectroscopy. Nanocrystalline cellulose was used to serve as a model system of the crystalline parts of the fibrils in pulp fibers. Characterization of the nanocrystalline cellulose dimensions was carried out using scanning electron microscopy. The samples were treated by drying and wetting cycles prior to NMR analysis where the hornification phenomenon was recorded by spectral changes of the cellulose C-4 carbon signals. An increase of the crystalline signal and a decrease of the signals corresponding to the accessible amorphous domains were found for both paper pulp and nanocrystalline cellulose. These spectral changes grew stronger with repeating drying and wetting cycles. The results show that cellulose co-crystallization contribute to hornification. Another conclusion is that the surfaces of higher hydrophobicity in cellulose fibrils have an increased preference for aggregation. Copyright © 2012 Elsevier Ltd. All rights reserved.

  10. Acidic properties of SSZ-33 and SSZ-35 novel zeolites: a complex infrared and MAS NMR study

    Czech Academy of Sciences Publication Activity Database

    Gil, B.; Zones, S. I.; Hwang, S.-J.; Voláková, Martina; Čejka, Jiří

    2008-01-01

    Roč. 112, č. 8 (2008), s. 2997-3007 ISSN 1932-7447 R&D Projects: GA ČR GA104/07/0383; GA AV ČR 1QS400400560 Institutional research plan: CEZ:AV0Z40400503 Keywords : nuclear magnetic resonance * adsorbed probe molecules * angle- spinning NMR Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.396, year: 2008

  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. Transitions in Al Coordination during Gibbsite Crystallization Using High-Field 27 Al and 23 Na MAS NMR Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Zhang, Xin [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Jaegers, Nicholas R. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Washington State University, Pullman, Washington 99164, United States; Wan, Chuan [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Graham, Trent R. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Washington State University, Pullman, Washington 99164, United States; Hu, Mary [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Pearce, Carolyn I. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Felmy, Andrew R. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Washington State University, Pullman, Washington 99164, United States; Clark, Sue B. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States; Washington State University, Pullman, Washington 99164, United States; Rosso, Kevin M. [Pacific Northwest National Laboratory, Richland, Washington 99354, United States

    2017-11-30

    Mechanisms of nucleation and growth of Al hydroxides such as gibbsite from aqueous solution, particularly in highly alkaline conditions, remain poorly understood. In this work, quantitative 27Al and 22Na MAS NMR experiments were conducted on solid samples extracted from the crystallization of gibbsite from an amorphous aluminum hydroxide gel precursor. The use of high magnetic field and fast sample spinning allowed transitional tetrahedral (AlT) and pentahedral (AlP) aluminum species to be observed along with the octahedral aluminum (AlO) that dominates the gibbsite product. Low-coordinated Al species could be detected at concentrations as low as 0.1% of the total Al sites. It is established that (a) AlT and AlP coexist on the surface of growing gibbsites even with a combined percentage over the total Al sites of less than 1%; (b) Different synthesis methods generate gibbsite with varying amounts of low-coordinated Al; (c) the amorphous gel precursor contains a significant amount of low-coordinated Al sites with AO: AlP: AlT ratios of approximately 4:2:1; (d) upon hydration, the external, low-coordinated Al sites become six-fold coordinated by interacting with the oxygen in H2O and the 27Al MAS NMR peak position shifts to that for the AlO sites; (e) gibbsite with increased long range order is synthesized over longer times by gradually incorporating residual AlP and AlT sites into octahedrally-coordinated AlO sites; (f) trace Na is predominantly a surface species on gibbsite particles. These findings provide a basis for understanding the gibbsite crystallization mechanism, along with a general means of characterizing gibbsite surface properties that are of equal importance for understanding related processes such as dissolution behavior.

  13. Metallic nature of Sn{sub 1-} {sub x} Sb {sub x} O{sub 2{+-}} {sub {delta}} (x=0.0, 0.10 and 0.20) mixed oxides: Probed by {sup 119}Sn MAS NMR

    Energy Technology Data Exchange (ETDEWEB)

    Jayakumar, O.D. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India)]. E-mail: ddjaya@apsara.barc.ernet.in; Sudarsan, V. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Kulshreshtha, S.K. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India)

    2007-04-15

    Antimony doped SnO{sub 2} samples were prepared by co-precipitation method and characterized by X-ray diffraction (XRD), {sup 119}Sn magic angle spinning nuclear magnetic resonance (MAS NMR) and variable temperature electrical conductivity measurements. Based on {sup 119}Sn MAS NMR measurements on these samples, it was established that only above 400 deg. C, the structural units of antimony and tin interacts, resulting in the metallic nature. Metallic behavior of the high-temperature heated samples was further confirmed by the variable temperature electrical conductivity measurements.

  14. Solubilization and localization of weakly polar lipids in unsonicated egg phosphatidylcholine: A 13C MAS NMR study

    International Nuclear Information System (INIS)

    Hamilton, J.A.; Fujito, D.T.; Hammer, C.F.

    1991-01-01

    The weakly polar lipids cholesteryl ester, triacylglycerol, and diacylglycerol incorporate to a limited extent into the lamellar structure of small unilamellar vesicles. The localization of the carbonyl group(s) at the aqueous interface was detected by [ 13 C]carbonyl chemical shift changes relative to the neat unhydrated lipid. This study uses 13 C NMR to investigate the interactions of thes lipids with unsonicated (multilamellar) phosphatidylcholine, a model system for cellular membranes and surfaces of emulsion particles with low curvature. Magic angle spinning reduced the broad lines of the unsonicated dispersions to narrow lines comparable to those from sonicated dispersions. [ 13 C]Carbonyl chemical shifts revealed incorporation of the three lipids into the lamellar structure of the unsonicated phospholipids and a partial hydration of the carbonyl groups similar to that observed in small vesicles. Other properties of interfacial weakly polar lipids in multilayers were similar to those in small unilamellar bilayers. There is thus a general tendency of weakly polar lipids to incorparate at least to a small extent into the lamellar structure of phospholipids and take on interfacial properties that are distinct from their bulk-phase properties. This pool of surface-located lipid is likely to be directly involved in enzymatyic transformations and protein-mediated transport. The 13 C magic angle spinning NMR method may be generally useful for determining the orientation of molecules in model membranes

  15. Biomolecular solid state NMR with magic-angle spinning at 25K.

    Science.gov (United States)

    Thurber, Kent R; Tycko, Robert

    2008-12-01

    A magic-angle spinning (MAS) probe has been constructed which allows the sample to be cooled with helium, while the MAS bearing and drive gases are nitrogen. The sample can be cooled to 25K using roughly 3 L/h of liquid helium, while the 4-mm diameter rotor spins at 6.7 kHz with good stability (+/-5 Hz) for many hours. Proton decoupling fields up to at least 130 kHz can be applied. This helium-cooled MAS probe enables a variety of one-dimensional and two-dimensional NMR experiments on biomolecular solids and other materials at low temperatures, with signal-to-noise proportional to 1/T. We show examples of low-temperature (13)C NMR data for two biomolecular samples, namely the peptide Abeta(14-23) in the form of amyloid fibrils and the protein HP35 in frozen glycerol/water solution. Issues related to temperature calibration, spin-lattice relaxation at low temperatures, paramagnetic doping of frozen solutions, and (13)C MAS NMR linewidths are discussed.

  16. Efficiency of free-energy calculations of spin lattices by spectral quantum algorithms

    International Nuclear Information System (INIS)

    Master, Cyrus P.; Yamaguchi, Fumiko; Yamamoto, Yoshihisa

    2003-01-01

    Ensemble quantum algorithms are well suited to calculate estimates of the energy spectra for spin-lattice systems. Based on the phase estimation algorithm, these algorithms efficiently estimate discrete Fourier coefficients of the density of states. Their efficiency in calculating the free energy per spin of general spin lattices to bounded error is examined. We find that the number of Fourier components required to bound the error in the free energy due to the broadening of the density of states scales polynomially with the number of spins in the lattice. However, the precision with which the Fourier components must be calculated is found to be an exponential function of the system size

  17. A quantum mechanical alternative to the Arrhenius equation in the interpretation of proton spin-lattice relaxation data for the methyl groups in solids.

    Science.gov (United States)

    Bernatowicz, Piotr; Shkurenko, Aleksander; Osior, Agnieszka; Kamieński, Bohdan; Szymański, Sławomir

    2015-11-21

    The theory of nuclear spin-lattice relaxation in methyl groups in solids has been a recurring problem in nuclear magnetic resonance (NMR) spectroscopy. The current view is that, except for extreme cases of low torsional barriers where special quantum effects are at stake, the relaxation behaviour of the nuclear spins in methyl groups is controlled by thermally activated classical jumps of the methyl group between its three orientations. The temperature effects on the relaxation rates can be modelled by Arrhenius behaviour of the correlation time of the jump process. The entire variety of relaxation effects in protonated methyl groups have recently been given a consistent quantum mechanical explanation not invoking the jump model regardless of the temperature range. It exploits the damped quantum rotation (DQR) theory originally developed to describe NMR line shape effects for hindered methyl groups. In the DQR model, the incoherent dynamics of the methyl group include two quantum rate (i.e., coherence-damping) processes. For proton relaxation only one of these processes is relevant. In this paper, temperature-dependent proton spin-lattice relaxation data for the methyl groups in polycrystalline methyltriphenyl silane and methyltriphenyl germanium, both deuterated in aromatic positions, are reported and interpreted in terms of the DQR model. A comparison with the conventional approach exploiting the phenomenological Arrhenius equation is made. The present observations provide further indications that incoherent motions of molecular moieties in the condensed phase can retain quantum character over much broader temperature range than is commonly thought.

  18. Quantum mechanical alternative to Arrhenius equation in the interpretation of proton spin-lattice relaxation data for the methyl groups in solids

    KAUST Repository

    Bernatowicz, Piotr

    2015-10-01

    Theory of nuclear spin-lattice relaxation in methyl groups in solids has been a recurring problem in nuclear magnetic resonance (NMR) spectroscopy. The current view is that, except for extreme cases of low torsional barriers where special quantum effects are at stake, the relaxation behaviour of the nuclear spins in methyl groups is controlled by thermally activated classical jumps of the methyl group between its three orientations. The temperature effects on the relaxation rates can be modelled by Arrhenius behaviour of the correlation time of the jump process. The entire variety of relaxation effects in protonated methyl groups has recently been given a consistently quantum mechanical explanation not invoking the jump model regardless of the temperature range. It exploits the damped quantum rotation (DQR) theory originally developed to describe NMR line shape effects for hindered methyl groups. In the DQR model, the incoherent dynamics of the methyl group include two quantum rate, i.e., coherence-damping processes. For proton relaxation only one of these processes is relevant. In this paper, temperature-dependent proton spin-lattice relaxation data for the methyl groups in polycrystalline methyltriphenyl silane and methyltriphenyl germanium, both deuterated in aromatic positions, are reported and interpreted in terms of the DQR model. A comparison with the conventional approach exploiting the phenomenological Arrhenius equation is made. The present observations provide further indications that incoherent motions of molecular moieties in condensed phase can retain quantum character over much broad temperature range than is commonly thought.

  19. Analysis of mercerization process based on the intensity change of deconvoluted resonances of 13C CP/MAS NMR: Cellulose mercerized under cooling and non-cooling conditions

    International Nuclear Information System (INIS)

    Miura, Kento; Nakano, Takato

    2015-01-01

    The area intensity change of C1, C4, and C6 in spectrum obtained by 13 C CP/MAS NMR and the mutual relationship between their changes were examined for cellulose samples treated with various concentrations of aqueous NaOH solutions under non-cooling and cooling conditions. The area intensity of C1-up and C6-down changed cooperatively with that of C4-down which corresponds to the crystallinity of samples: “-up” and “-down” are the up- and down- field component in a splitting peak of NMR spectrum, respectively. The intensity change of C1-up starts to decrease with decreasing in that of C4-down after that of C6-down is almost complete. These changes were more clearly observed for samples treated under cooling condition. It can be suggested that their characteristic change relates closely to the change in conformation of cellulose chains by induced decrystallization and the subsequent crystallization of cellulose II, and presumed that their changes at microscopic level relate to the macroscopic morphological changes such as contraction along the length of cellulose chains and recovery along the length. - Highlight: • Samples were mercerized at various NaOH concentrations under non-cooling and cooling. • The intensity change of C1 starts immediately after that of C6 is complete. • The creation of cell-II starts when decrystallization proceeds to a certain state. • This change relates closely to the change in conformation of cellulose chains. • The above change is more clearly found for samples treated under cooling

  20. Spin manipulation and spin-lattice interaction in magnetic colloidal quantum dots

    OpenAIRE

    Moro, F.; Turyanska, L.; Granwehr, J.; Patane, A.

    2014-01-01

    We report on the spin-lattice interaction and coherent manipulation of electron spins in Mn-doped colloidal PbS quantum dots (QDs) by electron spin resonance. We show that the phase memory time,TM, is limited by Mn-Mn dipolar interactions, hyperfine interactions of the protons (H1) on the QD capping ligands with Mn ions in their proximity (

  1. Effects of solvent concentration and composition on protein dynamics: 13C MAS NMR studies of elastin in glycerol-water mixtures.

    Science.gov (United States)

    Demuth, Dominik; Haase, Nils; Malzacher, Daniel; Vogel, Michael

    2015-08-01

    We use (13)C CP MAS NMR to investigate the dependence of elastin dynamics on the concentration and composition of the solvent at various temperatures. For elastin in pure glycerol, line-shape analysis shows that larger-scale fluctuations of the protein backbone require a minimum glycerol concentration of ~0.6 g/g at ambient temperature, while smaller-scale fluctuations are activated at lower solvation levels of ~0.2 g/g. Immersing elastin in various glycerol-water mixtures, we observe at room temperature that the protein mobility is higher for lower glycerol fractions in the solvent and, thus, lower solvent viscosity. When decreasing the temperature, the elastin spectra approach the line shape for the rigid protein at 245 K for all studied samples, indicating that the protein ceases to be mobile on the experimental time scale of ~10(-5) s. Our findings yield evidence for a strong coupling between elastin fluctuations and solvent dynamics and, hence, such interaction is not restricted to the case of protein-water mixtures. Spectral resolution of different carbon species reveals that the protein-solvent couplings can, however, be different for side chain and backbone units. We discuss these results against the background of the slaving model for protein dynamics. Copyright © 2015 Elsevier B.V. All rights reserved.

  2. A MAS NMR and DRIFT study of the Ga species in Ga/H-ZSM5 catalysts and their effect on propane ammoxidation

    Energy Technology Data Exchange (ETDEWEB)

    Pal, P. [Indian Inst. of Petroleum, Dehradun (India). Catalysis Division; Quartararo, J. [Liverpool Univ., Liverpool (United Kingdom). Leverhulme Centre for Innovative Catalysis, Dept. of Chemistry; Abd Hamid, S.B. [Malaya Univ., Postgraduate School, Bangunan (Malaysia); Derouane, E.G. [Algarve Univ., Faro (Portugal). Faculdade de Ciencias e Tecnologia; Vedrine, J.C. [Laboratoire de Physico-Chimie des Surface, Paris (France). Faculdade de Ciencias e Tecnologia; Magusin, P.C.M.M.; Anderson, B.G. [Eindhoven Univ. of Technology, Eindhoven (Netherlands). Schuit Institute of Catalysis

    2005-07-01

    This paper presents the results of a study that sought information about the nature and environment of the gallium (Ga) species in Ga/H-ZSM5 zeolites following H{sub 2}-O{sub 2} redox treatments applied during their activation by use of magic-angle spinning (MAS) {sup 71}Ga, {sup 27}Al, and {sup 29}Si NMR spectroscopy (Ga coordination) complemented by diffuse reflectance FT IR (DRIFT) spectroscopy (Bronsted acidity). This information was then correlated with their catalytic behavior for the ammoxidation of propane. Ga species were observed in several environments: octahedrally coordinated gallium in small Ga{sub 2}O{sub 3} particles at the external surface of the zeolite crystals; octahedrally coordinated gallium in GaO(OH) or related species; and tetrahedrally coordinated gallium in cationic-exchange positions inside the zeolite. Redox (H{sub 2}-O{sub 2}) cycles promote the migration of gallium from the GaO(OH) or Ga{sub 2}O{sub 3} species at the external surface of the zeolite crystals to cationic-exchange sites within the zeolite channels. It was concluded that the redox treatment had a beneficial effect on its catalytic performance for the ammoxidation of propane, which occurs via a bifunctional mechanism. The main product was acetonitrile at high gallium and aluminium contents. It was suggested that higher yields in acrylonitrile could be obtained through Ga-modified zeolites with a higher gallium and lower aluminium content. 22 refs., 1 tab., 6 figs.

  3. Fast MAS 1H NMR Study of Water Adsorption and Dissociation on the (100) Surface of Ceria Nanocubes: A Fully Hydroxylated, Hydrophobic Ceria Surface

    Energy Technology Data Exchange (ETDEWEB)

    Gill, Lance [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division; Beste, Ariana [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Joint Institute for Computational Sciences (JIBS); Univ. of Tennessee, Knoxville, TN (United States); Chen, Banghao [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division; Li, Meijun [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division; Mann, Amanda K. P. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division; Overbury, Steven H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division; Hagaman, Edward W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division

    2017-03-22

    1H nuclear magnetic resonance (NMR) spectroscopy was used to study hydroxylic surface species on ceria nanocubes, a crystalline, high-surface-area CeO2 that presents mostly (100) facets. Water adsorption and desorption experiments in combination with fast magic angle spinning (MAS, 20–40 kHz) 1H NMR provide high-resolution 1H spectra that allow the observation of ten resonance bands (water or hydroxyl) on or under the (100) surface. Assignments were made using a combination of adsorption and temperature-programmed desorption, quantitative spin counting, deuterium exchange, spin–lattice (T1) and spin–spin (T2) relaxation, and DFT calculations. In air, the (100) surface exists as a fully hydroxylated surface. Water adsorption and dissociation on dry ceria surfaces occur first at oxygen vacancies, but Ce3+ centers are not required since water dissociation is barrier-less on the fully oxidized surface. Surface $-$OH functionality occurs in two resolved bands representing isolated $-$OH (1 ppm) and hydrogen-bonded $-$OH (9 ppm), the latter being dominant. Deuterium exchange of surface hydroxyls with D2O does not occur under mild or forcing conditions. Despite large differences in the T1 of surface hydroxyls and physisorbed water, surface hydroxyl T1 values are independent of the presence or absence of physisorbed water, demonstrating that the protons within these two functional group pools are not in intimate contact. These observations show that, once hydroxylated, the surface $-$OH functionality preferentially forms hydrogen bonds with surface lattice oxygen, i.e., the hydroxylated (100) surface of ceria is hydrophobic. Near this surface it is energetically more favorable for physisorbed water to hydrogen bond to itself rather than to the surface. DFT calculations support this notion. Impurity Na+ remaining in incompletely washed ceria nanocubes

  4. Effect of Ge/Si substitutions on the local geometry of Si framework sites in zeolites: A combined high resolutionsup29/supSi MAS NMR and DFT/MM study on zeolite Beta polymorph C (BEC)

    Czech Academy of Sciences Publication Activity Database

    Whittleton, Sarah R.; Vicente, A.; Fernandez, C.; Rastegar, Somayeh F.; Fishchuk, Anna V.; Sklenák, Štěpán

    2018-01-01

    Roč. 267, SEP 2018 (2018), s. 124-133 ISSN 1387-1811 R&D Projects: GA ČR(CZ) GA15-14007S Grant - others:Ga MŠk(CZ) LM2015070 Institutional support: RVO:61388955 Keywords : 29 Si MAS NMR * bec * Ge-zeolites * Germanoaluminosilicates * Zeolite Beta polymorph C Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Physical chemistry Impact factor: 3.615, year: 2016

  5. {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.

  6. Homogeneity characterization of ethylene-co-vinyl acetate copolymer (EVA) and hydrophobic silica nanocomposite by low field NMR

    International Nuclear Information System (INIS)

    Stael, Giovanni Chaves; Tavares, Maria I.B.

    2005-01-01

    This project proposes the characterization of a polymeric matrix composite material using nanometric scale hydrophobic silica as charge element, with the ethylene-vinyl acetate (EVA), by using the spin-lattice relaxation time measurement applying the low field NMR

  7. Measurements of spin-lattice relaxation time in mixed alkali halide crystals

    International Nuclear Information System (INIS)

    Tannus, A.

    1983-01-01

    Using magneto-optic techniques the ground state spin-lattice relaxation times (T1) of 'F' centers in mixed Alkali Halide cristals (KCl-KBr), was studied. A computer assisted system to optically measure short relaxation times (approx. = 1mS), was described. The technique is based on the measurement of the Magnetic Circular Dicroism (MCD) presented by F centers. The T1 magnetic field dependency at 2 K (up to 65 KGauss), was obtained as well as the MCD spectra for different relative concentration at the mixed matrices. The theory developed by Panepucci and Mollenauer for F centers spin-lattice relaxation in pure matrices was modified to explain the behaviour of T1 in mixed cristals. The Direct Process results (T approx. = 2.0 K) compared against that theory shows that the main relaxation mecanism, up to 25 KGauss, continues to be phonon modulation of the hiperfine iteraction between F electrons and surrounding nuclei. (Author) [pt

  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. Nuclear spin-lattice relaxation in nitroxide spin-label EPR.

    Science.gov (United States)

    Marsh, Derek

    2016-11-01

    Nuclear relaxation is a sensitive monitor of rotational dynamics in spin-label EPR. It also contributes competing saturation transfer pathways in T 1 -exchange spectroscopy, and the determination of paramagnetic relaxation enhancement in site-directed spin labelling. A survey shows that the definition of nitrogen nuclear relaxation rate W n commonly used in the CW-EPR literature for 14 N-nitroxyl spin labels is inconsistent with that currently adopted in time-resolved EPR measurements of saturation recovery. Redefinition of the normalised 14 N spin-lattice relaxation rate, b=W n /(2W e ), preserves the expressions used for CW-EPR, whilst rendering them consistent with expressions for saturation recovery rates in pulsed EPR. Furthermore, values routinely quoted for nuclear relaxation times that are deduced from EPR spectral diffusion rates in 14 N-nitroxyl spin labels do not accord with conventional analysis of spin-lattice relaxation in this three-level system. Expressions for CW-saturation EPR with the revised definitions are summarised. Data on nitrogen nuclear spin-lattice relaxation times are compiled according to the three-level scheme for 14 N-relaxation: T 1 n =1/W n . Results are compared and contrasted with those for the two-level 15 N-nitroxide system. Copyright © 2016 Elsevier Inc. All rights reserved.

  10. Concentration dependence of fluorine impurity spin-lattice relaxation rate in bone mineral

    International Nuclear Information System (INIS)

    Code, R.F.; Armstrong, R.L.; Cheng, P.-T.

    1992-01-01

    The concentration dependence of the fluoride ion spin-lattice relaxation rate has been observed by nuclear magnetic resonance experiments on samples of defatted and dried bone. The 19 F spin-lattice relaxation rates increased linearly with bone fluoride concentration. Different results were obtained from trabecular than from cortical bone. For the same macroscopic fluoride content per gram of bone calcium, relaxation rate is significantly faster in cortical bone. Relaxation rates in cortical bone samples prepared from rats and dogs were apparently controlled by the same species-independent processes. For samples from beagle dogs, bulk fluoride concentrations measured by neutron activation analysis were 3.1±0.3 times greater in trabecular bone than in corresponding cortical bone. The beagle spin-lattice relaxation data suggest that microscopic fluoride concentrations in bone mineral were 1.8±0.4 times greater in trabecular bone than in cortical bone. It is concluded that accumulation of fluoride impurities in bone mineral is non-uniform. (author)

  11. Temperature dependence of the NMR spin-lattice relaxation rate for spin-1/2 chains

    Science.gov (United States)

    Coira, E.; Barmettler, P.; Giamarchi, T.; Kollath, C.

    2016-10-01

    We use recent developments in the framework of a time-dependent matrix product state method to compute the nuclear magnetic resonance relaxation rate 1 /T1 for spin-1/2 chains under magnetic field and for different Hamiltonians (XXX, XXZ, isotropically dimerized). We compute numerically the temperature dependence of the 1 /T1 . We consider both gapped and gapless phases, and also the proximity of quantum critical points. At temperatures much lower than the typical exchange energy scale, our results are in excellent agreement with analytical results, such as the ones derived from the Tomonaga-Luttinger liquid (TLL) theory and bosonization, which are valid in this regime. We also cover the regime for which the temperature T is comparable to the exchange coupling. In this case analytical theories are not appropriate, but this regime is relevant for various new compounds with exchange couplings in the range of tens of Kelvin. For the gapped phases, either the fully polarized phase for spin chains or the low-magnetic-field phase for the dimerized systems, we find an exponential decrease in Δ /(kBT ) of the relaxation time and can compute the gap Δ . Close to the quantum critical point our results are in good agreement with the scaling behavior based on the existence of free excitations.

  12. Phosphole complexes of Gold(I) halides: Comparison of solution and solid-state structures by a combination of solution and CP/MAS 31P NMR spectroscopy and x-ray crystallography

    International Nuclear Information System (INIS)

    Attar, S.; Nelson, J.H.; Bearden, W.H.; Alcock, N.W.; Alyea, E.C.

    1990-01-01

    A series of complexes of 1-phenyldibenzophosphole (DBP), 1-phenyl-3,4,-dimethylphosphole (DMPP), and triphenylphosphine of the type L n AuX (n = 1, L = DBP, DMPP, Ph 3 P, X = Cl, Br, I; n = 3, L = DBP, X = Cl, Br, I; n = 3, L = Ph 3 P, X = Cl; n = 4, L = DBP, DMPP, X = PF 6 ) have been prepared and characterized. The structures of (DBP)AuCl (1), (DBP) 3 AuCl (2), and (DMPP)AuCl (3) have been determined from three-dimensional x-ray data collected by counter methods. Crystal structure of the complexes is reported. The CP/MAS 31 P( 1 H) NMR spectrum of complex 1 shows two resonances in a 1:1 intensity ratio, and the CP/MAS 31 P( 1 H) NMR spectrum of complex 3 shows three resonances in a 1:1:1 intensity ratio for reasons that are not yet understood. Though the three phospholes are crystallographically inequivalent (d(AuP) = 2.359 (1), 2.382 (1), and 2.374 (2) angstrom) the molecule has effective C s symmetry as evidenced by the observation of two 31 P resonances in a 2:1 intensity ratio in its CP/MAS 31 P( 1 H) NMR spectrum. Variable-temperature 31 P( 1 H) NMR spectra obtained on solutions of LAuCl + L in various ratios were analyzed to determine the nature of the species present in solution and to gain information regarding their relative stabilities as a function of the nature of the phosphine. 79 refs., 8 figs., 9 tabs

  13. NMR

    International Nuclear Information System (INIS)

    Kneeland, J.B.; Lee, B.C.P.; Whalen, J.P.; Knowles, R.J.R.; Cahill, P.T.

    1984-01-01

    Although still quite new, NMR imaging has already emerged as a safe, noninvasive, painless, and effective diagnostic modality requiring no ionizing radiation. Also, NMR appears already to have established itself as the method of choice for the examination of the brain spinal cord (excluding herniated disks). Another area in which NMR excels is in the examination of the pelvis. The use of surface coils offers the promise of visualizing structures with resolution unobtainable by any other means. In addition, NMR, with its superb visualization of vascular structures and potential ability to measure flow, may soon revolutionize the diagnosis of cardiovascular disease. Finally, NMR, through biochemically and physiologically based T/sub 1/ and T/sub 2/ indices or through spectroscopy, may provide a means of monitoring therapeutic response so as to permit tailoring of treatment to the individual patient. In short, NMR is today probably at the same stage as the x-ray was in Roentgen's day

  14. Analysis of local molecular motions of aromatic sidechains in proteins by 2D and 3D fast MAS NMR spectroscopy and quantum mechanical calculations

    Czech Academy of Sciences Publication Activity Database

    Paluch, P.; Pawlak, T.; Jeziorna, A.; Trébosc, J.; Hou, G.; Vega, A. J.; Amoureux, J. P.; Dračínský, Martin; Polenova, T.; Potrzebowski, M. J.

    2015-01-01

    Roč. 17, č. 43 (2015), s. 28789-28801 ISSN 1463-9076 R&D Projects: GA ČR GA15-11223S Institutional support: RVO:61388963 Keywords : solid-state NMR * angle spinning NMR * NMR Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.449, year: 2015 http://pubs.rsc.org/en/content/articlepdf/2015/cp/c5cp04475h

  15. 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.

  16. Analytic treatment of nuclear spin-lattice relaxation for diffusion in a cone model

    Science.gov (United States)

    Sitnitsky, A. E.

    2011-12-01

    We consider nuclear spin-lattice relaxation rate resulted from a diffusion equation for rotational wobbling in a cone. We show that the widespread point of view that there are no analytical expressions for correlation functions for wobbling in a cone model is invalid and prove that nuclear spin-lattice relaxation in this model is exactly tractable and amenable to full analytical description. The mechanism of relaxation is assumed to be due to dipole-dipole interaction of nuclear spins and is treated within the framework of the standard Bloemberger, Purcell, Pound-Solomon scheme. We consider the general case of arbitrary orientation of the cone axis relative the magnetic field. The BPP-Solomon scheme is shown to remain valid for systems with the distribution of the cone axes depending only on the tilt relative the magnetic field but otherwise being isotropic. We consider the case of random isotropic orientation of cone axes relative the magnetic field taking place in powders. Also we consider the cases of their predominant orientation along or opposite the magnetic field and that of their predominant orientation transverse to the magnetic field which may be relevant for, e.g., liquid crystals. Besides we treat in details the model case of the cone axis directed along the magnetic field. The latter provides direct comparison of the limiting case of our formulas with the textbook formulas for free isotropic rotational diffusion. The dependence of the spin-lattice relaxation rate on the cone half-width yields results similar to those predicted by the model-free approach.

  17. NMR studies of spin dynamics in cuprates

    International Nuclear Information System (INIS)

    Takigawa, M.; Mitzi, D.B.

    1994-01-01

    The authors report recent NMR results in cuprates. The oxygen Knight shift and the Cu nuclear spin-lattice relaxation rate in Bi 2.1 Sr 1.94 Ca 0.88 Cu 2.07 O 8+σ single crystals revealed a gapless superconducting state, which can be most naturally explained by a d-wave pairing state and the intrinsic disorder in this material. The Cu nuclear spin-spin relaxation rate in underdoped YBa 2 Cu 3 O 6.63 shows distinct temperature dependence from the spin-lattice relaxation rate, providing direct evidence for a pseudo spin-gap near the antiferromagnetic wave vector

  18. NMR studies of spin dynamics in cuprates

    Science.gov (United States)

    Takigawa, M.; Mitzi, D. B.

    1994-04-01

    We report recent NMR results in cuprates. The oxygen Knight shift and the Cu nuclear spin-lattice relaxation rate in Bi2.1Sr1.94Ca0.88Cu2.07O8+δ single crystals revealed a gapless superconducting state, which can be most naturally explained by a d-wave pairing state and the intrinsic disorder in this material. The Cu nuclear spin-spin relaxation rate in underdoped YBa2Cu3O6.63 shows distinct temperature dependence from the spin-lattice relaxation rate, providing direct evidence for a pseudo spin-gap near the antiferromagnetic wave vector.

  19. Magnon and phonon dispersion, lifetime, and thermal conductivity of iron from spin-lattice dynamics simulations

    Science.gov (United States)

    Wu, Xufei; Liu, Zeyu; Luo, Tengfei

    2018-02-01

    In recent years, the fundamental physics of spin-lattice (e.g., magnon-phonon) interaction has attracted significant experimental and theoretical interests given its potential paradigm-shifting impacts in areas like spin-thermoelectrics, spin-caloritronics, and spintronics. Modelling studies of the transport of magnons and phonons in magnetic crystals are very rare. In this paper, we use spin-lattice dynamics (SLD) simulations to model ferromagnetic crystalline iron, where the spin and lattice systems are coupled through the atomic position-dependent exchange function, and thus the interaction between magnons and phonons is naturally considered. We then present a method combining SLD simulations with spectral energy analysis to calculate the magnon and phonon harmonic (e.g., dispersion, specific heat, and group velocity) and anharmonic (e.g., scattering rate) properties, based on which their thermal conductivity values are calculated. This work represents an example of using SLD simulations to understand the transport properties involving coupled magnon and phonon dynamics.

  20. Microwave Amplitude Modulation Technique to Measure Spin-Lattice (T 1) and Spin-Spin (T 2) Relaxation Times

    Science.gov (United States)

    Misra, Sushil K.

    The measurement of very short spin-lattice, or longitudinal, relaxation (SLR) times (i.e., 10-10 Misra, 1998), and polymer resins doped with rare-earth ions (Pescia et al., 1999a; Pescia et al. 1999b). The ability to measure such fast SLR data on amorphous Si and copper-chromium-tin spinel led to an understanding of the role of exchange interaction in affecting spin-lattice relaxation, while the data on polymer resins doped with rare-earth ions provided evidence of spin-fracton relaxation (Pescia et al., 1999a, b). But such fast SLR times are not measurable by the most commonly used techniques of saturation- and inversion-recovery (Poole, 1982; Alger, 1968), which only measure spin-lattice relaxation times longer than 10-6 s. A summary of relevant experimental data is presented in Table 1.

  1. A study of the adsorption activities of silanol surface structures on a fused silica model substrate by combining 29Si CP MAS NMR and inverse gas chromatographic data

    NARCIS (Netherlands)

    Scholten, A.B.; Janssen, J.G.M.; Haan, de J.W.; Cramers, C.A.

    1994-01-01

    The possibilities of inverse gas-solid chromatog. (IGC) in obtaining chromatog. data on fumed silica were examd. Aerosil A-200, a fused silica model substrate in 29Si NMR anal., was trimethylsilylated to different degrees. IGC was used to vary reproducibly det. the free specific energies of

  2. Parallel computer calculation of quantum spin lattices; Calcul de chaines de spins quantiques sur ordinateur parallele

    Energy Technology Data Exchange (ETDEWEB)

    Lamarcq, J. [Service de Physique Theorique, CEA Centre d`Etudes de Saclay, 91 - Gif-sur-Yvette (France)

    1998-07-10

    Numerical simulation allows the theorists to convince themselves about the validity of the models they use. Particularly by simulating the spin lattices one can judge about the validity of a conjecture. Simulating a system defined by a large number of degrees of freedom requires highly sophisticated machines. This study deals with modelling the magnetic interactions between the ions of a crystal. Many exact results have been found for spin 1/2 systems but not for systems of other spins for which many simulation have been carried out. The interest for simulations has been renewed by the Haldane`s conjecture stipulating the existence of a energy gap between the ground state and the first excited states of a spin 1 lattice. The existence of this gap has been experimentally demonstrated. This report contains the following four chapters: 1. Spin systems; 2. Calculation of eigenvalues; 3. Programming; 4. Parallel calculation 14 refs., 6 figs.

  3. Spin-lattice interactions studied by polarised and unpolarised inelastic scattering application to the invar problem

    Energy Technology Data Exchange (ETDEWEB)

    Brown, P J [Institut Max von Laue - Paul Langevin (ILL), 38 - Grenoble (France)

    1996-11-01

    A semi-quantitative analysis is given of some of the ways in which spin-lattice interactions can modify the cross-sections observable in neutron scattering experiments. This analysis is applied to the scattering from the invar alloy Fe{sub 65}Ni{sub 35} using a model in which the magnetic moment is a function of the near neighbour separation. This model has been applied to clarify the results of inelastic scattering experiments carried out on Fe{sub 65}Ni{sub 35} using both polarised and unpolarised neutrons. The extra information obtainable using polarised neutrons as well as the difficulties and limitations of the technique for inelastic scattering are discussed. (author) 8 figs., 14 refs.

  4. Spin-lattice dynamics simulation of external field effect on magnetic order of ferromagnetic iron

    Directory of Open Access Journals (Sweden)

    C. P. Chui

    2014-03-01

    Full Text Available Modeling of field-induced magnetization in ferromagnetic materials has been an active topic in the last dozen years, yet a dynamic treatment of distance-dependent exchange integral has been lacking. In view of that, we employ spin-lattice dynamics (SLD simulations to study the external field effect on magnetic order of ferromagnetic iron. Our results show that an external field can increase the inflection point of the temperature. Also the model provides a better description of the effect of spin correlation in response to an external field than the mean-field theory. An external field has a more prominent effect on the long range magnetic order than on the short range counterpart. Furthermore, an external field allows the magnon dispersion curves and the uniform precession modes to exhibit magnetic order variation from their temperature dependence.

  5. Spin manipulation and spin-lattice interaction in magnetic colloidal quantum dots

    Science.gov (United States)

    Moro, Fabrizio; Turyanska, Lyudmila; Granwehr, Josef; Patanè, Amalia

    2014-11-01

    We report on the spin-lattice interaction and coherent manipulation of electron spins in Mn-doped colloidal PbS quantum dots (QDs) by electron spin resonance. We show that the phase memory time,TM , is limited by Mn-Mn dipolar interactions, hyperfine interactions of the protons (1H) on the QD capping ligands with Mn ions in their proximity (limit and at low temperature, we achieve a long phase memory time constant TM˜0.9 μ s , thus enabling the observation of Rabi oscillations. Our findings suggest routes to the rational design of magnetic colloidal QDs with phase memory times exceeding the current limits of relevance for the implementation of QDs as qubits in quantum information processing.

  6. Nonuniversal scaling of the magnetocaloric effect as an insight into spin-lattice interactions in manganites

    DEFF Research Database (Denmark)

    Smith, Anders; Nielsen, Kaspar Kirstein; Neves Bez, Henrique

    2016-01-01

    is not given uniquely by the critical exponents of the ferromagnetic-paramagnetic phase transition, i.e., the scaling is nonuniversal. A theoretical description based on the Bean-Rodbell model and taking into account compositional inhomogeneities is shown to be able to account for the observed field dependence....... In this way the determination of the nonuniversal field dependence of the magnetocaloric effect close to a phase transition can be used as a method to gain insight into the strength of the spin-lattice interactions of magnetic materials. The approach is shown also to be applicable to first-order transitions.......We measure the magnetocaloric effect of the manganite series La0.67Ca0.33-xSrxMnO3 by determining the isothermal entropy change upon magnetization, using variable-field calorimetry. The results demonstrate that the field dependence of the magnetocaloric effect close to the critical temperature...

  7. Combined use of EPR and 23Na MAS NMR spectroscopy for assessing the properties of the mixed cobalt-nickel-manganese layers of P3-NayCo1-2xNixMnxO2.

    Science.gov (United States)

    Kalapsazova, M; Ivanova, S; Kukeva, R; Simova, S; Wegner, S; Zhecheva, E; Stoyanova, R

    2017-10-11

    Knowledge on the formation of mixed transition metal layers on lithium and sodium transition metal oxides, Li/Na(Co,Ni,Mn,)O 2 , determines the ability to control their electrochemical properties as electrode materials in alkaline ion batteries. Taking this into account, herein we combine the EPR and 23 Na MAS NMR spectroscopic techniques to gain insights into the structural peculiarities of the mixed cobalt-nickel-manganese layers of Na y Co 1-2x Ni x Mn x O 2 with a three-layer stacking (P3-type) structure. Two types of compositions are examined where diamagnetic Co 3+ and paramagnetic Ni 3+ and Mn 4+ are stabilized: Na 2/3 Co 1/3 Ni 1/3 Mn 1/3 O 2 and Na 1/2 Ni 1/2 Mn 1/2 O 2 . EPR spectroscopy operating in the X- and Q-band region is applied with an aim to improve the spectra resolution and, on the other hand, to provide straightforward information on the coordination of the transition metal ions inside the layers. The analysis of EPR spectra is based on the reference for the Mn 4+ and Ni 2+ ions occurring simultaneously in oxides with two layer stacking, P2-Na 2/3 Ni 1/3 Mn 2/3 O 2 . Complementary to EPR, 23 Na MAS NMR spectroscopy at high spinning rates is undertaken to assess the local structure of the Na nucleus in the layered P3-Na y Co 1-2x Ni x Mn x O 2 oxides. All results are discussed taking into account the EPR and NMR data for the well-known lithium analogues O3-LiCo 1/3 Ni 1/3 Mn 1/3 O 2 and O3-LiNi 1/2 Mn 1/2 O 2 . Finally, the structure peculiarities of the transition metal layers extracted from the EPR and NMR methods are demonstrated by electrochemical intercalation of Li + ions into P3-Na y Co 1-2x Ni x Mn x O 2 .

  8. Homogeneity characterization of ethylene-co-vinyl acetate copolymer (EVA) and hydrophobic silica nanocomposite by low field NMR; Caracterizacao da homogeneidade de nanocomposito do copolimero etileno acetato de vinila (EVA) e silica hidrofobica atraves de ressonancia magnetica nuclear de baixo campo

    Energy Technology Data Exchange (ETDEWEB)

    Stael, Giovanni Chaves [Observatorio Nacional, Rio de Janeiro, RJ (Brazil). Dept. de Geofisica (DGE); Tavares, Maria I.B. [Universidade Federal do Rio de Janeiro, RJ (Brazil). Inst. de Macromoleculas

    2005-07-01

    This project proposes the characterization of a polymeric matrix composite material using nanometric scale hydrophobic silica as charge element, with the ethylene-vinyl acetate (EVA), by using the spin-lattice relaxation time measurement applying the low field NMR.

  9. Proton NMR study of α-MnH 0.06

    Science.gov (United States)

    Soloninin, A. V.; Skripov, A. V.; Buzlukov, A. L.; Antonov, V. E.; Antonova, T. E.

    2004-07-01

    Proton nuclear magnetic resonance (NMR) spectra and spin-lattice relaxation rates for the solid solution α-MnH 0.06 have been measured over the temperature range 11-297 K and the resonance frequency range 20-90 MHz. A considerable shift and broadening of the proton NMR line and a sharp peak of the spin-lattice relaxation rate are observed near 130 K. These effects are attributed to the onset of antiferromagnetic ordering below the Néel temperature TN≈130 K. The proton NMR line does not disappear in the antiferromagnetic phase; this suggests a small magnitude of the local magnetic fields at H-sites in α-MnH 0.06. The spin-lattice relaxation rate in the paramagnetic phase is dominated by the effects of spin fluctuations.

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

    International Nuclear Information System (INIS)

    Bellstedt, Peter; Herbst, Christian; Häfner, Sabine; Leppert, Jörg; Görlach, Matthias; Ramachandran, Ramadurai

    2012-01-01

    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′C and 3D C′NCA with sequential 13 C acquisitions, 3D NHH and 3D NC′H with sequential 1 H acquisitions and 3D CANH and 3D C’NH with broadband 13 C– 15 N mixing are demonstrated using microcrystalline samples of the β1 immunoglobulin binding domain of protein G (GB1) and the chicken α-spectrin SH3 domain.

  11. Design of high-power, broadband 180o pulses and mixing sequences for fast MAS solid state chemical shift correlation NMR spectroscopy

    International Nuclear Information System (INIS)

    Herbst, Christian; Herbst, Jirada; Kirschstein, Anika; Leppert, Joerg; Ohlenschlaeger, Oliver; Goerlach, Matthias; Ramachandran, Ramadurai

    2009-01-01

    An approach for the design of high-power, broadband 180 o pulses and mixing sequences for generating dipolar and scalar coupling mediated 13 C- 13 C chemical shift correlation spectra of isotopically labelled biological systems at fast magic-angle spinning frequencies without 1 H decoupling during mixing is presented. Considering RF field strengths in the range of 100-120 kHz, as typically available in MAS probes employed at high spinning speeds, and limited B 1 field inhomogeneities, the Fourier coefficients defining the phase modulation profile of the RF pulses were optimised numerically to obtain broadband inversion and refocussing pulses and mixing sequences. Experimental measurements were carried out to assess the performance characteristics of the mixing sequences reported here

  12. 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.

  13. Fluorine dynamics in BaF2 superionic conductors investigated by NMR

    International Nuclear Information System (INIS)

    Gumann, Patryk

    2008-01-01

    In this work the dynamics of fluorine in solid-state electrolytes having BaF 2 -structure was investigated using three different NMR-methods: field cycling relaxometry, lineshape analysis, and static field gradient NMR. For this purpose a pure BaF 2 crystal, as well as crystals doped with trivalent impurities (LaF 3 ), were studied as a function of temperature. Using MAS NMR it was possible to identify two lines in Ba 0.9 La 0.1 F 2.1 having different chemical shift, and to refer them to the modified crystal structure. On this basis a model for the fluorine lineshape has been developed, taking into account three motional processes characterized by their correlation times. It includes jump diffusion of the fluorine ions among equivalent sites within two crystallographically distinct sublattices, and inter-lattice exchange processes. By measuring frequency and temperature-dependent spin lattice relaxation times, it was possible to gain information about fluorine dynamics on microscopic length scales. An attempt was also made to analyze the data for pure BaF 2 and low admixture concentration samples with a non-exponential correlation function. (orig.)

  14. Fluorine dynamics in BaF{sub 2} superionic conductors investigated by NMR

    Energy Technology Data Exchange (ETDEWEB)

    Gumann, Patryk

    2008-07-01

    In this work the dynamics of fluorine in solid-state electrolytes having BaF{sub 2}-structure was investigated using three different NMR-methods: field cycling relaxometry, lineshape analysis, and static field gradient NMR. For this purpose a pure BaF{sub 2} crystal, as well as crystals doped with trivalent impurities (LaF{sub 3}), were studied as a function of temperature. Using MAS NMR it was possible to identify two lines in Ba{sub 0.9}La{sub 0.1}F{sub 2.1} having different chemical shift, and to refer them to the modified crystal structure. On this basis a model for the fluorine lineshape has been developed, taking into account three motional processes characterized by their correlation times. It includes jump diffusion of the fluorine ions among equivalent sites within two crystallographically distinct sublattices, and inter-lattice exchange processes. By measuring frequency and temperature-dependent spin lattice relaxation times, it was possible to gain information about fluorine dynamics on microscopic length scales. An attempt was also made to analyze the data for pure BaF{sub 2} and low admixture concentration samples with a non-exponential correlation function. (orig.)

  15. Solid state {sup 1}H spin-lattice relaxation and isolated-molecule and cluster electronic structure calculations in organic molecular solids: The relationship between structure and methyl group and t-butyl group rotation

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xianlong, E-mail: WangXianlong@uestc.edu.cn, E-mail: pbeckman@brynmawr.edu [Key Laboratory for NeuroInformation of Ministry of Education, School of Life Science and Technology, University of Electronic Science and Technology of China, 4 North Jianshe Rd., 2nd Section, Chengdu 610054 (China); Mallory, Frank B. [Department of Chemistry, Bryn Mawr College, 101 North Merion Ave., Bryn Mawr, Pennsylvania 19010-2899 (United States); Mallory, Clelia W. [Department of Chemistry, Bryn Mawr College, 101 North Merion Ave., Bryn Mawr, Pennsylvania 19010-2899 (United States); Department of Chemistry, University of Pennsylvania, Philadelphia, Pennsylvania 19104-6323 (United States); Odhner, Hosanna R.; Beckmann, Peter A., E-mail: WangXianlong@uestc.edu.cn, E-mail: pbeckman@brynmawr.edu [Department of Physics, Bryn Mawr College, 101 North Merion Ave., Bryn Mawr, Pennsylvania 19010-2899 (United States)

    2014-05-21

    We report ab initio density functional theory electronic structure calculations of rotational barriers for t-butyl groups and their constituent methyl groups both in the isolated molecules and in central molecules in clusters built from the X-ray structure in four t-butyl aromatic compounds. The X-ray structures have been reported previously. We also report and interpret the temperature dependence of the solid state {sup 1}H nuclear magnetic resonance spin-lattice relaxation rate at 8.50, 22.5, and 53.0 MHz in one of the four compounds. Such experiments for the other three have been reported previously. We compare the computed barriers for methyl group and t-butyl group rotation in a central target molecule in the cluster with the activation energies determined from fitting the {sup 1}H NMR spin-lattice relaxation data. We formulate a dynamical model for the superposition of t-butyl group rotation and the rotation of the t-butyl group's constituent methyl groups. The four compounds are 2,7-di-t-butylpyrene, 1,4-di-t-butylbenzene, 2,6-di-t-butylnaphthalene, and 3-t-butylchrysene. We comment on the unusual ground state orientation of the t-butyl groups in the crystal of the pyrene and we comment on the unusually high rotational barrier of these t-butyl groups.

  16. Structural, (197)Au Mössbauer and solid state (31)P CP/MAS NMR studies on bis (cis-bis(diphenylphosphino)ethylene) gold(I) complexes [Au(dppey)(2)]X for X = PF(6), I.

    Science.gov (United States)

    Healy, Peter C; Loughrey, Bradley T; Bowmaker, Graham A; Hanna, John V

    2008-07-28

    (197)Au Mössbauer spectra for the d(10) gold(i) phosphine complexes, [Au(dppey)(2)]X (X = PF(6), I; dppey = (cis-bis(diphenylphosphino)ethylene), and the single crystal X-ray structure and solid state (31)P CPMAS NMR spectrum of [Au(dppey)(2)]I are reported here. In [Au(dppey)(2)]I the AuP(4) coordination geometry is distorted from the approximately D(2) symmetry observed for the PF(6)(-) complex with Au-P bond lengths 2.380(2)-2.426(2) A and inter-ligand P-Au-P angles 110.63(5)-137.71(8) degrees . Quadrupole splitting parameters derived from the Mössbauer spectra are consistent with the increased distortion of the AuP(4) coordination sphere with values of 1.22 and 1.46 mm s(-1) for the PF(6)(-) and I(-) complexes respectively. In the solid state (31)P CP MAS NMR spectrum of [Au(dppey)(2)]I, signals for each of the four crystallographically independent phosphorus nuclei are observed, with the magnitude of the (197)Au quadrupole coupling being sufficiently large to produce a collapse of (1)J(Au-P) splitting from quartets to doublets. The results highlight the important role played by the counter anion in the determination of the structural and spectroscopic properties of these sterically crowded d(10) complexes.

  17. 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.

  18. Xenon-Water Interaction in Bacterial Suspensions as Studied by NMR

    DEFF Research Database (Denmark)

    Rodin, V.; Ponomarev, Alexander; Gerasimov, Maxim

    2017-01-01

    suspensions of Escherichia coli in the presence of xenon using nuclear magnetic resonance (NMR). The work studied how the spin-lattice relaxation times of water protons in suspension change under xenon conditions. Xenon is able to form clathrate hydrates with water molecules at a temperature above the melting...... point of ice. The work studied NMR relaxation times which reflect the rotation freedom of water molecules in suspension. Lower relaxation times indicate reduced rotational freedom of water. Single exponential behavior of spin-lattice relaxation of protons in the suspensions of microorganisms has been...

  19. Nonlinear nano-scale localized breather modes in a discrete weak ferromagnetic spin lattice

    International Nuclear Information System (INIS)

    Kavitha, L.; Parasuraman, E.; Gopi, D.; Prabhu, A.; Vicencio, Rodrigo A.

    2016-01-01

    We investigate the propagation dynamics of highly localized discrete breather modes in a weak ferromagnetic spin lattice with on-site easy axis anisotropy due to crystal field effect. We derive the discrete nonlinear equation of motion by employing boson mappings and p-representation. We explore the onset of modulational instability both analytically in the framework of linear stability analysis and numerically by means of molecular dynamics (MD) simulations, and a perfect agreement was demonstrated. It is also explored that how the antisymmetric nature of the canted ferromagnetic lattice supports highly localized discrete breather (DBs) modes as shown in the stability/instability windows. The energy exchange between low amplitude discrete breathers favours the growth of higher amplitude DBs, resulting eventually in the formation of few long-lived high amplitude DBs. - Highlights: • The effects of DM and anisotropy interaction on the DB modes are studied. • The antisymmetric nature of the canted ferromagnetic medium supports the DB modes. • Dynamics of ferromagnetic chain is governed by boson mappings and p-representation.

  20. 31P spin-lattice relaxation time measurements in biological systems

    International Nuclear Information System (INIS)

    Suzuki, Eiji; Maeda, Munehiro; Kuki, Satoru; Tsukamoto, Kenji; Kawakami, Tsuyoshi; Seo, Yoshiteru; Murakami, Masataka; Watari, Hiroshi

    1989-01-01

    Spin-lattice relaxation time (T 1 ) of phosphorus compounds in the perfused heart, liver, kidney and erythrocytes of rats were measured by the DESPOT (Driven-equilibrium single-pulse observation of T 1 ) method at 8.45 T. This method is a rapid and accurate technique for the measurement of T 1 values. T 1 values of phosphomonoesters (PME), 2, 3-diphosphoglycerate (DPG), inorganic phosphate (Pi), phosphodiesters (PDE), phosphocreatine (PCr) and three phosphates of ATP were ranged from 0.15±0.02 sec (β-ATP in the liver) to 8.5±1.6 sec (PDE in the kidney). T 1 value of β-ATP in the liver was 1/4-1/5 of those in the mandibular gland, heart, erythrocytes and kidney. T 1 values obtained from biological materials are useful for selecting the optimal pulse repetition times and pulse angles to maximize the signal-to-noise ratio of 13 P spectra, and for correcting distortions of signal intensities in the spectra. (author)

  1. Dynamic Spin-Lattice Coupling and Nematic Fluctuations in NaFeAs

    Directory of Open Access Journals (Sweden)

    Yu Li

    2018-06-01

    Full Text Available We use inelastic neutron scattering to study acoustic phonons and spin excitations in single crystals of NaFeAs, a parent compound of iron-pnictide superconductors. NaFeAs exhibits a tetragonal-to-orthorhombic structural transition at T_{s}≈58  K and a collinear antiferromagnetic order at T_{N}≈45  K. While longitudinal and out-of-plane transverse acoustic phonons behave as expected, the in-plane transverse acoustic phonons reveal considerable softening on cooling to T_{s} and then harden on approaching T_{N} before saturating below T_{N}. In addition, we find that spin-spin correlation lengths of low-energy magnetic excitations within the FeAs layer and along the c axis increase dramatically below T_{s} and show a weak anomaly across T_{N}. These results suggest that the electronic nematic phase present in the paramagnetic tetragonal phase is closely associated with dynamic spin-lattice coupling, possibly arising from the one-phonon–two-magnon mechanism.

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

    Energy Technology Data Exchange (ETDEWEB)

    Tan, Kong Ooi; Meier, Beat H., E-mail: beme@ethz.ch, E-mail: maer@ethz.ch; Ernst, Matthias, E-mail: beme@ethz.ch, E-mail: maer@ethz.ch [Physical Chemistry, ETH Zürich, Vladimir-Prelog-Weg 2, 8093 Zürich (Switzerland); Agarwal, Vipin [Physical Chemistry, ETH Zürich, Vladimir-Prelog-Weg 2, 8093 Zürich (Switzerland); TIFR Centre for Interdisciplinary Sciences, 21 Brundavan Colony, Narsinghi, Hyderabad 500 075 (India)

    2016-09-07

    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.

  3. 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

    2016-09-07

    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.

  4. {sup 2}H NMR study of phase transition and hydrogen dynamics in hydrogen bonded organic antiferroelectric 55DMBP-H{sub 2}ca

    Energy Technology Data Exchange (ETDEWEB)

    Asaji, Tetsuo, E-mail: asaji@chs.nihon-u.ac.jp; Hara, Masamichi; Fujimori, Hiroki [Nihon University, Department of Chemistry, College of Humanities and Sciences (Japan); Hagiwara, Shoko [Nihon University, Department of Chemistry, Graduate School of Integrated Basic Sciences (Japan)

    2016-12-15

    Hydrogen dynamics in one-dimensional hydrogen bonded organic antiferroelectric, co-crystal of 5,5’-dimethyl-2,2’-bipyridine (55DMBP) and chloranilic acid (H{sub 2}ca), was investigated by use of {sup 2}H high resolution solid-state NMR. The two types of hydrogen bonds O-H …N and N{sup +}-H …O{sup −} in the antiferroelectric phase were clearly observed as the splitting of the side band of the {sup 2}H MAS NMR spectra of the acid-proton deuterated compound 55DMBP-D {sub 2}ca. The temperature dependence of the spin-lattice relaxation time was measured of the N{sup +}-H and O-H deuterons, respectively. It was suggested that the motion of the O-H deuteron is already in the antiferroelectric phase in the fast-motion regime in the NMR time scale, while that of the N{sup +}-H deuteron is a slow motion. In the high-temperature paraelectric phase, the both deuterons become equivalent and the fast motion of the deuterons in the NMR time scale is taking place with the activation energy of 7.9 kJ mol{sup −1}.

  5. Introduction to some basic aspects of NMR

    International Nuclear Information System (INIS)

    Goldman, M.

    1992-01-01

    The principal interactions are reviewed that are experienced by nuclear spins making magnetic resonance feasible and which disturb it in a way that gives access to the properties of bulk matter. The interactions leading to NMR include Zeeman interaction, dipole-dipole interactions, and exchange interactions. Spin-lattice relaxation relevant to NMR is revisited next. It is followed by an overview of spin temperature. Finally, the care of periodic Hamiltonian is discussed in detail as another contribution to NMR. (R.P.) 48 refs., 12 figs

  6. NMR study of LaPb2

    International Nuclear Information System (INIS)

    Ueda, K.; Kohara, T.; Yamada, Y.

    1995-01-01

    La and Pb NMR signals were observed in LaPb 2 with a superconducting transition temperature of about 7 K. The width of the Pb NMR spectrum with an asymmetric line shape was rather narrower than those of Er-, Gd- and Ho-Pb 2 . The spin-lattice relaxation time of Pb nuclei was twice longer than that of Pb metal. La NMR spectrum had satellites due to the electric quadrupole interaction. These results show that each local environment at La or Pb site in LaPb 2 compound is uniquely determined, compared with those in randomly substituted alloys. ((orig.))

  7. Analysis of mercerization process based on the intensity change of deconvoluted resonances of {sup 13}C CP/MAS NMR: Cellulose mercerized under cooling and non-cooling conditions

    Energy Technology Data Exchange (ETDEWEB)

    Miura, Kento [Mitsubishi Rayon Co., Ltd. Otake Research Laboratories (Japan); Nakano, Takato, E-mail: tnakano@kais.kyoto-u.ac.jp [Laboratory of Biomaterials Design, Division of Forest and Biomaterials Science, Graduate School of Agriculture, Kyoto University (Japan)

    2015-08-01

    The area intensity change of C1, C4, and C6 in spectrum obtained by {sup 13}C CP/MAS NMR and the mutual relationship between their changes were examined for cellulose samples treated with various concentrations of aqueous NaOH solutions under non-cooling and cooling conditions. The area intensity of C1-up and C6-down changed cooperatively with that of C4-down which corresponds to the crystallinity of samples: “-up” and “-down” are the up- and down- field component in a splitting peak of NMR spectrum, respectively. The intensity change of C1-up starts to decrease with decreasing in that of C4-down after that of C6-down is almost complete. These changes were more clearly observed for samples treated under cooling condition. It can be suggested that their characteristic change relates closely to the change in conformation of cellulose chains by induced decrystallization and the subsequent crystallization of cellulose II, and presumed that their changes at microscopic level relate to the macroscopic morphological changes such as contraction along the length of cellulose chains and recovery along the length. - Highlight: • Samples were mercerized at various NaOH concentrations under non-cooling and cooling. • The intensity change of C1 starts immediately after that of C6 is complete. • The creation of cell-II starts when decrystallization proceeds to a certain state. • This change relates closely to the change in conformation of cellulose chains. • The above change is more clearly found for samples treated under cooling.

  8. Spin Diffusion and Spin Lattice Relaxation of Dipolar Order in Solids Containing Paramagnetic Impurities

    International Nuclear Information System (INIS)

    Furman, G.B.; Panich, A.M.; Goren, S.D.

    1998-01-01

    The phenomena of spin diffusion and spin lattice relaxation of nuclear dipolar order in solids containing paramagnetic impurities (PI) is considered. We show that at the beginning of the relaxation process the diffusion vanishing regime realizes with non-exponential time dependence, R(t) ∼ exp [- (t/T 1d ) α ], where T 1d ∼ C p -1/α , C p is PI's concentration. For a homogeneous distribution of Pis and nuclear spins, α=Q/6, where Q is the sample dimensionality; for an inhomogeneous distribution, the sample is divided into q-dimensional subsystems, each containing one PI, yield- ing α= (Q + q) /6. This result coincides with experimental data for CaF 2 doped with 0.8 - 10 -3 ωt % of Mn 2+ , where the non-exponential decay of the dipolar signal with α= 0.83 has been observed [3]. Fitting the experimental data yields a good agreement with T 1d = 66 ms . For another independent check of the obtained results we use dependence of the relaxation time on impurities concentration. In accordance that 1/α=1.2 , we have T 1d ∼ C p -1 '. 2 . Exactly this dependence on impurity concentration of the relaxation time has been found in the experiment. Then the relaxation regime starts as a non-exponential time dependent, proceed asymptotically to an to an exponential function of time, to so called diffusion limited relaxation regime with relaxation time T 1d D is inversely depends on impurities concentration. This kind of relaxation behavior of the dipolar order takes place in the experiment [2]. Using experimental results [2] from this two regime we can estimate the diffusion coefficient of the nuclear dipolar order in CaF 2 , which gives for typical values of impurity concentration C p ∼ 10 18 cm 3 the diffusion coefficient of dipolar order in the interval D ∼ 10 -11 -i- 10 -12 cm 2 /sec which is coincide to the case of Zeeman energy spin diffusion

  9. Electron spin-lattice relaxation of low-symmetry Ni.sup.2+./sup. centers in LiF

    Czech Academy of Sciences Publication Activity Database

    Azamat, Dmitry; Badalyan, A. G.; Dejneka, Alexandr; Jastrabík, Lubomír; Lančok, Ján

    2014-01-01

    Roč. 104, č. 25 (2014), "252902-1"-"252902-4" ISSN 0003-6951 R&D Projects: GA MŠk(CZ) LM2011029; GA TA ČR TA01010517; GA ČR GAP108/12/1941 Grant - others:SAFMAT(XE) CZ.2.16/3.1.00/22132 Institutional support: RVO:68378271 Keywords : Ni 2+ centers * LiF single crystals * electron spin-lattice relaxation * electron spin echo technique Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 3.302, year: 2014

  10. Carbon-13 spin lattice relaxation and photoelectron spectroscopy of some aromatic sulphides and sulphones

    International Nuclear Information System (INIS)

    Mellink, W.A.

    1978-01-01

    Carbon-13 NMR spectroscopy and photoelectron spectroscopy have been used to study the electronic structure of symmetric dithienothiophenes and corresponding sulphones. The physical data obtained from both spectroscopic techniques have been interpreted with the aid of quantum mechanical calculations. (Auth.)

  11. Local electronic structure of TM-based alloys: a pulsed NMR study

    International Nuclear Information System (INIS)

    Guerra, D.A.

    1984-01-01

    A pulsed NMR study on several transition metal + metalloid amorphous alloys is reported. The analisis of Knight shifts and nuclear spin-lattice relaxation of metalloids indicates a dominant contribution of p-electrons in the Fermi level density of state, supporting the existence of a p-d hibridization. (author) [pt

  12. 1H NMR relaxometry in the TGBA* and TGBC*phases

    Czech Academy of Sciences Publication Activity Database

    Domenici, V.; Gradišek, A.; Apih, T.; Hamplová, Věra; Novotná, Vladimíra; Sebastião, P.J.

    2016-01-01

    Roč. 49, č. 1 (2016), 17-27 ISSN 0015-0193 Grant - others:AVČR(CZ) M100101204 Institutional support: RVO:68378271 Keywords : Ferroelectric liquid crystal * chiral liquid crystals * molecular dynamics * NMR * twist grain boundary phases * spin-lattice Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.551, year: 2016

  13. Heteronuclear 2D (1H-13C) MAS NMR Resolves the Electronic Structure of Coordinated Histidines in Light-Harvesting Complex II: Assessment of Charge Transfer and Electronic Delocalization Effect

    International Nuclear Information System (INIS)

    Matysik, Joerg; Boer, Ido de; Gast, Peter; Gorkom, Hans J. van; Groot, Huub J.M. de

    2004-01-01

    In a recent MAS NMR study, two types of histidine residues in the light-harvesting complex II (LH2) of Rhodopseudomonas acidophila were resolved: Type 1 (neutral) and Type 2 (positively charged) (Alia et al. J. Am. Chem. Soc.). The isotropic 13 C shifts of histidines coordinating to B850 BChl a are similar to fully positively charged histidine, while the 15 N shift anisotropy shows a predominantly neutral character. In addition the possibility that the ring currents are quenched by overlap in the superstructure of the complete ring of 18 B850 molecules in the LH2 complex could not be excluded. In the present work, by using two-dimensional heteronuclear ( 1 H- 13 C) dipolar correlation spectroscopy with phase-modulated Lee-Goldburg homonuclear 1 H decoupling applied during the t 1 period, a clear and unambiguous assignment of the protons of histidine interacting with the magnesium of a BChl a molecule is obtained and a significant ring current effect from B850 on the coordinating histidine is resolved. Using the ring current shift on 1 H, we refine the 13 C chemical shift assignment of the coordinating histidine and clearly distinguish the electronic structure of coordinating histidines from that of fully positively charged histidine. The DFT calculations corroborate that the coordinating histidines carry ∼0.2 electronic equivalent of positive charge in LH2. In addition, the data indicate that the ground state electronic structures of individual BChl a/His complexes is largely independent of supermolecular π interactions in the assembly of 18 B850 ring in LH2

  14. Effects of hydrostatic pressure on spin-lattice coupling in two-dimensional ferromagnetic Cr2Ge2Te6

    Science.gov (United States)

    Sun, Y.; Xiao, R. C.; Lin, G. T.; Zhang, R. R.; Ling, L. S.; Ma, Z. W.; Luo, X.; Lu, W. J.; Sun, Y. P.; Sheng, Z. G.

    2018-02-01

    Spin-lattice coupling plays an important role in both formation and understanding of the magnetism in two-dimensional magnetic semiconductors (2DMS). In this paper, the steady pressure effects on the lattice structure, Raman resonances, and magnetization of a 2DMS Cr2Ge2Te6 have been studied by both experiments and first principles calculations. It is found that the bond length of Cr-Cr decreases, the angle of Cr-Te-Cr diverges from 90°, and the Raman modes Eg3 and Ag1 show an increase with the application of external pressure. Consequently, the magnetic phase transition temperature TC decreases from 66.6 K to 60.6 K (˜9%) as the pressure increases from 0 to 1 GPa. These pressure effects not only confirm the existence of strong spin-lattice coupling but also reveal the detailed information about the lattice deformation effect on the magnetic properties in such 2DMS, which would be a benefit for the further understanding and manipulation of the magnetism in 2D materials.

  15. Nuclear Spin Lattice Relaxation and Conductivity Studies of the Non-Arrhenius Conductivity Behavior in Lithium Fast Ion Conducting Sulfide Glasses

    Energy Technology Data Exchange (ETDEWEB)

    Meyer, Benjamin Michael [Iowa State Univ., Ames, IA (United States)

    2003-01-01

    As time progresses, the world is using up more of the planet's natural resources. Without technological advances, the day will eventually arrive when these natural resources will no longer be sufficient to supply all of the energy needs. As a result, society is seeing a push for the development of alternative fuel sources such as wind power, solar power, fuel cells, and etc. These pursuits are even occurring in the state of Iowa with increasing social pressure to incorporate larger percentages of ethanol in gasoline. Consumers are increasingly demanding that energy sources be more powerful, more durable, and, ultimately, more cost efficient. Fast Ionic Conducting (FIC) glasses are a material that offers great potential for the development of new batteries and/or fuel cells to help inspire the energy density of battery power supplies. This dissertation probes the mechanisms by which ions conduct in these glasses. A variety of different experimental techniques give a better understanding of the interesting materials science taking place within these systems. This dissertation discusses Nuclear Magnetic Resonance (NMR) techniques performed on FIC glasses over the past few years. These NMR results have been complimented with other measurement techniques, primarily impedance spectroscopy, to develop models that describe the mechanisms by which ionic conduction takes place and the dependence of the ion dynamics on the local structure of the glass. The aim of these measurements was to probe the cause of a non-Arrhenius behavior of the conductivity which has been seen at high temperatures in the silver thio-borosilicate glasses. One aspect that will be addressed is if this behavior is unique to silver containing fast ion conducting glasses. more specifically, this study will determine if a non-Arrhenius correlation time, τ, can be observed in the Nuclear Spin Lattice Relaxation (NSLR) measurements. If so, then can this behavior be modeled with a new single

  16. NMR relaxation times in human brain tumors (preliminary results)

    International Nuclear Information System (INIS)

    Benoist, L.; Certaines, J. de; Chatel, M.; Menault, F.

    1981-01-01

    Since the early work of Damadian in 1971, proton NMR studies of tumors has been well documented. Present study concerns the spin-lattice T 1 and spin-spin T 2 relaxation times of normal dog brain according to the histological differentiation and of 35 human benignant or malignant tumors. The results principally show T 2 important variations between white and gray substance in normal brain but no discrimination between malignant and benignant tumors [fr

  17. Duchenne muscular dystrophy carriers. Proton spin-lattice relaxation times of skeletal muscles on magnetic resonance imaging

    Energy Technology Data Exchange (ETDEWEB)

    Matsumura, K.; Nakano, I. (Shimoshizu National Hospital, Chiba (Japan). Dept. of Neurology); Fukuda, N.; Ikehira, H.; Tateno, Y. (National Inst. of Radiological Sciences, Chiba (Japan). Div. of Clinical Research); Aoki, Y. (National Inst. of Radiological Sciences, Chiba (Japan))

    1989-11-01

    By means of magnetic resonance imaging (MRI), the proton spin-lattice relaxation times (T1 values) of the skeletal muscles were measured in Duchenne muscular dystrophy (DMD) carriers and normal controls. The bound water fraction (BWF) was calculated from the T1 values obtained, according to the fast proton diffusion model. In the DMD carriers, T1 values of the gluteus maximus and quadriceps femoris muscles were significantly higher, and BWFs of these muscles were significantly lower than in normal control. Degenerative muscular changes accompanied by interstitial edema were presumed responsible for this abnormality. No correlation was observed between the muscle T1 and serum creatine kinase values. The present study showed that MRI could be a useful method for studying the dynamic state of water in both normal and pathological skeletal muscles. Its possible utility for DMD carrier detection was discussed briefly. (orig.).

  18. Differential saturation study of radial and angular modulation mechanisms of electron spin--lattice relaxation for trapped hydrogen atoms in sulfuric acid glasses. [X radiation

    Energy Technology Data Exchange (ETDEWEB)

    Plonka, A; Kevan, L

    1976-11-01

    A differential ESR saturation study of allowed transitions and forbidden proton spin-flip satellite transitions for trapped hydrogen atoms in sulfuric acid glasses indicates that angular modulation dominates the spin-lattice relaxation mechanisms and suggests that the modulation arises from motion of the H atom.

  19. Low electron density of states at the boron site of TMB{sub 2} (TM = Ti, Zr, Hf, and Nb): a {sup 11}B NMR study

    Energy Technology Data Exchange (ETDEWEB)

    Paluch, S.; Zogal, O.J.; Peshev, P

    2004-11-30

    The local density of states at the boron site in TMB{sub 2} (TM=Ti, Zr, Hf, and Nb) has been examined using the solid-state {sup 11}B NMR technique. The magic angle spinning (MAS) NMR spectra at room temperature and the spin-lattice relaxation rates have been measured as functions of temperature (30-293 K). The resonance line shifts are small and become more negative in the direction from 3d- to 5d-elements. The relaxation rates follow a linear law characteristic of hyperfine magnetic interaction with conduction electrons. With borides of IV group metals the data can be understood in terms of a very low s-electron density of states and absence of a p-character of the conduction electron wave function at the Fermi level while in the case of NbB{sub 2} a small partial p-electron density of states is assumed. Then, the results are in good agreement with the earlier theoretical prediction.

  20. Some exercises in quantitative NMR imaging

    International Nuclear Information System (INIS)

    Bakker, C.J.G.

    1985-01-01

    The articles represented in this thesis result from a series of investigations that evaluate the potential of NMR imaging as a quantitative research tool. In the first article the possible use of proton spin-lattice relaxation time T 1 in tissue characterization, tumor recognition and monitoring tissue response to radiotherapy is explored. The next article addresses the question whether water proton spin-lattice relaxation curves of biological tissues are adequately described by a single time constant T 1 , and analyzes the implications of multi-exponentiality for quantitative NMR imaging. In the third article the use of NMR imaging as a quantitative research tool is discussed on the basis of phantom experiments. The fourth article describes a method which enables unambiguous retrieval of sign information in a set of magnetic resonance images of the inversion recovery type. The next article shows how this method can be adapted to allow accurate calculation of T 1 pictures on a pixel-by-pixel basis. The sixth article, finally, describes a simulation procedure which enables a straightforward determination of NMR imaging pulse sequence parameters for optimal tissue contrast. (orig.)

  1. Alternating spin chain compound AgVOAsO4 probed by 75As NMR

    Science.gov (United States)

    Ahmed, N.; Khuntia, P.; Ranjith, K. M.; Rosner, H.; Baenitz, M.; Tsirlin, A. A.; Nath, R.

    2017-12-01

    75As NMR measurements were performed on a polycrystalline sample of spin-1/2 alternating spin chain Heisenberg antiferromagnet AgVOAsO4. The temperature-dependent NMR shift K (T ) , which is a direct measure of the intrinsic spin susceptibility, agrees very well with the spin-1/2 alternating-chain model, justifying the assignment of the spin lattice. From the analysis of K (T ) , magnetic exchange parameters were estimated as follows: the leading exchange J /kB≃38.4 K and the alternation ratio α =J'/J ≃0.69 . The transferred hyperfine coupling between the 75As nucleus and V4 + spins obtained by comparing the NMR shift with the bulk susceptibility amounts to Ahf≃3.3 TμB. The effect of interchain couplings on the low-temperature activated behavior of K (T ) and the spin-lattice relaxation rate 1 /T1 is identified.

  2. Resonantly enhanced spin-lattice relaxation of Mn2 + ions in diluted magnetic (Zn,Mn)Se/(Zn,Be)Se quantum wells

    Science.gov (United States)

    Debus, J.; Ivanov, V. Yu.; Ryabchenko, S. M.; Yakovlev, D. R.; Maksimov, A. A.; Semenov, Yu. G.; Braukmann, D.; Rautert, J.; Löw, U.; Godlewski, M.; Waag, A.; Bayer, M.

    2016-05-01

    The dynamics of spin-lattice relaxation in the magnetic Mn2 + ion system of (Zn,Mn)Se/(Zn,Be)Se quantum-well structures are studied using optical methods. Pronounced cusps are found in the giant Zeeman shift of the quantum-well exciton photoluminescence at specific magnetic fields below 10 T, when the Mn spin system is heated by photogenerated carriers. The spin-lattice relaxation time of the Mn ions is resonantly accelerated at the cusp magnetic fields. Our theoretical analysis demonstrates that a cusp occurs at a spin-level mixing of single Mn2 + ions and a quick-relaxing cluster of nearest-neighbor Mn ions, which can be described as intrinsic cross-relaxation resonance within the Mn spin system.

  3. 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.

  4. Carbonaceous species (coke) characterization in zeolites by solid state {sup 13} C NMR; Caracterizacao de especies carbonaceas (coque) em zeolitos por RMN de {sup 13} C estado solido (CP/MAS)

    Energy Technology Data Exchange (ETDEWEB)

    Mota, Claudio J.A.; Menezes, Sonia C [PETROBRAS, Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

    1992-12-31

    This work applies solid state {sup 13} C NMR for characterization of carbonaceous species (coke) deposited on zeolites after contact with n-hexane at 370 deg C. The results have shown two types of carbon: saturated (sp{sup 3}) and unsaturated (sp{sup 2}) 4 refs., 4 tabs.

  5. Time domain NMR evaluation of poly(vinyl alcohol) xerogels

    Energy Technology Data Exchange (ETDEWEB)

    Rodrigues, Elton Jorge da Rocha; Cavalcante, Maxwell de Paula; Tavares, Maria Ines Bruno, E-mail: mibt@ima.ufrj.br [Universidade Federal do Rio de Janeiro (IMA/UFRJ), Rio de Janeiro, RJ (Brazil). Centro de Tecnologia. Instituto de Macromoleculas Professora Eloisa Mano

    2016-05-15

    Poly(vinyl alcohol) (PVA)-based chemically cross-linked xerogels, both neat and loaded with nanoparticulate hydrophilic silica (SiO{sub 2}), were obtained and characterized mainly through time domain NMR experiments (TD-NMR). Fourier-transform infrared (FT-IR) and wide angle X-ray diffraction (WAXD) analyses were employed as secondary methods. TD-NMR, through the interpretation of the spin-lattice relaxation constant values and related information, showed both cross-linking and nanoparticle influences on PVA matrix. SiO{sub 2} does not interact chemically with the PVA chains, but has effect on its molecular mobility, as investigated via TD-NMR. Apparent energy of activation, spin-lattice time constant and size of spin domains in the sample have almost linear dependence with the degree of cross-linking of the PVA and are affected by the addition of SiO{sub 2}. These three parameters were derived from a single set of TD-NMR experiments, which demonstrates the versatility of the technique for characterization of inorganic-organic hybrid xerogels, an important class of materials. (author)

  6. Spin dynamics at level crossing in molecular AF rings probed by NMR

    Energy Technology Data Exchange (ETDEWEB)

    Lascialfari, A. E-mail: lascialfari@fisicavolta.unipv.it; Borsa, F.; Julien, M.-H.; Micotti, E.; Furukawa, Y.; Jang, Z.H.; Cornia, A.; Gatteschi, D.; Horvatic, M.; Van Slageren, J

    2004-05-01

    The low-temperature spin dynamics in molecular rings with a finite number (N{<=}10) of magnetic ions was studied by means of {sup 1}H NMR. When an external magnetic field (B) induces a crossing between energy levels, peaks are observed in the spin-lattice relaxation rate of protons, 1/T{sub 1}(B), at constant temperature. We discuss similarities and differences in the data from three different rings: Fe10, Fe6:Li and Cr8.

  7. Spin dynamics at level crossing in molecular AF rings probed by NMR

    International Nuclear Information System (INIS)

    Lascialfari, A.; Borsa, F.; Julien, M.-H.; Micotti, E.; Furukawa, Y.; Jang, Z.H.; Cornia, A.; Gatteschi, D.; Horvatic, M.; Van Slageren, J.

    2004-01-01

    The low-temperature spin dynamics in molecular rings with a finite number (N≤10) of magnetic ions was studied by means of 1 H NMR. When an external magnetic field (B) induces a crossing between energy levels, peaks are observed in the spin-lattice relaxation rate of protons, 1/T 1 (B), at constant temperature. We discuss similarities and differences in the data from three different rings: Fe10, Fe6:Li and Cr8

  8. Spin freezing in geometrically frustrated magnetic molecule Fe30 revealed by NMR

    International Nuclear Information System (INIS)

    Furukawa, Yuji; Borsa, Ferdinando; Fang Xikui; Kögerler, Paul; Micotti, Edoardo; Lascialfari, Alessandro; Kumagai, Ken-ichi

    2012-01-01

    Static and dynamical properties of Fe 3+ (3d 5 ; S = 5/2) spins in geometrically frustrated magnetic molecule Fe30 have been investigated by nuclear magnetic resonance (NMR) in the temperature range T = 0.1–300 K From a measurement of nuclear spin-lattice relaxation rates as a function of temperature, the fluctuation frequency of Fe 3+ spins is found to decrease with decreasing temperature, indicating spin freezing at low temperatures.

  9. Antiferromagnetism Induced in the Vortex Core of Tl2Ba2CuO6++δ Probed by Spatially-Resolved 205Tl-NMR

    International Nuclear Information System (INIS)

    Kumagai, K.; Kakuyanagi, K.; Matsuda, Y.; Hasegawa, T.

    2003-01-01

    Magnetism in the vortex core state has been studied by spatially-resolved NMR. The nuclear spin lattice relaxation rate T 1 -1 of 205 Tl in nearly optimal-doped Tl 2 Ba 2 CuO 6+ δ (T c =85 K) is significantly enhanced in the vortex core region. The NMR results suggest that the suppression of the d-wave superconducting order parameter in the vortex core leads to the nucleation of islands with local antiferromagnetic (AF) order. (author)

  10. Fully automated system for pulsed NMR measurements

    International Nuclear Information System (INIS)

    Cantor, D.M.

    1977-01-01

    A system is described which places many of the complex, tedious operations for pulsed NMR experiments under computer control. It automatically optimizes the experiment parameters of pulse length and phase, and precision, accuracy, and measurement speed are improved. The hardware interface between the computer and the NMR instrument is described. Design features, justification of the choices made between alternative design strategies, and details of the implementation of design goals are presented. Software features common to all the available experiments are discussed. Optimization of pulse lengths and phases is performed via a sequential search technique called Uniplex. Measurements of the spin-lattice and spin-spin relaxation times and of diffusion constants are automatic. Options for expansion of the system are explored along with some of the limitations of the system

  11. 13C solid state NMR investigation of natural resins components

    International Nuclear Information System (INIS)

    Tavares, Maria I.B.; Bathista, Andre L.B.S.; Silva, Emerson O.; Priante Filho, Nicolau; Nogueira, Jose S.

    2001-01-01

    The objective of this work is to establish and analytical methodology as a routine using solid state nuclear magnetic resonance (NMR) techniques to investigate the mainly chemical components presented in natural resins in bulk. And also to evaluate the molecular behaviour of these resins. The routine solid state techniques allow us to assign the main compounds presented in the resins. Therefore, applying specialised techniques, like variable contact time, delayed contact time, dephasing time and proton spin lattice relaxation time in the rotating frame (T 1 H ρ), more information about chemical structure and molecular dynamic is available

  12. Single crystal NMR studies of high temperature superconductors

    International Nuclear Information System (INIS)

    Pennington, C.H.; Durand, D.J.; Zax, D.B.; Slichter, C.P.; Rice, J.P.; Bukowski, E.D.; Ginsberg, D.M.

    1989-01-01

    The authors report Cu NMR studies in the normal state of a single crystal of the T/sub c/ = 90 K superconductor YBa 2 Cu 3 O/sub 7/minus/δ/. The authors have measured the magnetic shift tensor, the electric field gradient tensor, the nuclear spin-lattice relaxation rate tensor, and the time dependence and functional form of the transverse decay. From these data they obtain information about the charge state and magnetic state of the Cu atoms, and the existence and size of the electronic exchange coupling between spins of adjacent Cu atoms. 18 refs., 3 figs., 2 tabs

  13. Identifying inter-residue resonances in crowded 2D {sup 13}C-{sup 13}C chemical shift correlation spectra of membrane proteins by solid-state MAS NMR difference spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Miao Yimin; Cross, Timothy A. [Florida State University, Department of Chemistry and Biochemistry (United States); Fu Riqiang, E-mail: rfu@magnet.fsu.edu [National High Magnet Field Lab (United States)

    2013-07-15

    The feasibility of using difference spectroscopy, i.e. subtraction of two correlation spectra at different mixing times, for substantially enhanced resolution in crowded two-dimensional {sup 13}C-{sup 13}C chemical shift correlation spectra is presented. With the analyses of {sup 13}C-{sup 13}C spin diffusion in simple spin systems, difference spectroscopy is proposed to partially separate the spin diffusion resonances of relatively short intra-residue distances from the longer inter-residue distances, leading to a better identification of the inter-residue resonances. Here solid-state magic-angle-spinning NMR spectra of the full length M2 protein embedded in synthetic lipid bilayers have been used to illustrate the resolution enhancement in the difference spectra. The integral membrane M2 protein of Influenza A virus assembles as a tetrameric bundle to form a proton-conducting channel that is activated by low pH and is essential for the viral lifecycle. Based on known amino acid resonance assignments from amino acid specific labeled samples of truncated M2 sequences or from time-consuming 3D experiments of uniformly labeled samples, some inter-residue resonances of the full length M2 protein can be identified in the difference spectra of uniformly {sup 13}C labeled protein that are consistent with the high resolution structure of the M2 (22-62) protein (Sharma et al., Science 330(6003):509-512, 2010)

  14. 53Cr NMR study of CuCrO2 multiferroic

    Science.gov (United States)

    Smol'nikov, A. G.; Ogloblichev, V. V.; Verkhovskii, S. V.; Mikhalev, K. N.; Yakubovskii, A. Yu.; Kumagai, K.; Furukawa, Y.; Sadykov, A. F.; Piskunov, Yu. V.; Gerashchenko, A. P.; Barilo, S. N.; Shiryaev, S. V.

    2015-11-01

    The magnetically ordered phase of the CuCrO2 single crystal has been studied by the nuclear magnetic resonance (NMR) method on 53Cr nuclei in the absence of an external magnetic field. The 53Cr NMR spectrum is observed in the frequency range νres = 61-66 MHz. The shape of the spectrum depends on the delay tdel between pulses in the pulse sequence τπ/2- t del-τπ- t del-echo. The spin-spin and spin-lattice relaxation times have been measured. Components of the electric field gradient, hyperfine fields, and the magnetic moment on chromium atoms have been estimated.

  15. E/Z MAS demonstration

    International Nuclear Information System (INIS)

    Boor, M.G.; Hurford, J.M.; Landry, R.P.; Martinez, B.J.; Solem, A.M.; Whiteson, R.; Zardecki, A.

    1998-01-01

    Los Alamos National Laboratory has developed E/Z MAS, a new generation nuclear material accountability application based on the latest technology and designed for facilities required to track nuclear materials with a simple-to-use interface. E/Z MAS is based on years of experience spent developing nuclear material accounting systems. E/Z MAS uses a modern relational database with a web server and enables users on a classified local area network to interact with the database with web browsers. The E/Z MAS Demonstration poster session demonstrates the E/Z MAS functions required by an operational nuclear facility to track material as it enters and leaves a facility and to account for the material as it moves through a process. The generation of internal facility reports and external reports for the Russian Federal system will be demonstrated. Bar-code readers will be used to demonstrate the ability of EZ MAS to automate certain functions, such as physical inventories at facilities

  16. {sup 119}Sn-NMR investigations on superconducting Ca{sub 3}Ir{sub 4}Sn{sub 13}: Evidence for multigap superconductivity

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, R., E-mail: rajibsarkarsinp@gmail.com [Institute for Solid State Physics, TU Dresden, D-01069 Dresden (Germany); Brückner, F.; Günther, M. [Institute for Solid State Physics, TU Dresden, D-01069 Dresden (Germany); Wang, Kefeng; Petrovic, C. [Condensed Matter Physics and Materials Science Department, Brookhaven National Laboratory, Upton, NY 11973 (United States); Biswas, P.K.; Luetkens, H.; Morenzoni, E.; Amato, A. [Laboratory for Muon Spin Spectroscopy, Paul Scherrer Institute, CH-5232 Villigen PSI (Switzerland); Klauss, H-H. [Institute for Solid State Physics, TU Dresden, D-01069 Dresden (Germany)

    2015-12-15

    We report bulk superconductivity (SC) in Ca{sub 3}Ir{sub 4}Sn{sub 13} by means of {sup 119}Sn nuclear magnetic resonance (NMR) experiments. Two classical signatures of BCS superconductivity in spin-lattice relaxation rate (1/T{sub 1}), namely the Hebel–Slichter coherence peak just below the T{sub c}, and the exponential decay in the superconducting phase, are evident. The noticeable decrease of {sup 119}Sn Knight shift below T{sub c} indicates spin-singlet superconductivity. The temperature dependence of the spin-lattice relaxation rate {sup 119}(1/T{sub 1}) is convincingly described by the multigap isotropic superconducting gap. NMR experiments do not witness any sign of enhanced spin fluctuations.

  17. High Magnetic Field Vortex Microscopy by NMR

    Science.gov (United States)

    Mitrović, V. F.; Sigmund, E. E.; Bachman, H. N.; Halperin, W. P.; Reyes, A. P.; Kuhns, P.; Moulton, W. G.

    2001-03-01

    At low temperatures the ^17O NMR spectrum of HTS exhibits a characteristic vortex lattice line shape. Measurements of spin-lattice relaxation rate, T_1-1, across the vortex spectrum represent a probe of low-energy quasiparticle excitations as a function of distance from the vortex core. We report ^17O(2,3) T_1-1 measurements of YBa_2Cu_3O7 at low temperatures in magnetic fields up to 37 T. We find that the rate increases on approaching the vortex core. In the vortex core region at 37 T we observe an additional increase in the relaxation rate. The temperature dependence of the rate will also be discussed. Work at Northwestern University is supported by the NSF (DMR 91-20000) through the Science and Technology Center for Superconductivity.

  18. NMR mechanisms in gel dosimetry

    International Nuclear Information System (INIS)

    Schreiner, L J

    2009-01-01

    observed rate is a function of the absorbed dose. In this review I will first develop the fast exchange model for the spin lattice relaxation Fricke gel dosimeter system, as this is conceptually the simpler system. Fundamental concepts such as relaxivity (which specifies the ability of some species to enhance the relaxation of water protons) and chemical yield will be presented. The linear dose relationship for Fricke gel dosimeters, and the reduced dose sensitivity of Fricke dosimeters containing chelators, will be explained. The model will then be extended to the spin-spin relaxation of polymer gel systems and the main differences discussed. The reasons for the enhanced dose sensitivy and dynamic range for spin-spin (R2) rather than spin-lattice (R1) relaxation will be presented.

  19. Lattice vibrations and barrier to hindered rotation in lithium tetradeuteroaluminate by 2H, 7Li and 27Al NMR

    International Nuclear Information System (INIS)

    Tarasov, V.P.; Kirakosyan, G.A.

    1996-01-01

    Temperature dependences of 2 H, 7 Li, 27 Al NMR line shape in LiAlD 4 lithium polycrystal tetradeuteroaluminate in the range of 103-420 K have been studied. The quadrupole bond constants and asymmetry parameters of electric field gradient tensor have been measured. The frequencies of lattice vibrations have been evaluated in the framework of the Buyer model. From temperature dependences of spin-lattice relaxation time and 2 H NMR line shape the activation energies of AlD 4 anion decelerated rotation, amounting to 74 and 62 k J/mol respectively, have been determined. 15 refs.; 5 figs.; 2 tabs

  20. 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.

  1. Lithium ion mobility in lithium phosphidosilicates: Crystal structure, {sup 7}Li, {sup 29}Si, and {sup 31}P MAS NMR spectroscopy, and impedance spectroscopy of Li{sub 8}SiP{sub 4} and Li{sub 2}SiP{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Toffoletti, Lorenzo; Landesfeind, Johannes; Klein, Wilhelm; Gasteiger, Hubert A.; Faessler, Thomas F. [Department of Chemistry, Technische Universitaet Muenchen, Lichtenbergstrasse 4, 85747, Garching bei Muenchen (Germany); Kirchhain, Holger; Wuellen, Leo van [Department of Physics, University of Augsburg, Universitaetsstrasse 1, 86159, Augsburg (Germany)

    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, Li{sub 8}SiP{sub 4} and Li{sub 2}SiP{sub 2}, 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) x 10{sup -6} Scm{sup -1} at 0 C to 1.2(2) x 10{sup -4} Scm{sup -1} at 75 C (Li{sub 8}SiP{sub 4}) and from 6.1(7) x 10{sup -8} Scm{sup -1} at 0 C to 6(1) x 10{sup -6} Scm{sup -1} at 75 C (Li{sub 2}SiP{sub 2}), as determined by impedance measurements. Temperature-dependent solid-state {sup 7}Li NMR spectroscopy revealed low activation energies of about 36 kJ mol{sup -1} for Li{sub 8}SiP{sub 4} and about 47 kJ mol{sup -1} for Li{sub 2}SiP{sub 2}. Both compounds were structurally characterized by X-ray diffraction analysis (single crystal and powder methods) and by {sup 7}Li, {sup 29}Si, and {sup 31}P MAS NMR spectroscopy. Both phases consist of tetrahedral SiP{sub 4} anions and Li counterions. Li{sub 8}SiP{sub 4} contains isolated SiP{sub 4} units surrounded by Li atoms, while Li{sub 2}SiP{sub 2} comprises a three-dimensional network based on corner-sharing SiP{sub 4} tetrahedra, with the Li ions located in cavities and channels. (copyright 2016 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. Effect of pressure on the short-range structure and speciation of carbon in alkali silicate and aluminosilicate glasses and melts at high pressure up to 8 GPa: 13C, 27Al, 17O and 29Si solid-state NMR study

    Science.gov (United States)

    Kim, Eun Jeong; Fei, Yingwei; Lee, Sung Keun

    2018-03-01

    increase in peak width of [4]Si with pressure. 17O NMR spectrum shows that the fraction of Na⋯Osbnd [5]Si in carbon-bearing NS3 glasses is less than that of carbon-free NS3 glasses at 6 GPa potentially due to the formation of bridging carbonate species. While its presence is not evident from the 17O NMR spectrum primarily due to low carbon concentration, 13C MAS NMR results imply the formation of bridging carbonates, [4]Si(CO3)[4]Si, above 6 GPa. The spin-lattice relaxation time (T1) of CO2 in albite melts increases with increasing pressure from 42 s (at 1.5 GPa) to 149 s (at 6 GPa). Taking the pressure-induced change in T1 of carbon species into consideration, total carbon content in carbon-bearing albite melts increases with pressure from ∼1 wt% at 1.5 GPa to ∼4.1 wt% at 6 GPa. The results also reveal a noticeable drop in the peak intensity of free carbonates in carbon-bearing NS3 melts at 6 GPa, implying a potential non-linear change in the carbon solubility with pressure. The current results of carbon speciation in the silicate melts above 4 GPa provide an improved link among the atomic configurations around carbon species, their carbon contents, and isotope composition of carbon-bearing melts in the upper mantle.

  3. Broad line NMR study of modified polypropylene fibres

    International Nuclear Information System (INIS)

    Olcak, D.; Sevcovic, L.; Mucha, L.

    1999-01-01

    Study of drawn fibres prepared from an isostatic polypropylene modified by an ethylene aminoalkylacrylate copolymer has been done using the broad line of 1 H NMR. NMR spectra were measured on the set of fibres prepared with a draw ratio λ from 1 to 5.5 at two temperatures, one of them corresponding to the onset of segmental motion and the other one is the minddle of the temperature interval as determined by decrease of the second moment M 2 . Decomposition of the spectra into elementary components related to the amorphous, intermediate and crystalline regions of partially crystalline polymers has been made. The drawing of the fibres was found to enhance the chain mobility in the amorphous region and to restrain the molecular motion in the intermediate region. Such behaviour well supports conclusions predicted in the earlier study based on the spin-lattice relaxation time T 1 and dynamic mechanical data treated using the WLF theory. (Authors)

  4. Investigation of the spin-lattice coupling in M n3G a1 -xS nxN antiperovskites

    Science.gov (United States)

    Shi, Kewen; Sun, Ying; Colin, Claire V.; Wang, Lei; Yan, Jun; Deng, Sihao; Lu, Huiqing; Zhao, Wenjun; Kazunari, Yamaura; Bordet, Pierre; Wang, Cong

    2018-02-01

    The magnetovolume effects (MVEs) of M n3G a1 -xS nxN antiperovskite compounds have been investigated by means of neutron powder diffraction. Increasing the Sn-doping content at the Ga site leads to the broadening of the magnetic phase transition temperature range and the thermal expansion behavior changes from negative to positive. We establish the relationship between the square of the ordered magnetic moment m2 and the volume variation Δ ωm for the antiferromagnetic phase (Γ5 g magnetic structure with rhombohedral symmetry R 3 ¯m ). The temperature variations of Δ ωm(T ) , m2(T ) and the magnetoelastic coupling constant C (T ) are also quantitatively analyzed according to the itinerant-electron theory. Moreover, the increase of the phonon contribution to the thermal expansion induced by Sn doping and the corresponding decrease of dm/dT are revealed to be the key parameters for tuning the MVEs. Our results allow elucidating and quantifying the mechanism of the spin-lattice coupling and can be used to design magnetic functional materials with controlled thermal expansion behaviors for specific applications.

  5. Magneto-optical measurement of spin-lattice relaxation time in KBr and in the Na and Cs halogenetes and Co++ ion magnetic circular dichroism study in KCl

    International Nuclear Information System (INIS)

    Carvalho, R.A.

    1977-01-01

    A magnetic circular dicroism spectrometer is described, which was used in the following experiments: 1) The spin-lattice relaxation time (T 1 ) for F centers in NaCl, NaBr, CsBr and CsCl, at 1,8 0 K in magnetic fields up to 15000Gs is described. The suitability of the theory of ref. (08) to explain the differences observed for halides of differents alkali ions as well as for different structures is verified proves that the hyperfine interaction is the most important mechanism for this kind of centers. It is also verified that, for temperatures between 6 0 K and 15 0 K, T 1 experimental values fits the theory of ref. (21) reasonably well, for F centers in KBr. This theory us an extension of that of ref. (8). 2) The MCD spectra for KCl:Co ++ and Caf 2 :Co ++ in different magnetic fields up to 56KGs, and in temperature range between 1,8 0 K and 4,2 0 K is obtained. The results are consistent with the assumption that Co ++ centers are intersticial in KCl lattice [pt

  6. Anisotropy of the proton spin--lattice relaxation time in the superconducting intercalation complex TaS2(NH3): Structural and bonding implications

    International Nuclear Information System (INIS)

    Gamble, F.R.; Silbernagel, B.G.

    1975-01-01

    The nature of the interaction responsible for the formation of molecular intercalation complexes between Lewis bases and layered transition metal dichalcogenides is not well understood. To some extent this is due to a lack of structural information. A prototype of these complexes is TaS 2 (NH 3 ), in which monolayers of ammonia are inserted between the metallic, superconducting layers of TaS 2 . The compound is crystalline and stoichiometric. Measurement of the anisotropy of the proton spin--lattice relaxation time at 300 degreeK indicates that the molecular threefold symmetry axis is not perpendicular to the disulfide layers as suggested by other workers, but is parallel to the layers. This orientation precludes direct interaction between the molecular lone pair orbital and the transition metal atoms. The interactions governing the structure of this complex may be similar to those obtaining in the intercalation complexes between TaS 2 and a number of substituted pyridines, in which complexes the axis of the lone pair orbital is also parallel to the layers

  7. Towards Using NMR to Screen for Spoiled Tomatoes Stored in 1,000 L, Aseptically Sealed, Metal-Lined Totes

    Directory of Open Access Journals (Sweden)

    Michael D. Pinter

    2014-03-01

    Full Text Available Nuclear magnetic resonance (NMR spectroscopy is used to track factory relevant tomato paste spoilage. It was found that spoilage in tomato paste test samples leads to longer spin lattice relaxation times T1 using a conventional low magnetic field NMR system. The increase in T1 value for contaminated samples over a five day room temperature exposure period prompted the work to be extended to the study of industry standard, 1,000 L, non-ferrous, metal-lined totes. NMR signals and T1 values were recovered from a large format container with a single-sided NMR sensor. The results of this work suggest that a handheld NMR device can be used to study tomato paste spoilage in factory process environments.

  8. Electron spin-lattice relaxation mechanisms of radiation produced trapped electrons and hydrogen atoms in aqueous and organic glassy matrices. Modulation of electron nuclear dipolar interaction by tunnelling modes in a glassy matrix. [. gamma. rays

    Energy Technology Data Exchange (ETDEWEB)

    Bowman, M K; Kevan, L [Wayne State Univ., Detroit, Mich. (USA). Dept. of Chemistry

    1977-01-01

    The spin lattice relaxation of trapped electrons in aqueous and organic glasses and trapped hydrogen atoms in phosphoric acid glass has been directly studied as a function of temperature by the saturation recovery method. Below 50 to 100 K, the major spin lattice relaxation mechanism involves modulation of the electron nuclear dipolar (END) interaction with nuclei in the radical's environment by tunnelling of those nuclei between two or more positions. This relaxation mechanism occurs with high efficiency and has a characteristic linear temperature dependence. The tunnelling nuclei around trapped electrons do not seem to involve the nearest neighbor nuclei which are oriented by the electron in the process of solvation. Instead the tunnelling nuclei typically appear to be next nearest neighbors to the trapped electron. The identities of the tunnelling nuclei have been deduced by isotopic substitution and are attributed to: Na in 10 mol dm/sup -3/ NaOH aqueous glass, ethyl protons in ethanol glass, methyl protons in methanol glass and methyl protons in MTHF glass. For trapped hydrogen atoms in phosphoric acid, the phosphorus nuclei appear to be the effective tunnelling nuclei. Below approximately 10 K the spin lattice relaxation is dominated by a temperature independent cross relaxation term for H atoms in phosphoric acid glass and for electrons in 10 mol dm/sup -3/ NaOH aqueous glass, but not for electrons in organic glasses. This is compared with recent electron-electron double resonance studies of cross relaxation in these glasses. The spin lattice relaxation of O/sup -/ formed in 10 mol dm/sup -3/ NaOH aqueous glass was also studied and found to be mainly dominated by a Raman process with an effective Debye temperature of about 100 K.

  9. Recent advances in solid state NMR and its application to ceramics

    International Nuclear Information System (INIS)

    Maekawa, Hideki

    2006-01-01

    The basic principles of solid state NMR are explained. Four application examples contained amorphous glass, determination of defects of oxide crystal, nano particle and ionic materials. The structure of inorganic glass is measured by 29 Si, 11 B, 31 P and 23 Na NMR and Magic Angle Spinning NMR (MAS-NMR), chemical species near hydrogen by Cross-Polarization Magic Angle Spinning (CP/MAS) method, and hydrogen by Combined Rotation And Multiple Pulse Spectroscopy (CRAMPS) and MAS-NMR. Hydrous and anhydrous silicate glass with condensed 17 O was measured by 17 O Multi Quantum Magic Angle Spinning (MQ/MAS). 27 Al in slags was analyzed by 27 Al 5Q-MAS. 89 Y NMR spectrum of YSZ (Yttria Stabilization Zirconia, Y 2 O 3 -ZrO 2 ) was explained. The ion transfer phenomena in the electrolyte are observed directly by the solid state NMR. (S.Y.)

  10. 121Sb-NMR study of filled skutterudite CeOs4Sb12

    International Nuclear Information System (INIS)

    Yogi, M.; Niki, H.; Mukuda, H.; Kitaoka, Y.; Sugawara, H.; Sato, H.

    2007-01-01

    121 Sb nuclear magnetic resonance (NMR) of filled skutterudite compound CeOs 4 Sb 12 has been carried out to investigate a spin fluctuation below T∼25K. In spite of a powdered sample, many sharp peaks, similar to a data for single crystal, were observed because of an orientation of the sample from the anisotropy of the magnetization. A numerical calculation well reproduces resonance fields for Sb(1) sites with H parallel V zz . The nuclear spin-lattice relaxation rate divided by temperature 1/T 1 T shows continuous decrease with increasing magnetic field, indicating a suppression of the spin fluctuation by the field

  11. A many-body analysis of NMR in spin-1/2 system

    International Nuclear Information System (INIS)

    Roy, G.K.; Sinha, S.K.

    1977-01-01

    The NMR absorption in a spin-1/2 system at finite temperature has been analysed by using the linear response theory and calculating the finite-temperature retarted spin Green's function. In this calculations, the Drone-Fermion representation for the spin operators has been used. A model spin-lattice interaction which is linear in phonon and Fermion operators has been considered, and its effect on a mutually non-interacting spin system has been calculated using the diagrammatic expansions technique. It is found that the complete summing up of a particular class of diagrams yields the Lorentzian shape of the resonance line. (author)

  12. Unconventional superconductivity in PuRhGa5: Ga NMR/NQR study

    International Nuclear Information System (INIS)

    Sakai, H.; Tokunaga, Y.; Fujimoto, T.; Kambe, S.; Walstedt, R.E.; Yasuoka, H.; Aoki, D.; Homma, Y.; Yamamoto, E.; Nakamura, A.; Shiokawa, Y.; Nakajima, K.; Arai, Y.; Matsuda, T.D.; Haga, Y.; Onuki, Y.

    2006-01-01

    69,71 Ga NMR/NQR studies have been performed on a single crystal of the transuranium superconductor PuRhGa 5 with T c ∼9K. The spin-lattice relaxation rate 1/T 1 reveals that PuRhGa 5 is an unconventional superconductor having an anisotropic superconducting gap. Moreover, Korringa behavior (1/T 1 T=const.) is observed in the normal state below ∼30K. This result suggests that the superconductivity sets in after the formation of a Fermi liquid state in this compound

  13. Broad line and pulsed NMR study of molecular motion in furfuryl alcohol resins

    International Nuclear Information System (INIS)

    Glowinkowski, S.; Pajak, Z.

    1978-01-01

    Broad line and pulsed nuclear magnetic resonance studies are carried out on a number of furfuryl alcohol resins differentiated by viscosity. Proton NMR spectra and relaxation times T 1 and Tsub(1rho) are measured over a wide temperature range and the results are interpreted in terms of molecular motion. The marked decrease in second moment and existence of high temperature spin-lattice relaxation times minima are presumed to result from rotational motion of polymer chains. The relaxation processes at low temperature are believed to be due to rotational motion of methyl endgroup and paramagnetic centres. (author)

  14. NMR relaxation rates and Knight shifts in the alloy Mg1-xAlxB2

    International Nuclear Information System (INIS)

    Serventi, S; Allodi, G; Bucci, C; Renzi, R De; Guidi, G; Pavarini, E; Manfrinetti, P; Palenzona, A

    2003-01-01

    We measured the 27 Al and 11 B NMR spin lattice relaxation rates and the isotropic Knight shifts in powder samples of Mg 1-x Al x B 2 , as a function of the Al concentration, x. The temperature independence of the Knight shifts and the linear temperature dependence of the relaxation are verified throughout the compositions explored. The variation with x of the measured quantities is discussed in terms of the projected densities of states at the Fermi energy, finding good qualitative as well as quantitative agreement with recent band structure calculations

  15. Inorganic-organic hybrids based on poly (ε-Caprolactone and silica oxide and characterization by relaxometry applying low-field NMR

    Directory of Open Access Journals (Sweden)

    Mariana Sato de Souza de Bustamante Monteiro

    2012-12-01

    Full Text Available Poly (ε-caprolactone (PCL based hybrids containing different amounts of modified (Aerosil® R972 and unmodified (Aerosil® A200 silica oxide were prepared employing the solution method, using chloroform. The relationships of the amount of nanofillers, organic coating, molecular structure and intermolecular interaction of the hybrid materials were investigated mainly using low-field nuclear magnetic resonance (NMR. The NMR analyses involved the hydrogen spin-lattice relaxation time (T1H and hydrogen spin-lattice relaxation time in the rotating frame (T1ρH. The spin-lattice relaxation time measurements revealed that the PCL/silica oxide hybrids were heterogeneous, meaning their components were well dispersed. X-ray diffraction (XRD, differential scanning calorimetry (DSC and thermogravimetric analysis (TGA were also employed. The DSC data showed that all the materials had lower crystallization temperature (Tc and melting temperature (Tm, so the crystallinity degree of the PCL decreased in the hybrids. The TGA analysis demonstrated that the addition of modified and unmodified silica oxide does not cause considerable changes to PCL's thermal stability, since no significant variations in the maximum temperature (Tmax were observed in relation to the neat polymer.

  16. Novel 1H NMR approach to quantitative tissue oximetry using hexamethyldisiloxane.

    Science.gov (United States)

    Kodibagkar, Vikram D; Cui, Weina; Merritt, Matthew E; Mason, Ralph P

    2006-04-01

    19F NMR spin-lattice relaxometry of hexafluorobenzene (HFB) has been shown to be a highly sensitive indicator of tumor oxygenation. In this study hexamethyldisiloxane (HMDSO) was identified as a proton NMR analog, and its potential as a probe for investigating dynamic changes in tissue oxygen tension (pO2) was evaluated. HMDSO has a single proton resonance (delta= -0.3 ppm) and the spin-lattice relaxation rate, Rl (= 1/T1) exhibits a linear dependence on pO2: R1 (s(-1)) = 0.1126 + 0.0013* pO2 (torr) at 37 degrees C. To demonstrate application in vivo, HMDSO was administered into healthy rat thigh muscle (100 microl) and tumors (50 microl). Local pO2 was determined by using pulse-burst saturation recovery (PBSR) 1H NMR spectroscopy to assess R1. Water and fat signals were effectively suppressed by frequency-selective excitation of the HMDSO resonance. Rat thigh muscle had a mean baseline pO2 of 35 +/- 11 torr, with a typical stability of +/-3 torr over 20 min, when the rats breathed air. Altering the inhaled gas to oxygen produced a significant increase in pO2 to 100-200 torr. In tumors, altering the inspired gas also produced significant (albeit generally smaller) changes. This new pO2 reporter molecule offers a potentially valuable new tool for investigating pO2 in vivo. (c) 2006 Wiley-Liss, Inc.

  17. Quantum-optical magnets with competing short- and long-range interactions: Rydberg-dressed spin lattice in an optical cavity

    Directory of Open Access Journals (Sweden)

    Jan Gelhausen, Michael Buchhold, Achim Rosch, Philipp Strack

    2016-10-01

    Full Text Available The fields of quantum simulation with cold atoms [1] and quantum optics [2] are currently being merged. In a set of recent pathbreaking experiments with atoms in optical cavities [3,4] lattice quantum many-body systems with both, a short-range interaction and a strong interaction potential of infinite range -mediated by a quantized optical light field- were realized. A theoretical modelling of these systems faces considerable complexity at the interface of: (i spontaneous symmetry-breaking and emergent phases of interacting many-body systems with a large number of atoms $N\\rightarrow\\infty$, (ii quantum optics and the dynamics of fluctuating light fields, and (iii non-equilibrium physics of driven, open quantum systems. Here we propose what is possibly the simplest, quantum-optical magnet with competing short- and long-range interactions, in which all three elements can be analyzed comprehensively: a Rydberg-dressed spin lattice [5] coherently coupled to a single photon mode. Solving a set of coupled even-odd sublattice Master equations for atomic spin and photon mean-field amplitudes, we find three key results. (R1: Superradiance and a coherent photon field can coexist with spontaneously broken magnetic translation symmetry. The latter is induced by the short-range nearest-neighbor interaction from weakly admixed Rydberg levels. (R2: This broken even-odd sublattice symmetry leaves its imprint in the light via a novel peak in the cavity spectrum beyond the conventional polariton modes. (R3: The combined effect of atomic spontaneous emission, drive, and interactions can lead to phases with anomalous photon number oscillations. Extensions of our work include nano-photonic crystals coupled to interacting atoms and multi-mode photon dynamics in Rydberg systems.

  18. 27Al NMR studies of NpPd5Al2

    International Nuclear Information System (INIS)

    Chudo, H.; Sakai, H.; Tokunaga, Y.; Kambe, S.; Aoki, D.; Homma, Y.; Shiokawa, Y.; Haga, Y.; Ikeda, S.; Matsuda, T.D.; Onuki, Y.; Yasuoka, H.

    2009-01-01

    We present 27 Al NMR studies for a single crystal of the Np-based superconductor NpPd 5 Al 2 (T c =4.9K). We have observed a five-line 27 Al NMR spectrum with a center line and four satellite lines separated by first-order nuclear quadrupole splittings. The Knight shift clearly drops below T c . The temperature dependence of the 27 Al nuclear spin-lattice relaxation rate shows no coherence peak below T c , indicating that NpPd 5 Al 2 is an unconventional superconductor with an anisotropic gap. The analysis of the present NMR data provides evidence for strong-coupling d-wave superconductivity in NpPd 5 Al 2 .

  19. High Tech M&As

    DEFF Research Database (Denmark)

    Toppenberg, Gustav

    2013-01-01

    Technology driven industries have seen fast moving technology changes, higher complexity and reduced product life cycles. These emerging trends present challenges for companies in industries where technology is at the forefront. The extant research deals with ‘low-tech’ industries and majority...... 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...

  20. Morphological study of chitin from Xiphopenaeus kroyeri exoskeletons by using atomic force microscopy (AFM) and CPMAS {sup 13} C NMR; Estudo morfologico de quitina da exocuticula de Xiphopenaeus kroyeri por AFM e por CPMAS {sup 13} C NMR

    Energy Technology Data Exchange (ETDEWEB)

    Silva, K.M.; Tavares, M.I.; Andrade, C.T. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Macromoleculas; Simao, R.A. [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Programa de Engenharia Metalurgica e de Materiais

    1999-07-01

    A sample of {alpha} chitin was isolated from exoskeletons of Xiphopenaeus kroyeri. This sample ws dissolved in phosphoric acid and recovered as a fibrous precipitate. Atomic force microscopy was used in noncontact mode to obtain images of the native chitin sample. Different morphological features were observed, including rigid rod crystals 200-300 nm wide. Solid state {sup 13} C NMR techniques were used to investigate chitin samples, and revealed molecular order in both samples. The differences observed in the proton spin-lattice relaxation times in the rotating frame, T{sup H1}{sub p} were attributed to the formation of hydrogen bonds in preferential sites in the samples. (author)

  1. Investigation of the molecular motions in Cd(NH/sub 3/)/sub 6/Cl/sub 2/ by NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Pislewski, N [Polska Akademia Nauk, Poznan. Inst. Fizyki Molekularnej; Ferris, L T.H. [University Coll., London (UK). Dept. of Chemistry

    1981-07-01

    NMR results are reported for intramolecular motion in Cd(NH/sub 3/)/sub 6/Cl/sub 2/. Below the 180 K phase transition, the motion of the NH/sub 3/ groups is well described by the Hilt-Hubbard theory with an activation energy of 9.63 kJ/mol. The inter-proton distance in NH/sub 3/ determined from relaxational measurements is 0.161 nm. Several K below and above the transition point, two phases with different spin-lattice relaxation times coexist.

  2. Morphological study of chitin from Xiphopenaeus kroyeri exoskeletons by using atomic force microscopy (AFM) and CPMAS 13 C NMR

    International Nuclear Information System (INIS)

    Silva, K.M.; Tavares, M.I.; Andrade, C.T.; Simao, R.A.

    1999-01-01

    A sample of α chitin was isolated from exoskeletons of Xiphopenaeus kroyeri. This sample ws dissolved in phosphoric acid and recovered as a fibrous precipitate. Atomic force microscopy was used in noncontact mode to obtain images of the native chitin sample. Different morphological features were observed, including rigid rod crystals 200-300 nm wide. Solid state 13 C NMR techniques were used to investigate chitin samples, and revealed molecular order in both samples. The differences observed in the proton spin-lattice relaxation times in the rotating frame, T H1 p were attributed to the formation of hydrogen bonds in preferential sites in the samples. (author)

  3. NMR study of CeCoSi3

    International Nuclear Information System (INIS)

    Iwamoto, Y.

    1995-01-01

    Low-temperature susceptibility, NMR and NQR of the 59 Co signal in CeCoSi 3 have been measured. CeCoSi 3 showed a superconducting transition at 0.7-1.2K. From NQR measurement, the nuclear quadrupole frequency and the full width at half maximum (FWHM) of 59 Co in CeCoSi 3 were estimated to be about 1.08MHz and 0.08MHz, respectively. The 59 Co nuclear spin-lattice relaxation rate (1/T 1 ) in CeCoSi 3 was proportional to the temperature (T) as the Fermi liquid state above the superconducting transition temperature (T c ), and then rapidly decreased below T c . ((orig.))

  4. Regional tumor oximetry: 19F NMR spectroscopy of hexafluorobenzene

    International Nuclear Information System (INIS)

    Hunjan, Sandeep; Mason, Ralph P.; Constantinescu, Anca; Peschke, Peter; Hahn, Eric W.; Antich, Peter P.

    1998-01-01

    Purpose: An accurate method for monitoring oxygen tension (pO 2 ) of individual tumors could be valuable for optimizing treatment plans. We have recently shown that 19 F nuclear magnetic resonance (NMR) spin-lattice relaxometry of hexafluorobenzene (HFB) provides a highly sensitive indicator of tumor oxygenation. We have now refined the methodology to provide enhanced precision, and applied the method to investigate dynamic changes in tumor oxygenation. Methods and Materials: Dunning prostate adenocarcinoma R3327-AT1 was grown in the form of pedicles on the foreback of male Copenhagen rats. When the tumors reached ≅1 cm diameter, HFB (20 μl) was administered, either centrally or peripherally, by direct intratumoral (IT) injection. Local pO 2 was determined using pulse-burst saturation recovery (PBSR) 19 F NMR spectroscopy on the basis of the spin-lattice relaxation rate, R1. Results: Interrogation of the central region of tumors provided typical values in the range pO 2 = 1.4-6.4 mmHg, with a typical stability of ±2 mmHg over a period of 20 min, when rats breathed 33% O 2 . Altering the inhaled gas to oxygen or carbogen (95% O 2 /5% CO 2 ) produced no significant change. In contrast, interrogation of tumor periphery indicated baseline pO 2 in the range 7.9-78.9 mmHg. Altering inspired gas produced significant changes (p 2 or carbogen, although the change was generally greater with carbogen. In each case, pO 2 returned to baseline within 16 min of returning the inhaled gas to baseline. Conclusion: We believe this method provides a valuable new approach with the requisite precision and accuracy to investigate tumor pO 2

  5. Solid state NMR of materials

    Energy Technology Data Exchange (ETDEWEB)

    Taylor, Sharon A; Ferguson, David B; Haw, James F [Texas A and M Univ., College Station, TX (United States). Dept. of Chemistry

    1994-12-31

    In situ NMR experiments are studied, including probe of several structures such as the structures of the organic adsorbates, Broensted acid sites, other nuclei associated with active sites, and other framework sites. The authors report that in the absence of high concentrations of paramagnetic sites or metal particles, high resolution MAS spectra are relatively easy to obtain and interpret. It is also concluded that NMR can measure spatial distributions and rates of diffusion; and are able to characterize equilibrium structures and the frequencies and amplitudes of molecular motion

  6. Temperature dependence of electron spin-lattice relaxation of radiation-produced silver atoms in polycrystalline aqueous and glassy organic matrices. Importance of relaxation by tunneling modes in disordered matrices

    International Nuclear Information System (INIS)

    Michalik, J.; Kevan, L.

    1978-01-01

    The electron spin-lattice relaxation of trapped silver atoms in polycrystalline ice matrices and in methanol, ethanol, propylene carbonate, and 2-methyltetrahydrofuran organic glasses has been directly studied as a function of temperature by the saturation-recovery method. Below 40 K the dominant electron spin-lattice relaxation mechanism involves modulation of the electron nuclear dipolar interaction with nuclei in the radical's environment by tunneling of those nuclei between two nearly equal energy configurations. This relaxation mechanism occurs with high efficiency, has a characteristic linear temperature dependence, and is typically found in highly disordered matrices. The efficiency of this relaxation mechanism seems to decrease with decreasing polarity of the matrix. Deuteration experiments show that the tunneling nuclei are protons and in methanol it is shown that the methyl protons have more tunneling modes available than the hydroxyl protons. In polycrystalline ice matrices silver atoms can be stabilized with two different orientations of surrounding water molecules; the efficiency of the tunneling relaxation reflects this difference. From these and previous results on tunneling relaxation of trapped electrons in glassy matrices it appears that tunneling relaxation may be used to distinguish models with different geometrical configurations and to determine the relative rigidity of such configurations around trapped radicals in disordered solids. (author)

  7. NMR relaxation and phase transitions in solid methane and deuterated derivatives

    International Nuclear Information System (INIS)

    Putten, D. van der.

    1984-01-01

    This thesis describes an investigation of properties of solid methane at high pressure (till 10 kbar) with temperatures ranging from 2 until 100 K. The high inverse moment of inertia of the molecule combined with low ordering potentials gives rise to properties for which quantum effects play an important role: e.g. the transition temperature to a partially ordered phase shows an isotope effect of 35% when CH 4 protons are substituted by deuterons. Interpretation of NMR properties of solid methane also show quantum effects. First, a helium cryostat is developed and described and NMR results for CH 4 , CH 2 D 2 and CD 4 are given. The influence of discrete tunnel states on the spin-lattice relaxation is studied theoretically. Application of group theory has simplified the calculations considerably. (G.J.P.)

  8. 133Cs NMR investigation of 2D frustrated Heisenberg antiferromagnet, Cs2CuCl4

    Science.gov (United States)

    Vachon, M.-A.; Kundhikanjana, W.; Straub, A.; Mitrovic, V. F.; Reyes, A. P.; Kuhns, P.; Coldea, R.; Tylczynski, Z.

    2006-10-01

    We report 133Cs nuclear magnetic resonance (NMR) measurements on the 2D frustrated Heisenberg antiferromagnet Cs2CuCl4 down to 2 K and up to 15 T. We show that 133Cs NMR is a good probe of the magnetic degrees of freedom in this material. Cu spin degrees of freedom are sensed through a strong anisotropic hyperfine coupling. The spin excitation gap opens above the critical saturation field. The gap value was determined from the activation energy of the nuclear spin-lattice relaxation rate in a magnetic field applied parallel to the Cu chains (\\skew3\\hat{b} axis). The values of the g-factor and the saturation field are consistent with the neutron-scattering and magnetization results. The measurements of the spin spin relaxation time are exploited to show that no structural changes occur down to the lowest temperatures investigated.

  9. Luther-Emery liquid in the NMR relaxation rate of carbon nanotubes

    International Nuclear Information System (INIS)

    Gulacsi, Miklos; Simon, Ferenc; Wzietek, Pawel; Kuzmany, Hans; Dora, Balazs

    2008-01-01

    We analyze a recent NMR experiments by Singer et al.[Singer et al. Phys. Rev. Lett. 95, 236403 (2005).], which showed a deviation from Fermi-liquid behavior in carbon nanotubes with an energy gap evident at low temperatures. A comprehensive theory for the magnetic field and temperature dependent NMR 13 C spin-lattice relaxation is given in the framework of the Luther-Emery and Luttinger liquids. The low temperature properties are governed by a gapped relaxation due to a spin gap (∝30 K), described by the Luther-Emery liquid picture, which crosses over smoothly to the Luttinger liquid behaviour with increasing temperature. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  10. NMR studies of hydrogen diffusion in hydrogen uranyl phosphate tetrahydrate (HUP)

    International Nuclear Information System (INIS)

    Metcalfe, K.

    1988-01-01

    1 H NMR spin-lattice relaxation times, T 1 (Zeeman) and T 1p (rotating frame) and spin-spin relaxation times, T 2 , and 31 P NMR solid-echoes are reported for phase I and II of hydrogen uranyl phosphate tetrahydrate (HUP) at temperatures in the range 200-323 K. The spectral density functions extracted from the measured relaxation times for phases I and II are consistent with a 2D diffusion mechanism for hydrogen motion. 31 P second moments determined from the solid-echoes show that all the hydrogens diffuse rapidly in phase I, and that the hydrogen-bond site nearest to the phosphate oxygen is not occupied in phase II. The mechanism for diffusion in phase II is discussed. 30 refs.; 6 figs.; 2 tabs

  11. Study of relaxation times of nanocomposites of starch/montmorillonite employing low field NMR

    International Nuclear Information System (INIS)

    Brito, Luciana M.; Tavares, Maria Ines B.

    2011-01-01

    Due to its various applications and features, especially in therapies for controlled release of pharmaceuticals, polymers are among the most widely used excipients in pharmaceutical technology. One of the most promising nanocomposites is formed from organic polymer and inorganic clay minerals. Nanocomposites of starch/montmorillonite were prepared employing solution intercalation and characterized by proton spin-lattice relaxation time, through NMR relaxometry. The characterization of nanocomposites was done by X-ray diffraction and by nuclear magnetic resonance. The results showed that nanostructured films were obtained by intercalation from solution. Furthermore, the use of low field NMR, T1H, provided more precise information about the movement of materials, being complementary to the results obtained by X-ray diffraction. (author)

  12. 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 1.3 mm-rotor diameter has been analyzed for spinning rates up to 67 kHz. 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 1.3 mm-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 1.3-7 mm 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.

  13. Hierarchical MAS based control strategy for microgrid

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, Z.; Li, T.; Huang, M.; Shi, J.; Yang, J.; Yu, J. [School of Information Science and Engineering, Yunnan University, Kunming 650091 (China); Xiao, Z. [School of Electrical and Electronic Engineering, Nanyang Technological University, Western Catchment Area, 639798 (Singapore); Wu, W. [Communication Branch of Yunnan Power Grid Corporation, Kunming, Yunnan 650217 (China)

    2010-09-15

    Microgrids have become a hot topic driven by the dual pressures of environmental protection concerns and the energy crisis. In this paper, a challenge for the distributed control of a modern electric grid incorporating clusters of residential microgrids is elaborated and a hierarchical multi-agent system (MAS) is proposed as a solution. The issues of how to realize the hierarchical MAS and how to improve coordination and control strategies are discussed. Based on MATLAB and ZEUS platforms, bilateral switching between grid-connected mode and island mode is performed under control of the proposed MAS to enhance and support its effectiveness. (authors)

  14. NMR study of quasi-one-dimensional itinerant-electron magnets RMn{sub 4}Al{sub 8} (R=Y, Lu and Sc)

    Energy Technology Data Exchange (ETDEWEB)

    Muro, Y. [Graduate School of Material Science, University of Hyogo, Kamigori, Ako-gun, Hyogo 678-1297 (Japan)], E-mail: rk04j052@yahoo.co.jp; Nakamura, H.; Kohara, T. [Graduate School of Material Science, University of Hyogo, Kamigori, Ako-gun, Hyogo 678-1297 (Japan)

    2008-04-01

    {sup 55}Mn-NMR measurements, which revealed previously the presence of spin pseudogap in YMn{sub 4}Al{sub 8}, have been extended to LuMn{sub 4}Al{sub 8} and ScMn{sub 4}Al{sub 8}. Temperature (T) dependences of the Knight shift, K, and the nuclear spin-lattice relaxation rate, 1/T{sub 1}, are well explained by the same pseudogap model used to explain a broad maximum observed in the T-dependence of the susceptibility, indicating common nature in the spin excitation spectrum in the quasi-one-dimensional itinerant-electron compounds.

  15. Proton NMR relaxation in hydrous melts

    International Nuclear Information System (INIS)

    Braunstein, J.; Bacarella, A.L.; Benjamin, B.M.; Brown, L.L.; Girard, C.

    1976-01-01

    Pulse and continuous wave NMR measurements are reported for protons in hydrous melts of calcium nitrate at temperatures between -4 and 120 0 C. Although measured in different temperature ranges, spin-lattice (T 1 ) and spin-spin (T 2 ) relaxation times appear to be nearly equal to each other and proportional to the self-diffusion coefficients of solute metal cations such as Cd 2+ . At temperatures near 50 0 C, mean Arrhenius coefficients Δ H/sub T 1 / (kcal/mol) are 7.9, 7.3, and 4.8, respectively, for melts containing 2.8, 4.0, and 8.0 moles of water per mole of calcium nitrate, compared to 4.6 kcal/mol for pure water. Temperature dependence of T 1 and T 2 in Ca(NO 3 ) 2 -2.8 H 2 O between -4 and 120 0 C are non-Arrhenius and can be represented by a Fulcher-type equation with a ''zero mobility temperature'' (T 0 ) of 225 0 K, close to the value of T 0 for solute diffusion, electrical conductance and viscosity. Resolution of the relaxation rates into correlation times for intramolecular (rotational) and intermolecular (translational) diffusional motion is discussed in terms of the Bloembergen-Purcell-Pound and more recent models for dipolar relaxation

  16. Tunneling splitting of magnetic levels in Fe8 detected by 1H NMR cross relaxation

    Science.gov (United States)

    Furukawa, Y.; Aizawa, K.; Kumagai, K.; Ullu, R.; Lascialfari, A.; Borsa, F.

    2003-05-01

    Measurements of proton NMR and the spin lattice relaxation rate 1/T1 in the octanuclear iron (III) cluster [Fe8(N3C6H15)6O2(OH)12]ṡ[Br8ṡ9H2O], in short Fe8, have been performed at 1.5 K in a powder sample aligned along the main anisotropy z axis, as a function of a transverse magnetic field (i.e., perpendicular to the main easy axis z). A big enhancement of 1/T1 is observed over a wide range of fields (2.5-5 T), which can be attributed to the tunneling dynamics; in fact, when the tunneling splitting of the pairwise degenerate m=±10 states of the Fe8 molecule becomes equal to the proton Larmor frequency a very effective spin lattice relaxation channel for the nuclei is opened. The experimental results are explained satisfactorily by considering the distribution of tunneling splitting resulting from the distribution of the angles in the hard xy plane for the aligned powder, and the results of the direct diagonalization of the model Hamiltonian.

  17. Carbon-13 NMR of glycogen: Hydration response studied by using solids methods

    International Nuclear Information System (INIS)

    Jackson, C.L.; Bryant, R.G.

    1989-01-01

    The carbon-13 NMR spectra of glycogen are reported by using the methods of magic-angle sample spinning and high-power proton decoupling to provide a dynamic report on the glucose monomer behavior as a function of hydration. Although the glycogen behaves as a typical polymer in the dry state, addition of water makes a significant difference in the spectral appearance. Water addition decreases the carbon spin-lattice relaxation times by 2 orders of magnitude over the range from 7% to 70% water by weight. The proton-carbon dipole-dipole coupling, which broadens the carbon spectrum and permits cross-polarization spectroscopy, is lost with increasing hydration over this range. By 60% water by weight, scalar decoupling methods are sufficient to achieve a reasonably high-resolution spectrum. Further, at this concentration, the carbon spin-lattice relaxation times are near their minimum values at a resonance frequency of 50.3 MHz, making acquisition of carbon spectra relatively insensitive to intensity distortions associated with saturation effects. Though motional averaging places the spectrum in the solution phase limit, the static spectrum shows a residual broader component that would not necessarily be detected readily by using high-resolution liquid-state experiments

  18. Non-Arrhenius conductivity in the fast ionic conductor Li0.5La0.5TiO3: Reconciling spin-lattice and electrical-conductivity relaxations

    International Nuclear Information System (INIS)

    Leon, C.; Santamaria, J.; Paris, M.A.; Sanz, J.; Ibarra, J.; Torres, L.M.

    1997-01-01

    Nuclear magnetic resonance and electrical conductivity measurements are conducted to study the dynamics of the ionic diffusion process in the crystalline ionic conductor Li 0.5 La 0.5 TiO 3 . dc conductivity shows a non-Arrhenius temperature dependence, similar to the one recently reported for some ionic conducting glasses. Spin-lattice and conductivity relaxations are analyzed in the same frequency and temperature range in terms of the non-Arrhenius dependence of the correlation time. Both relaxations are then described using a single correlation function of the form f(t)=exp(-(t/τ) β ), with β=0.4 over the whole temperature range. copyright 1997 The American Physical Society

  19. 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.

  20. Measurements of electric quadrupole moments of neutron-deficient Au, Pt, and Ir nuclei with NMR-ON in hcp-Co

    CERN Multimedia

    Smolic, E; Hagn, E; Zech, E; Seewald, G

    2002-01-01

    The aim of the experiments is the measurement of $\\,$i) nuclear magnetic moments and electric quadrupole moments of neutron-deficient isotopes in the region Os-Ir-Pt-Au with the methods of quadrupole-interaction-resolved NMR on oriented nuclei " QI-NMR-ON " and modulated adiabatic passage on oriented nuclei " MAPON " and $\\,$ii) the magnetic hyperfine field, electric field gradient (EFG), and spin-lattice relaxation of 5d elements in ferromagnetic Fe, Ni, fcc-Co and hcp-Co.\\\\ The measurements on Au isotopes have been finished successfully. The quadrupole moments of $^{186}$Au, $^{193m}$Au, $^{195}$Au, $^{195m}$Au, $^{197m}$Au, $^{198}$Au and $^{199}$Au were determined with high precision.\\\\ For neutron-deficient Ir isotopes QI-NMR-ON measurements were performed after implantation of Hg precursors. The EFG of Ir in hcp-Co has been calibrated. Thus precise values for the spectroscopic quadrupole mo...

  1. An NMR database for simulations of membrane dynamics.

    Science.gov (United States)

    Leftin, Avigdor; Brown, Michael F

    2011-03-01

    Computational methods are powerful in capturing the results of experimental studies in terms of force fields that both explain and predict biological structures. Validation of molecular simulations requires comparison with experimental data to test and confirm computational predictions. Here we report a comprehensive database of NMR results for membrane phospholipids with interpretations intended to be accessible by non-NMR specialists. Experimental ¹³C-¹H and ²H NMR segmental order parameters (S(CH) or S(CD)) and spin-lattice (Zeeman) relaxation times (T(1Z)) are summarized in convenient tabular form for various saturated, unsaturated, and biological membrane phospholipids. Segmental order parameters give direct information about bilayer structural properties, including the area per lipid and volumetric hydrocarbon thickness. In addition, relaxation rates provide complementary information about molecular dynamics. Particular attention is paid to the magnetic field dependence (frequency dispersion) of the NMR relaxation rates in terms of various simplified power laws. Model-free reduction of the T(1Z) studies in terms of a power-law formalism shows that the relaxation rates for saturated phosphatidylcholines follow a single frequency-dispersive trend within the MHz regime. We show how analytical models can guide the continued development of atomistic and coarse-grained force fields. Our interpretation suggests that lipid diffusion and collective order fluctuations are implicitly governed by the viscoelastic nature of the liquid-crystalline ensemble. Collective bilayer excitations are emergent over mesoscopic length scales that fall between the molecular and bilayer dimensions, and are important for lipid organization and lipid-protein interactions. Future conceptual advances and theoretical reductions will foster understanding of biomembrane structural dynamics through a synergy of NMR measurements and molecular simulations. Copyright © 2010 Elsevier B.V. All

  2. Sup(1)H n.m.r. relaxation of radiation induced crosslinking in polyester-styrene systems

    International Nuclear Information System (INIS)

    Andreis, M.; Veksli, Z.; Ranogajec, F.; Hedvig, P.

    1989-01-01

    The structure and dynamics of a network formed by radiation induced crosslinking of polyesters based on 1,6-hexane diol and 1,2-propylene glycol and maleic anhydride (HDF and PGF, respectively) with styrene is studied by proton pulsed n.m.r. spectroscopy. The dependence of spin-lattice, T 1 , and spin-spin, T 2 , relaxation times on the structure of polyester chain, molar ratios of styrene to polyester unsaturations and the radiation doses are analysed in terms of network formation and structure, and their effect on molecular motion. Above the gel point, at temperatures above the glass transition, the presence of two T 2 components reflects the heterogeneity of the network structure in both resins. Parallel with the n.m.r. relaxation measurements the crosslink density was determined from the extracted gel phase or double bonds (fumaric and styrene) participating in the crosslinking process. (author)

  3. Whole-core analysis by 13C NMR

    International Nuclear Information System (INIS)

    Vinegar, H.J.; Tutunjian, P.N.; Edelstein, W.A.; Roemer, P.B.

    1991-01-01

    This paper reports on a whole-core nuclear magnetic resonance (NMR) system that was used to obtain natural abundance 13 C spectra. The system enables rapid, nondestructive measurements of bulk volume of movable oil, aliphatic/aromatic ratio, oil viscosity, and organic vs. carbonate carbon. 13 C NMR can be used in cores where the 1 H NMR spectrum is too broad to resolve oil and water resonances separately. A 5 1/4-in. 13 C/ 1 H NMR coil was installed on a General Electric (GE) CSI-2T NMR imager/spectrometer. With a 4-in.-OD whole core, good 13 C signal/noise ratio (SNR) is obtained within minutes, while 1 H spectra are obtained in seconds. NMR measurements have been made of the 13 C and 1 H density of crude oils with a wide range of API gravities. For light- and medium-gravity oils, the 13 C and 1 H signal per unit volume is constant within about 3.5%. For heavy crudes, the 13 C and 1 H density measured by NMR is reduced by the shortening of spin-spin relaxation time. 13 C and 1 H NMR spin-lattice relaxation times were measured on a suite of Cannon viscosity standards, crude oils (4 to 60 degrees API), and alkanes (C 5 through C 16 ) with viscosities at 77 degrees F ranging from 0.5 cp to 2.5 x 10 7 cp. The 13 C and 1 H relaxation times show a similar correlation with viscosity from which oil viscosity can be estimated accurately for viscosities up to 100 cp. The 13 C surface relaxation rate for oils on water-wet rocks is very low. Nonproton decoupled 13 C NMR is shown to be insensitive to kerogen; thus, 13 C NMR measures only the movable hydrocarbon content of the cores. In carbonates, the 13 C spectrum also contains a carbonate powder pattern useful in quantifying inorganic carbon and distinguishing organic from carbonate carbon

  4. NMR imaging

    International Nuclear Information System (INIS)

    Andrew, E.R.

    1983-01-01

    Since hydrogen is the most abundant element in all living organisms, proton NMR lends itself well as a method of investigation in biology and medicine. NMR imaging has some special advantages as a diagnostic tool: no ionizing radiation is used, it is noninvasive; it provides a safer means of imaging than the use of x-rays, gamma rays, positrons, or heavy ions. In contrast with ultrasound, the radiation penetrates the bony structures without attenuation. In additional to morphological information, NMR imaging provides additional diagnostic insights through relaxation parameters, which are not available from other imaging methods. In the decade since the first primitive NMR images were obtained, the quality of images now obtained approaches those from CT x-ray scanners. Prototype instruments are being constructed for clinical evaluation and the first whole-body scanners are beginning to appear on the market at costs comparable to CT scanners. Primary differences in equipment for conventional NMR and NMR imaging are the much larger aperture magnets that are required for the examination of human subjects and the addition of coils to generate field gradients and facilities for manipulating the gradients. Early results from clinical trials in many parts of the world are encouraging, and in a few years, the usefuleness of this modality of medical imaging to the medical profession in diagnosis and treatment of disease will be defined. 10 figures

  5. 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

    to the different temperature dependence of their isotropic shifts. An activation energy of 6.3(4) kJ/mol is determined for the D3O+ motion in the isostructural compound D3OAl3(SO4)2(OD)6. Our NMR results support theories that ascribes the spin glass behavior of (H3O)Fe3(SO4)2(OD)6 is to disorder of the D3O+ ion...... and/or a less distorted Fe coordination environment. No sign of proton transfer reactions from the D3O+ ion to the framework is observed....

  6. Minimization of spin-lattice relaxation time with highly viscous solvents for acquisition of natural abundance nitrogen-15 and silicon-29 nuclear magnetic resonance spectra

    International Nuclear Information System (INIS)

    Bammel, B.P.; Evilia, R.F.

    1982-01-01

    The use of high viscosity solution conditions to decrease T 1 of 15 N and 29 Si nuclei so that natural abundance NMR spectra can be acquired in reasonable times is illustrated. Significant T 1 decreases with negligible increases in peak width are observed. No spectral shifts are observed in any of the cases studied. Highly viscous solutions are produced by using glycerol as a solvent for water-soluble molecules and a mixed solvent consisting of toluene saturated with polystyrene for organic-soluble molecules. The microviscosity in the latter solvent is found to be much less than the observed macroviscosity. Hydrogen bonding of glycerol to the NH 2 of 2-aminopyridine results in a greater than predicted decrease in T 1 for this nitrogen. The technique appears to be a useful alternative to paramagnetic relaxation reagents

  7. Sensitivity enhancement of 13C nuclei in 2D J-resolved NMR spectroscopy using a recycled-flow system

    International Nuclear Information System (INIS)

    Ha, S.T.K.; Lee, R.W.K.; Wilkins, C.L.

    1987-01-01

    Recycled-flow nuclear magnetic resonance for sensitivity enhancement in 1/2 spin nuclei has been reported previously, achieving several-fold signal enhancement. The success of the method depends upon premagnetization of nuclei prior to flowing into the detector region, obviating the need for delays following data acquisition to allow spin-lattice relaxation and reduce experiment time. The actual gains of sensitivity enhancement for 13 C- 1 H 2D J-resolved NMR using a recycled-flow method are evaluated. Possible enhancements for two types of J-resolved measurements, namely, one-bond 13 C- 1 H and long range J-resolved spectroscopy, are estimated using a simple Carr-Purcell spin-echo approach to quantify the 13 C signals. The pulse sequence is simply 90 0 -t /sub 1/2/-180 0 -t/sub 1/2/-AT-t/sub d/, where t/sub 1/2/ is half the evolution time, AT is the acquisition time, and t/sub d/ the experiment repetition time. In a static 2D NMR experiment, t/sub d/ usually must be the same order of the longest spin-lattice relaxation time (T 1 ) of nuclei. Quantitative measurements using a recycled-flow system indicate t/dub d/ can be reduced to a fraction of T 1 ; hence significant time savings can be achieved. Time-savings of between 2 and 25 can be anticipated for 2D spectroscopy under flow measurement conditions used in the present study. Other types of 2D NMR spectroscopy (autocorrelation and double quantum NMR) are discussed

  8. Evaluation of PHB nanocomposite by low field NMR

    International Nuclear Information System (INIS)

    Silva, Mariana Bruno Rocha e; Tavares, Maria Ines Bruno

    2009-01-01

    Poly(3-hydroxybutyrate) (PHB) based on nanocomposites containing different amounts of a commercial organically modified clay (viscogel B8) were prepared employing solution intercalation method. The relationship among the processing conditions; molecular structure and intermolecular interaction, between both nanocomposite components, were investigated using a nuclear magnetic resonance (NMR), as a part of characterization methodology, which has been used by Tavares et al. It involves the proton spin-lattice relaxation time, T1 H, by solid state nuclear magnetic resonance, employing low field NMR. X-ray diffraction was also employed because it is a conventional technique, generally used to obtain the first information on nanocomposite formation. Changes in PHB crystallinity were observed after the organophilic nanoclay had been incorporated in the polymer matrix. These changes, in the microstructure, were detected by the variation of proton nuclear relaxation time values and by X-ray, which showed an increase in the clay interlamellar space due to the intercalation of the polymer in the clay between lamellae. (author)

  9. Comparative NMR investigation of the Re-based borides

    Science.gov (United States)

    Lue, C. S.; Tao, Y. F.; Su, T. H.

    2008-07-01

    We report a systematic study of the rhenium-based borides, ReB2 , Re7B3 , and Re3B , by means of the B11 nuclear magnetic resonance (NMR) spectroscopy. While Re7B3 and Re3B are superconductors, ReB2 exhibits no superconducting signature but is of current interest due to its superhard mechanical property. Since the major focus of this investigation is their electronic characteristics in the normal states, we performed the measurements at temperatures between 77 and 295 K. For Re7B3 and Re3B , s -character electrons were found to be responsible for the observed B11 NMR Knight shift and spin-lattice relaxation rate (1/T1) . From T1 analysis, we thus deduce the partial Bs Fermi-level density of states (DOS) of both borides. On the other hand, the relaxation rate of ReB2 is mainly associated with p electrons, similar to the cases of OsB2 and RuB2 . In addition, the extracted B2p Fermi-level DOS is in good agreement with the theoretical prediction from band-structure calculations.

  10. NMR study of magnetic properties in filled skutterudite compound EuRu4P12

    International Nuclear Information System (INIS)

    Magishi, Ko-ichi; Iwahashi, Yoshinori; Horimoto, Takuji; Sugawara, Hitoshi; Saito, Takahito; Koyama, Kuniyuki

    2007-01-01

    We report the results of 31 P NMR measurements on a Eu-based filled skutterudite phosphide EuRu 4 P 12 with ferromagnetic transition at T C =18K in order to investigate the magnetic properties from a microscopic point of view. The temperature dependence of the Knight shift is similar to that of the magnetic susceptibility. Also, the nuclear spin-lattice relaxation rate 1/T 1 is practically constant at higher temperatures above 50K due to the interaction of the 31 P nucleus with fluctuating local moments at the Eu 2+ sites, but decreases rapidly at low temperatures below T C , indicating the supression of the spin fluctuations by magnetic ordering

  11. Tunneling splitting of magnetic levels in Fe8 detected by 1H NMR cross relaxation

    OpenAIRE

    Furukawa, Y.; Aizawa, K.; Kumagai, K.; Ullu, R.; Lascialfari, A.; Borsa, F.

    2003-01-01

    Measurements of proton NMR and the spin lattice relaxation rate 1/T1 in the octanuclear iron (III) cluster [Fe8(N3C6H15)6O2(OH)12][Br8 9H2O], in short Fe8, have been performed at 1.5 K in a powder sample aligned along the main anisotropy z axis, as a function of a transverse magnetic field (i.e., perpendicular to the main easy axis z). A big enhancement of 1/T1 is observed over a wide range of fields (2.5-5 T), which can be attributed to the tunneling dynamics; in fact, when the tunneling spl...

  12. Observation of isolated carbon atoms and the study of their mobility on Pt clusters by NMR

    International Nuclear Information System (INIS)

    Wang, P.; Ansermet, J.; Slichter, C.P.; Sinfelt, J.H.

    1985-01-01

    The authors have used NMR to determine the structure of surface species after the C-C bond scission of adsorbed acetylene and ethylene on Pt clusters produced by heating the samples to 690 K. They have found the species to be predominantly isolated carbon atoms adsorbed on Pt surfaces. They have studied the mobility of adsorbed carbon atoms from motional narrowing of the 13 C line shapes and motion-induced shortening of the spin-lattice relaxation times. They have found that the carbon atoms on Pt clusters are very mobile, their activation energy of 7 +- 1 kcal/mole for translational motion being less than half that of CO on Pt clusters

  13. 87Rb-NMR in Rb2ZnCl4 below the incommensurable phase

    International Nuclear Information System (INIS)

    Grande, S.; Moskvich, Yu.N.; Aleksandrova, I.P.

    1983-01-01

    In Rb 2 ZnCl 4 crystals the curly polar phase, which changes into the incommensurable phase below 192 K, has been investigated by pulsed NMR. The angular correlations of the second-order quadrupole shifts have been measured and the corresponding tensors of the electric field gradient have been calculated. The six Rb layers change differently in magnitude and orientation compared to the paraelectric phase. The temperature dependences within the C-phase are also different. The spin-lattice relaxation times have been measured and discussed for each layer in the C-phase. All relaxation times show an anomaly at a further phase transition occurring at 72 K connected with an increase of the number of spectral lines

  14. Use of a paramagnetic substance, colloidal manganese sulfide, as an NMR contrast material in rats

    Energy Technology Data Exchange (ETDEWEB)

    Chilton, H.M.; Jackels, S.C.; Hinson, W.H.; Ekstrand, K.E.

    1984-05-01

    To determine whether an insoluble magnetopharmaceutical might be useful in such service, the authors investigated the effect of a colloidal preparation of manganese sulfide (MnSC) upon liver and lung spin-lattice relaxation time (T/sub 1/) in rats following intravenous administration. NMR tissue sample measurements were made at 24 MHz, and showed that after MnSC treatment, liver T/sub 1/ values - and to a lesser extent lung T/sub 1/ values - were depressed below control values. Liver manganese content (as determined by flame atomic absorption spectrophotometry) increased in proportion to the dose of MnSC, and the reciprocal of the liver T/sub 1/ values also increased in proportion to the dose of MnSC.

  15. Monovacancy paramagnetism in neutron-irradiated graphite probed by 13C NMR.

    Science.gov (United States)

    Zhang, Z T; Xu, C; Dmytriieva, D; Molatta, S; Wosnitza, J; Wang, Y T; Helm, M; Zhou, Shengqiang; Kühne, H

    2017-10-20

    We report on the magnetic properties of monovacancy defects in neutron-irradiated graphite, probed by 13 C nuclear magnetic resonance spectroscopy. The bulk paramagnetism of the defect moments is revealed by the temperature dependence of the NMR frequency shift and spectral linewidth, both of which follow a Curie behavior, in agreement with measurements of the macroscopic magnetization. Compared to pristine graphite, the fluctuating hyperfine fields generated by the defect moments lead to an enhancement of the 13 C nuclear spin-lattice relaxation rate [Formula: see text] by about two orders of magnitude. With an applied magnetic field of 7.1 T, the temperature dependence of [Formula: see text] below about 10 K can well be described by a thermally activated form, [Formula: see text], yielding a singular Zeeman energy of ([Formula: see text]) meV, in excellent agreement with the sole presence of polarized, non-interacting defect moments.

  16. 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

    2017-03-01

    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.

  17. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

    Energy Technology Data Exchange (ETDEWEB)

    Mandal, Abhishek; Boatz, Jennifer C. [University of Pittsburgh School of Medicine, Department of Structural Biology (United States); Wheeler, Travis B. [University of Pittsburgh School of Medicine, Department of Cell Biology (United States); Wel, Patrick C. A. van der, E-mail: vanderwel@pitt.edu [University of Pittsburgh School of Medicine, Department of Structural Biology (United States)

    2017-03-15

    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.

  18. 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.

  19. NMR spectroscopy study of agar-based polymers electrolytes

    Energy Technology Data Exchange (ETDEWEB)

    Mattos, R.I.; Tambelli, C.E. [Universidade de Sao Paulo (USP), Pirassununga, SP (Brazil). Fac. de Zootecnia e Engenharia de Alimentos; Raphael, E. [Universidade Federal de Sao Joao del-Rey (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Silva, I.D.A.; Magon, C.J.; Donoso, J.P. [Universidade de Sao Paulo (IFSC/USP), Sao Carlos, SP (Brazil). Inst. de Fisica

    2012-07-01

    Full text: This communication presents the results of preparation and characterization of transparent films obtained from agar and acetic acid. The films were characterized by electrochemical impedance spectroscopy (EIS) and nuclear magnetic resonance (NMR). The film formed by agar (Sigma Aldrich) was dispersed in water and kept under stirring and heating at 100 deg C. Next, glycerol, formaldehyde and different quantities of acetic acid (25 and 50 wt%) were added to this solution. The obtained solution was placed on a glass plate and left to dry for 48 hours in oven at 50 deg C to obtain the films, which were kept under vacuum before characterization. The ionic conductivity of the films display an Arrhenius behavior with activation energy E{sub a} = 78 (25 wt% of acetic acid) and E{sub a} = 87 kJ/mol (50 wt% of acetic acid). The conductivity values were 3:0 X 10{sup -6} and 1:2 X 10{sup -4} S/cm at room temperature and 4:4 X 10{sup -4} and 1:5 X 10{sup -3}S/cm at 70 deg C, for the 25 and 50 wt% of acetic acid respectively. To investigate the mechanism of protonic conduction in the polymer proton conductor proton NMR measurements were performed in the temperature range 200-370 K. The {sup 1}H-NMR results exhibit the qualitative feature associated with the proton mobility, namely the presence of well defined {sup 1}H spin-lattice relaxation maxima at 300 K. Activation energy of the order of 40 kJ/mol was obtained from the {sup 1}H-NMR line narrowing data. The ionic conductivity of the film combined with their transparency, flexibility, homogeneity and good adhesion to the glasses or metals indicate that agar-based SPEs are promising materials for used on optoelectronic applications. (author)

  20. Perspective of MAS in Power System via a Fuzzy Framework

    Directory of Open Access Journals (Sweden)

    S. Razini

    2017-03-01

    Full Text Available Multi agent systems (MAS are popularly used in practice, however; a few studies have looked at MAS capabilities from the power engineering perspective. This paper presents the results of an investigation concerning the compatibility of MAS capabilities in different power engineering categories. Five MAS capabilities and seven power system categories are established. A framework for applying MAS in power engineering is developed. A fuzzy inference system is adopted to evaluate the paper proposed framework. Two approaches, namely simulation and real, are considered for different power categories. The paper shows that MAS capabilities are generally compatible with both approaches, although compatibility of MAS with real approach is more significant. The paper concludes that in the near future MAS is anticipated to be a key important tool in the development of intelligent systems and smart grids in power system. This paper contributes to thinking on perspective of MAS in power System.

  1. NMR-CT in muscular disorders

    International Nuclear Information System (INIS)

    Matsumura, Kiichiro; Nakano, Imaharu; Fukuda, Nobuo; Ikehira, Hiroo; Tateno, Yukio.

    1987-01-01

    Proton NMR-CT (magnetic field strength 0.1 Tesla, resonant frequency 4.5 MHz) was performed in 10 normal females and 19 Duchenne muscular dystrophy (DMD) carriers. The mean age was 39 ± 12 years for the normal females and 42 ± 6 years for the DMD carriers. In DMD carriers, there were 4 definite, 4 probable, and 11 possible carriers. T 1 (spin-lattice relaxation time) image was obtained for a slice at the buttock, mid-thigh and calf levels respectively. T 1 values were measured for the medial portion of the gluteus maximus, the vastus lateralis of the quadriceps femoris, and the gastrocnemius. The bound water fraction (BWF) was calculated from Fullerton's equation based on the fast proton diffusion model. The following results were obtained: (1) In normal females, muscle T 1 value was highest in the gastrocnemius and lowest in the gluteus maximus. (2) In DMD carriers, T 1 values of the gluteus maximus and quadriceps femoris were significantly higher than those of the normal females. There was, however, no significant difference in T 1 value of the gastrocnemius between DMD carriers and normal females. (3) In DMD carriers, BWFs of the gluteus maximus and quadriceps femoris were significantly lower than those of the normal females. (4) In DMD carriers, no significant correlation was observed between the muscle T 1 values and the serum creatine phosphokinase values. Increased tissue water content in the lower parts of the body due to gravity is considered to be the primary cause of the high T 1 value in the gastrocnemius of normal females. The presence of the degenerating muscle fibers are presumed responsible for the high T 1 value and low BWF in the proximal muscles of DMD carriers. (author)

  2. NMR imaging

    International Nuclear Information System (INIS)

    Ouchi, Toshihiro; Steiner, R.E.

    1984-01-01

    Three epidermoid and two dermoid tumours, pathologically proven, were examined by NMR and CT scans. Although most brain tumours have a low signal with a long T 1 , a dermoid cyst and one of the two components of the other dermoid tumour had a high signal and therefore a short T 1 . All three epidermoid tumours had a low signal and a long T 1 . Because of the high level contrast between some of the tumours and cerebrospinal fluid, NMR is helpful to detect the lesion. Neither of the liquid fluid levels in the tumour cysts or floating fat in the subarachnoid space was recognized in one patients, but the fine leakage of the content from the epidermoid cyst into the lateral ventricle was detected on a saturation recovery 1000 image in one case. (author)

  3. Hyperpolarized 129Xe as an NMR probe for functional studies

    International Nuclear Information System (INIS)

    Wolber, J.

    2000-01-01

    The nuclear spin polarization of 129 Xe can be enhanced by several orders of magnitude using optical pumping techniques, resulting in a dramatic enhancement of the 129 Xe Nuclear Magnetic Resonance (NMR) signal. The 'hyperpolarized' gas can be used for Magnetic Resonance Imaging (MRI) of the void spaces of the lungs after introduction of the gas into the respiratory system. Furthermore, the high solubility of xenon in blood and lipids suggests the use of 129 Xe NMR for studying blood flow, permeability, perfusion and blood volume. Hyperpolarized 129 Xe MRI has the potential of combining the high sensitivity and functional information of radioactive tracer studies with the high spatial and temporal resolution of MRI. The spin-lattice relaxation time T 1 of 129 Xe in blood determines the loss of polarization during transit from the lungs to the tissue of interest. A difference in the relaxation times of xenon in oxygenated and deoxygenated blood could be used as a contrast mechanism in functional Magnetic Resonance Imaging (fMRI). In this thesis, the hyperpolarized 129 Xe T 1 in human blood is measured in vitro as a function of blood oxygenation, and the relevant relaxation mechanisms are discussed. A new and unexpected finding is that the hyperpolarized 129 Xe NMR spectrum in blood is highly sensitive to blood oxygenation. Therefore, hyperpolarized 129 Xe NMR provides a powerful means of measuring blood oxygenation quantitatively and non-invasively. The interaction of xenon with hemoglobin is responsible for an oxygen-dependent shift of the 129 Xe NMR resonance of xenon in red blood cells. Injection delivery of hyperpolarized 129 Xe in solution could be a more efficient method of administrating the gas for functional NMR studies. For this purpose, suitable biocompatible carrier media have been studied. In particular, the use of perfluorocarbon emulsions, which are already in use as blood substitutes, as delivery media for hyperpolarized 129 Xe has been investigates

  4. 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.

  5. NMR Study of the S=1/2 Quantum Kagome Lattice Antiferromagnet [Cu_3(titmb)_2(CH_3CO_2)_6]・H_2O(Frustrated Systems, Field-Induced Phase Transitions and Dynamics in Quantum Spin Systems)

    OpenAIRE

    Satoru, MAEGAWA; Kenji, YOSHIOKA; Shinichi, KAWAHARA; Akira, OYAMADA; Kenichi, FUJITA; Ryohei, YAMAGUCHI; Graduate School of Human and Environmental Studies, Kyoto University; Graduate School of Human and Environmental Studies, Kyoto University; Graduate School of Human and Environmental Studies, Kyoto University; Graduate School of Human and Environmental Studies, Kyoto University; Graduate School of Human and Environmental Studies, Kyoto University; Graduate School of Human and Environmental Studies, Kyoto University

    2005-01-01

    A quantum kagome lattice magnet, [Cu_3(titmb)_2(CH_3CO_2)_6]・H_2O with s=1/2 has been studied by magnetization and NMR experiments. No magnetic phase transition was observed down to 180mK. The spin-lattice relaxation rate T^_1 above 20K is almost temperature independent, while below 10K the rates decrease sharply as the temperature is decreased, and can be described as T^_1=B exp(-△/κ_BT). The field dependence on the energy gap △ has been obtained and is found to show plateaus between 3.2 and...

  6. NMR studies of spin excitations in superconducting Bi2Sr2CaCu2O8+δ single crystals

    Science.gov (United States)

    Takigawa, M.; Mitzi, D. B.

    1994-08-01

    The oxygen NMR shift and the Cu nuclear spin-lattice relaxation rate (1/T1) were measured in Bi2.1Sr1.9Ca0.9Cu2.1O8+δ single crystals. While both the shift and 1/(T1T) decrease sharply near Tc, 1/(T1T) becomes nearly constant at low temperatures, indicating a gapless superconducting state with finite density of states at the Fermi level. From the oxygen shift data, the residual spin susceptibility at T=0 is estimated to be 10% of the value at room temperature. Our results are most consistent with a d-wave pairing model with strong (resonant) impurity scattering.

  7. Study of paramagnetic contrast agents for NMR imaging: theoretical and experimental aspects (the case of Mn2+ ion)

    International Nuclear Information System (INIS)

    Chavoix, M.E.

    1984-06-01

    The use of contrast enhancing agents and the evaluation of magnetic properties of tissues, extend the diagnostic usefulness of Nuclear Magnetic Resonance (NMR) imaging. From this point of view, proton T 1 (spin-lattice) relaxation times of rat tissue, following parenteral administration of Mn(II) to increase the relaxation rate (R 1 =1/T 1 ), have been studied at 20 MHz. Differenciation of free (MF) and bound (Mb) manganese in these tissues was thus determined by measuring, total exogenous Mn ++ ions by Atomic Absorption spectrometry and free (non protein complexed) ions by Electron Spin Resonance Analysis. From these results, the diffusion of Mn ++ into various organs, was evaluated 15 min. after injection. A significant difference in the fixation of manganese occured between the liver and the pancreas with uptakes of 50% and 1% of the administration dose respectively [fr

  8. First order magnetic transition in single crystal CaFe2As2 detected by 75As NMR

    Energy Technology Data Exchange (ETDEWEB)

    Baek, Seung Ho [Los Alamos National Laboratory; Curro, Nicholas J [UC - DAVIS

    2008-01-01

    We report {sup 75}As Nuclear Magnetic Resonance data in a single crystal of CaFe{sub 2}As{sub 2}. The Knight shift, the electric field gradient, and the spin lattice relaxation rate are strongly temperature dependent in the paramagnetic state, and change discontinuously at the structural transition temperature, T{sub S} = T{sub N} = 167 K. Immediately below, the NMR spectra reveal an internal field at the As site associated with the presence of a commensurate magnetic order. These results indicate that the structural and magnetic transitions in CaFe{sub 2}As{sub 2} are first order and strongly coupled, and that the electron density in the FeAs plane is highly sensitive to the out-of-plane structure.

  9. Transport and NMR characteristics of the skutterudite-related compound Ca3Rh4Sn13

    Science.gov (United States)

    Tseng, C. W.; Kuo, C. N.; Li, B. S.; Wang, L. M.; Gippius, A. A.; Kuo, Y. K.; Lue, C. S.

    2018-02-01

    We report the electronic properties of the Yb3Rh4Sn13-type single crystalline Ca3Rh4Sn13 by means of the electrical resistivity, Hall coefficient, Seebeck coefficient, thermal conductivity, as well as 119Sn nuclear magnetic resonance (NMR) measurements. The negative sign of the Hall coefficient and Seebeck coefficient at low temperatures suggests that the n-type carriers dominate the electrical transport in Ca3Rh4Sn13, in contrast to the observations in Sr3Rh4Sn13 which has a p-type conduction. Such a finding indicates a significant difference in the electronic features between these two stannides. Furthermore, we analyzed the temperature-dependent 119Sn NMR spin-lattice relaxation rate for Ca3Rh4Sn13, (Sr0.7Ca0.3)3Rh4Sn13, and Sr3Rh4Sn13 to examine the change of the electronic Fermi-level density of states (DOS) in (Sr1-xCax)3Rh4Sn13. It indicates that the Sn 5s partial Fermi-level DOS enhances with increasing the Ca content, being consistent with the trend of the superconducting temperature. Since the total Fermi-level DOS usually obeys the same trend of the partial Fermi-level DOS, the NMR analysis provides microscopic evidence for the correlation between the electronic DOS and superconductivity of the (Sr1-xCax)3Rh4Sn13 system.

  10. Characterization of polyurethane/organophilic montmorillonite nanocomposites by low field NMR

    International Nuclear Information System (INIS)

    Silva, Marcos Anacleto da; Tavares, Maria I.B.; Nascimento, Suelen A.M.; Rodrigues, Elton J. da R

    2012-01-01

    Polyurethanes are important and versatile materials, mainly due to some of their properties, such as high resistance to abrasion and tearing, excellent absorption of mechanical shocks and good flexibility and elasticity. However, they have some drawbacks as well, such as low thermal stability and barrier properties. To overcome these disadvantages, various studies have been conducted involving organophilic polyurethane/montmorillonite nanocomposites. The investigation of the structure of polyurethane/clay nanocomposites has mainly been done by X-ray diffraction (XRD) and transmission electron microscopy (TEM). In this work, PU/clay nanocomposite films obtained by solution intercalation were studied. The nanocomposites were characterized by XRD and low-field nuclear magnetic resonance (LF-NMR). The LF-NMR measurements, with determination of the spin-lattice relaxation time of the hydrogen nucleus, supplied important information about the molecular dynamics of these nanocomposites. The X-ray diffraction measurements validated the results found by NMR. The thermal stability of the material was also determined by thermogravimetric analysis (TGA) under an inert atmosphere. A slight improvement in this stability was observed in the nanocomposite in comparison with polyurethane (author)

  11. NMR evidence of charge fluctuations in multiferroic CuBr2

    Science.gov (United States)

    Wang, Rui-Qi; Zheng, Jia-Cheng; Chen, Tao; Wang, Peng-Shuai; Zhang, Jin-Shan; Cui, Yi; Wang, Chao; Li, Yuan; Xu, Sheng; Yuan, Feng; Yu, Wei-Qiang

    2018-03-01

    We report combined magnetic susceptibility, dielectric constant, nuclear quadruple resonance (NQR), and zero-field nuclear magnetic resonance (NMR) measurements on single crystals of multiferroics CuBr2. High quality of the sample is demonstrated by the sharp magnetic and magnetic-driven ferroelectric transition at {T}{{N}}={T}{{C}}≈ 74 K. The zero-field 79Br and 81Br NMR are resolved below T N. The spin-lattice relaxation rates reveal charge fluctuations when cooled below 60 K. Evidences of an increase of NMR linewidth, a reduction of dielectric constant, and an increase of magnetic susceptibility are also seen at low temperatures. These data suggest an emergent instability which competes with the spiral magnetic ordering and the ferroelectricity. Candidate mechanisms are discussed based on the quasi-one-dimensional nature of the magnetic system. Project supported by the Ministry of Science and Technology of China (Grant No. 2016YFA0300504), the National Natural Science Foundation of China (Grant No. 11374364), the Fundamental Research Funds for the Central Universities of China, and the Research Funds of Renmin University, China (Grant No. 14XNLF08).

  12. Solid-state NMR paramagnetic relaxation enhancement immersion depth studies in phospholipid bilayers

    KAUST Repository

    Chu, Shidong

    2010-11-01

    A new approach for determining the membrane immersion depth of a spin-labeled probe has been developed using paramagnetic relaxation enhancement (PRE) in solid-state NMR spectroscopy. A DOXYL spin label was placed at different sites of 1-palmitoyl-2-stearoyl-sn-glycero-3-phosphocholine (PSPC) phospholipid bilayers as paramagnetic moieties and the resulting enhancements of the longitudinal relaxation (T1) times of 31P nuclei on the surface of the bilayers were measured by a standard inversion recovery pulse sequence. The 31P NMR spin-lattice relaxation times decrease steadily as the DOXYL spin label moves closer to the surface as well as the concentration of the spin-labeled lipids increase. The enhanced relaxation vs. the position and concentration of spin-labels indicate that PRE induced by the DOXYL spin label are significant to determine longer distances over the whole range of the membrane depths. When these data were combined with estimated correlation times τc, the r-6-weighted, time-averaged distances between the spin-labels and the 31P nuclei on the membrane surface were estimated. The application of using this solid-state NMR PRE approach coupled with site-directed spin labeling (SDSL) may be a powerful method for measuring membrane protein immersion depth. © 2010 Elsevier Inc. All rights reserved.

  13. Structure and motion of phospholipids in human plasma lipoproteins. A 31P NMR study

    International Nuclear Information System (INIS)

    Fenske, D.B.; Chana, R.S.; Parmar, Y.I.; Treleaven, W.D.; Cushley, R.J.

    1990-01-01

    The structure and motion of phospholipids in human plasma lipoproteins have been studied by using 31 P NMR. Lateral diffusion coefficients, D T , obtained from the viscosity dependence of the 31 P NMR line widths, were obtained for very low density lipoprotein (VLDL), low-density lipoprotein (LDL), high-density lipoproteins (HDL 2 , HDL 3 ), and egg PC/TO microemulsions at 25 degree C, for VLDL at 40 degree C, and for LDL at 45 degree C. In order to prove the orientation and/or order of the phospholipid head-group, estimates of the residual chemical shift anistropy, Δσ, have been obtained for all the lipoproteins and the microemulsions from the viscosity and field dependence for the 31 P NMR line widths. These results suggest differences in the orientation and/or ordering of the head-group in the HDLs. The dynamic behavior of the phosphate moiety in LDL and HDL 3 has been obtained from the temperature dependence of the 31 P spin-lattice relaxation rates. Values of the correlation time for phosphate group reorientation and the activation energy for the motion are nearly identical in LDL and HDL 3 and are similar to values obtained for phospholipid bilayers. This argues against long-lived protein-lipid interactions being the source of either the slow diffusion in LDL or the altered head-group orientation in the HDLs

  14. Sensitivity and Resolution Enhanced Solid-State NMR for Paramagnetic Systems and Biomolecules under Very Fast Magic Angle Spinning

    KAUST Repository

    Parthasarathy, Sudhakar; Nishiyama, Yusuke; Ishii, Yoshitaka

    2013-01-01

    Recent research in fast magic angle spinning (MAS) methods has drastically improved the resolution and sensitivity of NMR spectroscopy of biomolecules and materials in solids. In this Account, we summarize recent and ongoing developments

  15. Applications of 1H-NMR relaxometry in experimental liver studies

    International Nuclear Information System (INIS)

    Holzmueller, P.

    1992-01-01

    Purpose of this study was to investigate applications of proton nuclear magnetic resonance ( 1 H-NMR) relaxometry in experimental medicine. Relaxometry was performed by measurements of spin-lattice (T 1 ) and spin-spin (T 2 ) relaxation time parameters on liver biopsies up to four hours after biopsy excision. Variations of relaxation times due to species and strain, different sample handling and different liver damage models, ethionine fatty liver and paracetamol liver necrosis, were investigated. Cell integrity effects were studied on homogenized liver samples. Relaxation time parameters, especially 'main' components T 1A and T 2A of biexponential model fit, were identified to react very sensitive after tissue damages as well as to cell viability. Thus, investigation of stored liver grafts was performed in order to evaluate the possibility of a rapid liver graft viability testing method for human liver transplantation surgery by 1 H-NMR relaxometry. Another series of measurements was performed to investigate the applicability of isoflurane anesthesia for in vivo NMR experiments. This study proved the good appropriateness of isoflurane for that purpose provided that physiological monitoring and individual adjustment of anesthesia are performed. In these investigations it could be revealed that mainly T 1A and T 2A are influenced by tissue condition and that different information is inherent in these two parameters, with T 2A reflecting tissue viability and changes of tissue conditions very sensitively but rather unspecifically in respect to the damage applied. Based on these results the following future applications of 1 H-NMR relaxometry are suggested : (1) model investigations, (2) investigation of given pathologies, (3) investigation of basic requirements for in vivo NMR and (4) application in a liver graft viability testing protocol, which seems to be the most important future application of 1 H-NMR relaxometry in medicine. (author)

  16. NMR spectroscopy

    International Nuclear Information System (INIS)

    Gruenert, J.

    1989-01-01

    The book reviews the applications of NMR-spectroscopy in medicine and biology. The first chapter of about 40 pages summarizes the history of development and explains the chemical and physical fundamentals of this new and non-invasive method in an easily comprehensible manner. The other chapters summarize diagnostic results obtained with this method in organs and tissues, so that the reader will find a systematic overview of the available findings obtained in the various organ systems. It must be noted, however, that ongoing research work and new insight quite naturally will necessitate corrections to be done, as is the case here with some biochemical interpretations which would need adjustment to latest research results. NMR-spectroscopy is able to measure very fine energy differences on the molecular level, and thus offers insight into metabolic processes, with the advantage that there is no need of applying ionizing radiation in order to qualitatively or quantitatively analyse the metabolic processes in the various organ systems. (orig./DG) With 40 figs., 4 tabs [de

  17. Modification and intercalation of layered zirconium phosphates: a solid-state NMR monitoring.

    Science.gov (United States)

    Bakhmutov, Vladimir I; Kan, Yuwei; Sheikh, Javeed Ahmad; González-Villegas, Julissa; Colón, Jorge L; Clearfield, Abraham

    2017-07-01

    Several layered zirconium phosphates treated with Zr(IV) ions, modified by monomethoxy-polyethyleneglycol-monophosphate and intercalated with doxorubicin hydrochloride have been studied by solid-state MAS NMR techniques. The organic components of the phosphates have been characterized by the 13 C{ 1 H} CP MAS NMR spectra compared with those of initial compounds. The multinuclear NMR monitoring has provided to establish structure and covalent attachment of organic/inorganic moieties to the surface and interlayer spaces of the phosphates. The MAS NMR experiments including kinetics of proton-phosphorus cross polarization have resulted in an unusual structure of zirconium phosphate 6 combining decoration of the phosphate surface by polymer units and their partial intercalation into the interlayer space. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  18. Solid-state 13C magic angle spinning NMR spectroscopy characterization of particle size structural variations in synthetic nanodiamonds

    International Nuclear Information System (INIS)

    Alam, Todd M.

    2004-01-01

    Solid-state 13 C magic angle spinning (MAS) NMR spectroscopy has been used to quantify the different carbon species observed in synthetically produced nanodiamonds. Two different diamond-like carbon species were observed using 13 C MAS NMR, which have been attributed to a highly ordered crystalline diamond phase and a disordered crystalline diamond phase. The relative ratio of these different diamond phases was found to vary with the particle size of the nanodiamond materials

  19. Novel NMR tools to study structure and dynamics of biomembranes.

    Science.gov (United States)

    Gawrisch, Klaus; Eldho, Nadukkudy V; Polozov, Ivan V

    2002-06-01

    Nuclear magnetic resonance (NMR) studies on biomembranes have benefited greatly from introduction of magic angle spinning (MAS) NMR techniques. Improvements in MAS probe technology, combined with the higher magnetic field strength of modern instruments, enables almost liquid-like resolution of lipid resonances. The cross-relaxation rates measured by nuclear Overhauser enhancement spectroscopy (NOESY) provide new insights into conformation and dynamics of lipids with atomic-scale resolution. The data reflect the tremendous motional disorder in the lipid matrix. Transfer of magnetization by spin diffusion along the proton network of lipids is of secondary relevance, even at a long NOESY mixing time of 300 ms. MAS experiments with re-coupling of anisotropic interactions, like the 13C-(1)H dipolar couplings, benefit from the excellent resolution of 13C shifts that enables assignment of the couplings to specific carbon atoms. The traditional 2H NMR experiments on deuterated lipids have higher sensitivity when conducted on oriented samples at higher magnetic field strength. A very large number of NMR parameters from lipid bilayers is now accessible, providing information about conformation and dynamics for every lipid segment. The NMR methods have the sensitivity and resolution to study lipid-protein interaction, lateral lipid organization, and the location of solvents and drugs in the lipid matrix.

  20. Magnetic and structural properties of an octanuclear Cu(II) S=1/2 mesoscopic ring: Susceptibility and NMR measurements

    International Nuclear Information System (INIS)

    Lascialfari, A.; Jang, Z. H.; Borsa, F.; Gatteschi, D.; Cornia, A.; Rovai, D.; Caneschi, A.; Carretta, P.

    2000-01-01

    Magnetic susceptibility, 1 H NMR and 63 Cu NMR-NQR experiments on two slightly different species of the molecular S=1/2 antiferromagnetic (AF) ring Cu8, [Cu 8 (dmpz) 8 (OH) 8 ]·2C 5 H 5 N (Cu8P) and [Cu 8 (dmpz) 8 (OH) 8 ]·2C 5 H 5 NO 2 (Cu8N), are presented. The magnetic energy levels are calculated exactly for an isotropic Heisenberg model Hamiltonian in zero magnetic field. From the magnetic susceptibility measurements we estimate the AF exchange coupling constant J∼1000 K and the resulting gap Δ∼500 K between the S T =0 ground state and the S T =1 first excited state. The 63,65 Cu NQR spectra indicate the presence of four crystallographically inequivalent copper nuclei in each ring. From the combination of the 63 Cu NQR spectra and of the 63 Cu NMR spectra at high magnetic field, we estimate the quadrupole coupling constant v Q of each site and the average asymmetry parameter η of the electric-field gradient tensor. The nuclear spin-lattice relaxation rate (NSLR) decreases exponentially on decreasing temperature for all nuclei investigated. The gap parameter extracted from 63 Cu NQR-NSLR is the same as for the susceptibility while a smaller value is obtained from the 63 Cu NMR-NSLR in an external magnetic field of 8.2 T. (c) 2000 The American Physical Society

  1. Electron spin-lattice relaxation in fractals

    International Nuclear Information System (INIS)

    Shrivastava, K.N.

    1986-08-01

    We have developed the theory of the spin-fracton interaction for paramagnetic ions in fractal structures. The interaction is exponentially damped by the self-similarity length of the fractal and by the range dimensionality d Φ . The relaxation time of the spin due to the absorption and emission of the fracton has been calculated for a general dimensionality called the Raman dimensionality d R , which for the fractons differs from the Hausdorff (fractal) dimensionality, D, as well as from the Euclidean dimensionality, d. The exponent of the energy level separation in the relaxation rate varies with d R d Φ /D. We have calculated the spin relaxation rate due to a new type of Raman process in which one fracton is absorbed to affect a spin transition from one electronic level to another and later another fracton is emitted along with a spin transition such that the difference in the energies of the two fractons is equal to the electronic energy level separation. The temperature and the dimensionality dependence of such a process has been found in several approximations. In one of the approximations where the van Vleck relaxation rate for a spin in a crystal is known to vary with temperature as T 9 , our calculated variation for fractals turns out to be T 6.6 , whereas the experimental value for Fe 3+ in frozen solutions of myoglobin azide is T 6.3 . Since we used d R =4/3 and the fracton range dimensionality d Φ =D/1.8, we expect to measure the dimensionalities of the problem by measuring the temperature dependence of the relaxation times. We have also calculated the shift of the paramagnetic resonance transition for a spin in a fractal for general dimensionalities. (author)

  2. Proton and deuteron NMR study of PTFE ionomer membranes

    Energy Technology Data Exchange (ETDEWEB)

    Xu, G; Pak, Y S [Dept. of Materials Science, McMaster Univ., Hamilton, Ontario (Canada)

    1992-02-01

    Proton and deuteron NMR have been conducted to investigate the ionic motion in perfluorinated ionomer membranes from Dow Chemical (XUS) and DuPont (Nafion{sup R}). Two proton relaxation peaks were found in the XUS specimen absorbed with H{sub 2}O. The major (narrow) peak presented a spin-lattice relaxation time (T{sub 1}) of 107 ms while the minor (broader) one gave much longer T{sub 1}. While the former was attributed to the water molecules involved in restricted motion, the latter was expected to be associated with the protons located in the vicinity of the sulfonate groups. Similar to the previous results from the others, only a single peak was detected in Nafion{sup R} in {sup 1}H spectra, indicating that the protons in the different environments were engaging rapid exchange within NMR time scale. In contrast to the inverse proportion dependence of the linewidth on the water sorption in Nafion{sup R}, the major line of the XUS membrane exhibited insensitive linewidth dependence on the variation of H{sub 2}O concentration. The difference was attributed to the existence of narrow breaths of the pores in XUS sample, such that free water contribution to the enhancement of proton mobility was limited. The {sup 2}H spectra of Nafion{sup R} were found to possess a doublet, due to nuclear quadrupolar interaction. Dow (XUS) membrane treated in at 100% relative humidity (RH) D{sub 2}O presented a single peak with the linewidth insensitive to the amount of heavy water absorbed. An additional rise emerged on the ''shoulder'' of this single peak when treated at 33% RH. It is concluded that XUS membrane does not provide strong hydrogen bonding to eliminate the rapid motion average over the nuclear quadrupole interaction. (orig.).

  3. Nuclear spin phonon relaxation by Raman process in Na{sub 3}H(SO{sub 4}){sub 2} single crystals with the electric-quadrupole-type interaction using {sup 1}H and {sup 23}Na NMR

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Ae Ran [Department of Science Education, Jeonju University, Jeonju 560-759, Chonbuk (Korea, Republic of)], E-mail: aeranlim@hanmail.net; Shin, Chang Woo [Solid State Analysis Team, Korea Basic Science Institute, Daegu 702-701 (Korea, Republic of)

    2008-11-30

    Successive phase transitions in a Na{sub 3}H(SO{sub 4}){sub 2} single crystal were found at 296, 513, and 533 K. To investigate the mechanism of the phase transition at 296 K, the {sup 1}H and {sup 23}Na spin-lattice relaxation time and the spin-spin relaxation time of Na{sub 3}H(SO{sub 4}){sub 2} were measured near the phase transition temperature using a FT NMR spectrometer. The spin-lattice relaxation time, T{sub 1}, for {sup 1}H in Na{sub 3}H(SO{sub 4}){sub 2} crystals exhibits a minimum below T{sub C1} (=296 K) indicating the presence of distinct molecular motion governed by the Bloembergen-Purcell-Pound (BPP) theory. Although the results for the {sup 1}H and {sup 23}Na relaxation times provide no evidence of the phase transition at T{sub C1}, the separation of the {sup 23}Na resonance lines changes abruptly at T{sub C1}. The phase transition at 296 K produces a change in the separation of the Na resonance line that is associated with a change in the atomic positions in the vicinity of the Na ions. Also, the nuclear spin-lattice relaxation process in Na{sub 3}H(SO{sub 4}){sub 2} crystals with the electric-quadrupole-type interaction proceed via Raman process. These results are compared with those obtained for other M{sub 3}H(SO{sub 4}){sub 2} (M=K, Rb, and Cs) crystals, which have similar hydrogen-bonded structures.

  4. 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.

    quino- nes or semiquinones which exhibit 13C resonance at around 195 ppm. Free radicals of semiquinone type have been reported from the aquatic environment [2]. Spectra of all the four samples show absorption at 195 ppm. The total acidity of marine..., significant resonance at 55 ppm (8.9) from aromatic methoxy carbon suggests that phenol is present mostly as methyl ether and not as free phenol. The signal at 55 ppm is also attributed to aliphatic carbon adjacent to the amino functional group as in amino...

  5. HR-MAS NMR metabolomics of 'Swingle' citrumelo rootstock genetically modified to overproduce proline.

    Science.gov (United States)

    de Oliveira, Caroline S; Carlos, Eduardo F; Vieira, Luiz G E; Lião, Luciano M; Alcantara, Glaucia B

    2014-08-01

    The accumulation of proline is a typical physiological response to abiotic stresses in higher plants. 'Swingle' citrumelo, an important rootstock for citrus production, has been modified with a mutated Δ(1)-pyrroline-5-carboxylate synthetase gene (VaP5CSF129A) linked to the cauliflower mosaic virus 35S promoter to induce the overproduction of free proline. This paper presents a comparative metabolomic study of nontransgenic versus transgenic 'Swingle' citrumelo plants with high endogenous proline. (1)H high-resolution magic angle spinning nuclear magnetic resonance spectroscopy and multivariate analysis showed significant differences in some metabolites between the nontransgenic and transgenic leaves and roots. The overproduction of proline has reduced the sucrose content in transgenic leaves, revealing a metabolic cost for these plants. In roots, the high level of free proline acts for the adjustment of cation-anion balance, causing the reduction of acetic acid content. The same sucrose level in roots indicates that they can be considered as sucrose sink. Similar behavior may be waited for fruits produced on transgenic rootstock. Copyright © 2014 John Wiley & Sons, Ltd.

  6. Spin fluctuations in iron based superconductors probed by NMR relaxation rate

    Energy Technology Data Exchange (ETDEWEB)

    Graefe, Uwe; Kuehne, Tim; Wurmehl, Sabine; Buechner, Bernd; Grafe, Hans-Joachim [IFW Dresden, Institute for Solid State Research, PF 270116, 01171 Dresden (Germany); Hammerath, Franziska [IFW Dresden, Institute for Solid State Research, PF 270116, 01171 Dresden (Germany); Department of Physics ' ' A. Volta' ' , University of Pavia-CNISM, I-27100 Pavia (Italy); Lang, Guillaume [3LPEM-UPR5, CNRS, ESPCI Paris Tech, 10 Rue Vauquelin, 75005 Paris (France)

    2013-07-01

    We present {sup 75}As nuclear magnetic resonance (NMR) results in F doped LaOFeAs iron pnictides. In the underdoped superconducting samples, pronounced spin fluctuations lead to a peak in the NMR spin lattice relaxation rate, (T{sub 1}T){sup -1}. The peak shows a typical field dependence that indicates a critical slowing of spin fluctuations: it is reduced in height and shifted to higher temperatures. In contrast, a similar peak in the underdoped magnetic samples at the ordering temperature of the spin density wave does not show such a field dependence. Furthermore, the peak is absent in optimally and overdoped samples, suggesting the absence of strong spin fluctuations. Our results indicate a glassy magnetic ordering in the underdoped samples that is in contrast to the often reported Curie Weiss like increase of spin fluctuations towards T{sub c}. Additional measurements of the linewidth and the spin spin relaxation rate are in agreement with such a glassy magnetic ordering that is most likely competing with superconductivity. Our results will be compared to Co doped BaFe{sub 2}As{sub 2}, where a similar peak in (T{sub 1}T){sup -1} has been observed.

  7. Nuclear magnetic moment of 69As from on-line β-NMR on oriented nuclei

    International Nuclear Information System (INIS)

    Golovko, V.V.; Kraev, I.S.; Phalet, T.; Severijns, N.; Delaure, B.; Beck, M.; Kozlov, V.Yu.; Lindroth, A.; Coeck, S.; Zakoucky, D.; Venos, D.; Srnka, D.; Honusek, M.; Herzog, P.; Tramm, C.; Koester, U.

    2005-01-01

    A precise value for the magnetic moment of the 69 As 5/2 - ground state has been obtained from nuclear magnetic resonance on oriented nuclei (NMR/ON) using the NICOLE 3 He- 4 He dilution refrigerator setup at ISOLDE/CERN. The NMR/ON signal was observed by monitoring the anisotropy of the 69 As β particles. The center frequency ν[B ext =0.0994(10)T]=169.98(9) MHz corresponds to μ[ 69 As]=+1.6229(16)μ N . This result differs considerably from the πf 5/2 single-particle value obtained with g factors for a free proton but is in reasonable agreement with the value obtained with effective g factors and with values from a core polarization calculation and from calculations in the framework of the interacting boson-fermion model. Assuming a single exponential spin-lattice relaxation behavior a relaxation time T 1 ' =10(25) s was observed for 69 AsFe -bar at a temperature of about 20 mK in a magnetic field B=0.1 T

  8. Discriminating binding and positioning of amphiphiles to lipid bilayers by {sup 1}H NMR

    Energy Technology Data Exchange (ETDEWEB)

    Evanics, F. [Department of Chemistry, University of Toronto, UTM, 3359 Mississauga Rd. North Mississauga, Ont., L5L 1C6 (Canada); Prosser, R.S. [Department of Chemistry, University of Toronto, UTM, 3359 Mississauga Rd. North Mississauga, Ont., L5L 1C6 (Canada)]. E-mail: sprosser@utm.utoronto.ca

    2005-04-04

    The binding and positioning in lipid bilayers of three well-known drugs--imipramine, nicotine, and caffeine--have been studied using {sup 1}H NMR. The membrane model system consisted of 'fast-tumbling' lipid bicelles, in which a bilayered lipid domain, composed of the unsaturated lipid, 1,2-dimyristelaidoyl-sn-glycero-3-phosphocholine (DMLPC) was surrounded by a rim of deuterated detergent-like lipids, consisting of 1,2-dihexanoyl-sn-glycero-3-phosphocholine (DHPC-d22). Binding and immersion depth information was obtained by three experiments. (1) {sup 1}H chemical shift perturbations, upon transfer of the amphiphiles from water to a bicelle mixture, were used to estimate regions of the amphiphiles that interact with the membrane. (2) Water contact to resolvable protons was measured through a Nuclear Overhauser Effect (NOE) between water and resolvable drug and lipid resonances. In the case of both lipids and membrane bound drugs, positive NOEs with large cross-relaxation rates were measured for most resonances originating from the membrane hydrophilic region, while negative NOEs were observed predominantly to resonances in the hydrophobic region of the membrane. (3) {sup 1}H NMR measurements of oxygen-induced (paramagnetic) spin-lattice relaxation rates, which are known to increase with membrane immersion depth, were used to corroborate conclusions based on chemical shift perturbations and water-ligand NOEs.

  9. Local NMR relaxation rates T1-1 and T2-1 depending on the d -vector symmetry in the vortex state of chiral and helical p -wave superconductors

    Science.gov (United States)

    Tanaka, Kenta K.; Ichioka, Masanori; Onari, Seiichiro

    2018-04-01

    Local NMR relaxation rates in the vortex state of chiral and helical p -wave superconductors are investigated by the quasiclassical Eilenberger theory. We calculate the spatial and resonance frequency dependences of the local NMR spin-lattice relaxation rate T1-1 and spin-spin relaxation rate T2-1. Depending on the relation between the NMR relaxation direction and the d -vector symmetry, the local T1-1 and T2-1 in the vortex core region show different behaviors. When the NMR relaxation direction is parallel to the d -vector component, the local NMR relaxation rate is anomalously suppressed by the negative coherence effect due to the spin dependence of the odd-frequency s -wave spin-triplet Cooper pairs. The difference between the local T1-1 and T2-1 in the site-selective NMR measurement is expected to be a method to examine the d -vector symmetry of candidate materials for spin-triplet superconductors.

  10. DAMPAK KEBIJAKAN PEMERINTAH TERHADAP KOMODITAS PISANG MAS KIRANA

    Directory of Open Access Journals (Sweden)

    Ariq Dewi Maharani

    2016-10-01

    Full Text Available ABSTRAKPenelitian ini bertujuan untuk menganalisis aspek profitabilitas pisang mas Kirana di Kabupaten Lumajang, dan menganalisis dampak kebijakan pemerintah terhadap pisang mas Kirana di Kabupaten Lumajang. Penentuan lokasi dilakukan secara sengaja (purposive method di Kabupaten Lumajang. Data yang digunakan meliputi data primer dan data sekunder. Analisa data menggunakan Policy Analysis Matrix (PAM untuk menganalisis aspek profitabilitas dan dampak kebijakan pemerintah terhadap pisang mas Kirana. Hasil penelitian menunjukkan bahwa Komoditas pisang mas Kirana menguntungkan secara finansial dan ekonomi yang ditunjukkan dengan keuntungan privat (PP Rp 10.444.911,8 per hektar dan keuntungan sosial (SP sebesar Rp 23.108.983,7 per hektar. Keuntungan privat pisang mas Kirana lebih kecil daripada keuntungan sosialnya (PPmas Kirana, terdapat dampak kebijakan subsidi terhadap harga-harga input pada usahatani pisang mas Kirana; masih belum ada lembaga yang dapat memberikan pelayanan yang kompetitif serta informasi yang lengkap dan rendahnya harga beli pisang mas Kirana di dalam negeri. ABSTRACTThe purpose of this research for: to analyse the aspect of profitability Kirana Mas banana and to analyse impact of government policy on Kirana Mas banana in Lumajang District. Determination of location was done intentionally or purposive method in Lumajang regency. The data that was used covering primary data and secondary data. Data analysis used Policy Analysis Matrix (PAM for knowing of profitability aspect and impact of government policy on Kirana Mas banana. The results showed that Commodity of Kirana Mas banana has financially and economically beneficial, shown by private profit (PP Rp 10,444,911.8 per hectare and social benefits (SP Rp 23,108,983.7 per hectare. Private profits of “Kirana mas” banana are smaller than social benefit (PP

  11. CAMEX-4 ER-2 MODIS AIRBORNE SIMULATOR (MAS) V1

    Data.gov (United States)

    National Aeronautics and Space Administration — The MODIS Airborne Simulator (MAS) is an airborne scanning spectrometer that acquires high spatial resolution imagery of cloud and surface features from its vantage...

  12. 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

  13. Experimental solid state NMR of gas hydrates : problems and solutions

    Energy Technology Data Exchange (ETDEWEB)

    Moudrakovski, I.; Lu, H.; Ripmeester, J. [National Research Council of Canada, Ottawa, ON (Canada). Steacie Inst. for Molecular Sciences; Kumar, R.; Susilo, R. [British Columbia Univ., Vancouver, BC (Canada). Dept. of Chemical and Biological Engineering; Luzi, M. [GeoForschungsZentrum Potsdam, Potsdam (Germany)

    2008-07-01

    Solid State NMR is a suitable spectroscopic technique for hydrate research for several reasons, including its capability to distinguish between different structural types of hydrates, its quantitative nature and potential for both in-situ and time resolved experiments. This study illustrated the applications of solid state NMR for compositional and structural studies of clathrate hydrates, with particular emphasis on experimental techniques and potential ways to overcome technical difficulties. In order to use the method to its full capacity, some instrumental developments are needed to adapt it to the specific experimental requirements of hydrate studies, such as very low temperatures and high pressures. This presentation discussed the quantification of the Carbon-13 spectra with examples from natural and synthetic hydrates prepared from multi-component mixtures of hydrocarbons. The main approach used for the first two examples was Carbon-13 NMR with Magic Angle Spinning (MAS) at -100 degrees C. The detailed characterization of mixed hydrogen hydrates required low temperature hydrogen MAS. The quantification problems encountered during these experiments were also discussed. The purpose of these recent experimental developments was to prompt wider application of Solid State NMR in hydrate research. NMR proved to be a viable method for analyzing the composition and structure of multi-component mixed gas hydrates; characterizing natural gas hydrates; and, evaluating the formation conditions and properties of mixed hydrogen hydrates. The limitations of the method were highlighted and sensible choices of experimental conditions and techniques that ensure accurate results were discussed. 34 refs., 10 figs.

  14. 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...

  15. NMR of dielectrically oriented molecules

    International Nuclear Information System (INIS)

    Ruessink, B.H.

    1986-01-01

    General information on experimental aspects of EFNMR is given. It is shown that the complete 14 N quadrupole tensor (qct) of pyridine and pyrimidine in the liquid state is accessible to EFNMR. Information obtained about 17 O qct in liquid nitromethane, is compared with results from other techniques. The 33 S qct in liquid sulfolane is investigated. The EFNMR results, combined with those from spin-lattice relaxation time measurements and from Hartree-Fock-Slater MO calculations, allowed the complete assignment of the 33 S qct. The quadrupole coupling of both 10 B and 11 B in a carborane compound is investigated and, together with the results of spin-lattice relaxation time measurements, detailed information about the assignment of the boron qct's could be derived. EFNMR studies of apolar molecules are described. A limitation in EFNMR is the inhomogeneity (delta B) of the magnetic field, which is introduced by the use of non-spinning sample cells. A way out is the detection of zero quantum transitions, their widths being independent of delta B. The results and prospectives of this approach are shown for the simple three spin 1/2 system of acrylonitrile in which the small dipolar proton-proton couplings could be revealed via zero quantum transitions. (Auth.)

  16. NMR study of spin dynamics in mesoscopic molecular clusters

    Science.gov (United States)

    Borsa, Ferdinando

    1998-03-01

    Recent published and umpublished work regarding the magnetic properties and the spin dynamics of molecules containing rings of 6,8 and 10 spins and of molecules containing clusters of 8 and 12 spins are reviewed. The 1H nuclear spin-lattice relaxation rate (NSLR) and the Muon Spin Resonance relaxation in Mn12 (A.Lascialfari, D.Gatteschi, F.Borsa, A.Shastri, Z.H.Jang and P.Carretta, Phys.Rev. B 1 January 1998) and Fe8 clusters are presented and discussed with regards to the high temperature spin dynamics of the Mn (Fe) magnetic moments and with regards to the low temperature superparamagnetic behavior. 1H and 63Cu NMR results are presented for two "quantum" spin rings : Cu6 and Cu8. The Cu6 is a weakly coupled (J/k=60K) ferromagnetic S=1/2 spin ring while Cu8 is a strongly coupled (J/k greater than 400K) antiferromagnetic S=1/2 spin ring.The dependence of the NSRL from temperature and from applied magnetic field are analyzed in terms of the calculated magnetic energy levels of the magnetic ring. The values of the energy gap between the ground state and the first excited state are extracted from the exponential decrease of the NSLR as the temperature is lowered. The results in the Cu ( S=1/2) "quantum" rings are compared with the results in "quantum" chains and ladders and with the results in "classical" Fe (S=5/2) antiferromagnetic rings : Fe6 and Fe10 (A.Lascialfari, D.Gatteschi, F.Borsa and A.Cornia , Phys.Rev. 55B,14341,1997) ).

  17. The structure of phosphate and borosilicate glasses and their structural evolution at high temperatures as studied with solid state NMR spectroscopy: Phase separation, crystallisation and dynamic species exchange

    International Nuclear Information System (INIS)

    Wegner, S.; Van Wullen, L.; Tricot, G.; Tricot, G.

    2010-01-01

    In this contribution we present an in-depth study of the network structure of different phosphate based and borosilicate glasses and its evolution at high temperatures. Employing a range of advanced solid state NMR methodologies, complemented by the results of XPS, the structural motifs on short and intermediate length scales are identified. For the phosphate based glasses, at temperatures above the glass transition temperature Tg, structural relaxation processes and the devitrification of the glasses were monitored in situ employing MAS NMR spectroscopy and X-ray diffraction. Dynamic species exchange involving rapid P-O-P and P-O-Al bond breaking and reforming was observed employing in situ 27 Al and 31 P MAS NMR spectroscopy and could be linked to viscous flow. For the borosilicate glasses, an atomic scale investigation of the phase separation processes was possible in a combined effort of ex situ NMR studies on glass samples with different thermal histories and in situ NMR studies using high temperature MAS NMR spectroscopy including 11 B MAS, 29 Si MAS and in situ 29 Si{ 11 B} REAPDOR NMR spectroscopy. (authors)

  18. A combined NMR and XRD study of AFI and AEL type molecular sieves

    NARCIS (Netherlands)

    Peeters, M.P.J.; Ven, van de L.J.M.; Haan, de J.W.; Hooff, van J.H.C.

    1993-01-01

    Calcined dehydrated AlPO4-5 was studied by x-ray powder diffraction, 31P MAS, and 27Al double-resonance (DOR) NMR. Three crystallog. different sites can be distinguished in the structure of dehydrated AlPO4-5 in the ratio 1:1:1. The obsd. splitting of the NMR spectra is correlated to the line width

  19. 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

    Introduction: 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. Methods: 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. Results: 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 mmHg2), and low-frequency component of systolic BPV (0.12±0.11 vs 0.47±0.34 mmHg2). Conclusions: 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. PMID:27080540

  20. 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

  1. NMR spectroscopy applied to the eye: Drugs and metabolic studies

    International Nuclear Information System (INIS)

    Saether, Oddbjoern

    2005-01-01

    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

  2. Magnetization transfer from macromolecules to water protons in murine dental tissues as revealed by 500 MHz 1H-NMR

    International Nuclear Information System (INIS)

    Nakamura, Koji; Era, Seiichi; Nagai, Naoki; Sogami, Masaru; Takasaki, Akihiko; Kato, Kazuo.

    1997-01-01

    Although much is known about magnetization transfer phenomena in biological soft tissues, little is known about those in hard tissues. Using a 500 MHz 1 H-NMR spectrometer, we studied the spin-lattice relaxation time (T 1 (H 2 O)) and the intermolecular cross-relaxation times (T IS (H 2 O)) from irradiated macromolecular protons to observed water protons in murine lower incisors (hard tissue) and compared with those in murine lens tissue (soft tissue). Mean values for the water content (%) of murine lower incisors and lens tissue were 16.02±2.39 (n=14) and 67.20±4.60 (n=15), respectively. These findings were consistent with the large different in water content between soft tissues and hard tissues. T IS (H 2 O) values obtained by f 2 -irradiation at 7.13 or -4.00 ppm showed no significant difference between lower incisors and lens tissue. Plots of 1/T IS (H 2 O) values vs. tissue dry weight (W(%)) for lower incisor tissue approximated a straight line with slope approximately equal for that obtained for lens tissue. These results suggest that the state of water in hard tissue may be similar to that in soft tissues, in spite of the significant difference in water content. Thus, saturation transfer NMR techniques such as measurement of T IS (H 2 O) values may be applicable to the study of water-macromolecule interactions in both biological soft and hard tissues. (author)

  3. Single ferromagnetic fluctuations in UCoGe revealed by 73Ge- and 59Co-NMR studies

    Science.gov (United States)

    Manago, Masahiro; Ishida, Kenji; Aoki, Dai

    2018-02-01

    73Ge and 59Co nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements have been performed on a 73Ge-enriched single-crystalline sample of the ferromagnetic superconductor UCoGe in the paramagnetic state. The 73Ge NQR parameters deduced from NQR and NMR are close to those of another isostructural ferromagnetic superconductor URhGe. The Knight shifts of the Ge and Co sites are well scaled to each other when the magnetic field is parallel to the b or c axis. The hyperfine coupling constants of Ge are estimated to be close to those of Co. The large difference of spin susceptibilities between the a and b axes could lead to the different response of the superconductivity and ferromagnetism with the field parallel to these directions. The temperature dependence of the nuclear spin-lattice relaxation rates 1 /T1 at the two sites is similar to each other above 5 K. These results indicate that the itinerant U-5 f electrons are responsible for the ferromagnetism in this compound, consistent with previous studies. The similarities and differences in the three ferromagnetic superconductors are discussed.

  4. 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

  5. MAS2-8 radar and digital control unit

    Science.gov (United States)

    Oberg, J. M.; Ulaby, F. T.

    1974-01-01

    The design of the MAS 2-8 (2 to 8 GHz microwave-active spectrometer), a ground-based sensor system, is presented. A major modification in 1974 to the MAS 2-8, that of a control subsystem to automate the data-taking operation, is the prime focus. The digital control unit automatically changes all system parameters except FM rate and records the return signal on paper tape. The overall system operation and a detailed discussion of the design and operation of the digital control unit are presented.

  6. NMR-CT scanner

    International Nuclear Information System (INIS)

    Kose, Katsumi; Sato, Kozo; Sugimoto, Hiroshi; Sato, Masataka.

    1983-01-01

    A brief explanation is made on the imaging methods for a practical diagnostic NMR-CT scanner : A whole-body NMR-CT scanner utilizing a resistive magnet has been developed by Toshiba in cooperation with the Institute for Solid State Physics, the University of Tokyo. Typical NMR-CT images of volunteers and patients obtained in the clinical experiments using this device are presented. Detailed specifications are also shown about the practical NMR-CTs which are to be put on the market after obtaining the government approval. (author)

  7. NMR imaging and pharmaceutical sciences

    International Nuclear Information System (INIS)

    Beall, P.T.; Good, W.R.

    1986-01-01

    Described is the technique of NMR-imaging in diagnostic medicine. Proton and phosphorus NMR in diagnosis of abnormal tissue pathology. Discussed is the value of NMR to the pharmaceutical sciences. NMR may play an important role in monitoring the response of tissues to drugs, determining the localization of drugs, performing real time pharmacokinetics and testing the use of NMR contrast pharmaceuticals

  8. Crystal structure, {sup 139}La NMR and transport properties of the As-based filled skutterudites LaOs{sub 4}As{sub 12} and PrOs{sub 4}As{sub 12}

    Energy Technology Data Exchange (ETDEWEB)

    Wawryk, R.; Zogal, O.; Pietraszko, A.; Paluch, S.; Cichorek, T. [Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw (Poland); Yuhasz, W.M.; Sayles, T.A.; Ho, P.-C.; Yanagisawa, T.; Butch, N.P.; Maple, M.B. [Department of Physics and Institute for Pure and Applied Physical Sciences, University of California, San Diego (United States); Henkie, Z. [Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Wroclaw (Poland)], E-mail: Z.Henkie@int.pan.wroc.pl

    2008-02-28

    We have grown single crystals of LaOs{sub 4}As{sub 12} and PrOs{sub 4}As{sub 12}, which crystallize in the LaFe{sub 4}P{sub 12}-type structure (Im3-bar space group) with the lattice parameters of 8.542(1) A and 8.520(1) A, respectively. From a narrow {sup 139}La NMR line, we estimated an appreciable Knight shift ({sup 139}K) and a relatively long spin-lattice-relaxation time in the non-4f electron system LaOs{sub 4}As{sub 12}. Surprisingly, while {sup 139}K vary non-monotonically with temperature, the magnetic susceptibility increases upon cooling over the whole temperature range. Interestingly, the high-temperature dependence of the thermoelectric power of LaOs{sub 4}As{sub 12} is remarkably similar to that one of PrOs{sub 4}As{sub 12}.

  9. {sup 7}Li and {sup 23}Na NMR measurements on (Na{sub 0.75}Li{sub 0.25}){sub 2}IrO{sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Dey, Tusharkanti; Freund, Friedrich; Manni, Soham; Gegenwart, Philipp [EP-VI, Electronic Correlations and Magnetism, University of Augsburg (Germany); Prinz-Zwick, Markus; Schaedler, Martina; Buettgen, Norbert [EP-V, Electronic Correlations and Magnetism, University of Augsburg (Germany); Mahajan, Avinash [EP-V, Electronic Correlations and Magnetism, University of Augsburg (Germany); IIT Bombay (India)

    2016-07-01

    An experimental realization of the proposed Kitaev spin-liquid phase in Na{sub 2}IrO{sub 3} and Li{sub 2}IrO{sub 3} is still a big challenge. Efforts to suppress the magnetic ordering in Na{sub 2}IrO{sub 3} by substituting isoelectronic Li in the Na site was partially successful. An earlier report suggests the optimum doping to be 25% where the magnetic ordering is suppressed to 6 K while the structure remains undisturbed. Interestingly, for the (Na{sub 0.75}Li{sub 0.25}){sub 2}IrO{sub 3} sample Na and Li are crystallographically ordered where the Li ions reside at the centre of the Ir honeycombs. We have studied the material using both {sup 7}Li and {sup 23}Na NMR. Results of our spectra, spin-lattice and spin-spin relaxation measurements will be discussed in the poster.

  10. NMR of Cu satellites in the Kondo alloy CuCr

    International Nuclear Information System (INIS)

    Azevedo, L.J.; Follstaedt, D.; Narath, A.

    1978-01-01

    Using pulsed NMR techniques, resonances of Cu nuclei which are near neighbors to Cr impurities (c = 100 and 200 ppM) in CuCr (theta/sub k/ approx. 3K) have been studied in the temperature range 1 to 4K and applied fields H 0 = 20 to 125 kOe. At the highest fields and lowest temperatures the satellite shifts approach saturation. Above approx. 40 kOe the spin-lattice relaxation rate T 1 -1 is proportional to T/H 0 2 , indicating that the dominant relaxation mechanism arises from transverse fluctuations of a polarized local moment. The measured rates yield a local-moment/conduction-electron exchange interaction vertical bar J 0 vertical bar/g = 0.30, where g is the Cr g-value. Below approx. 40 kOe T 1 -1 appears to be slightly enhanced in comparison with the high-field behavior, but becomes field independent below approx. 30 kOe. Both effects are attributed to Kondo anomalies

  11. Deuteron-NMR investigation on the dynamics of supercooled, confined water

    Energy Technology Data Exchange (ETDEWEB)

    Sattig, Matthias; Vogel, Michael [TU Darmstadt, Institut fuer Festkoerperphysik (Germany)

    2013-07-01

    The dynamical behaviour of water in the regime of the supercooled liquid is a topic of large interest. In particular, the existence of a fragile-to-strong transition (FST) at T=225K related to the transition between two distinct phases of liquid water is controversially discussed. Due to crystallization the temperature range proposed for the FST is hardly accessible in bulk water. Therefore, we confine heavy water to narrow pores in the mesoporous silicate MCM-41. This suppresses the freezing of a substantial fraction of water, enabling direct investigation of the interesting temperatures. Deuteron-NMR methods are utilised to determine the rotational correlation times τ of water on time scales from ns up to s. The spin-lattice-relaxation time T{sub 1} exhibits a typical minimum at about T = 230 K. Above this minimum the correlation times follow a Vogel-Fulcher-Tammann law. Below the minimum, two relaxation processes could be observed. The low-temperature processes show a different temperature dependence, where the curves τ(T) of all processes intersect at about T = 230 K. A comparison with literature data from neutron scattering and dielectric spectroscopy gives rise to the idea that the observed crossover is due to this intersection of processes rather than to a FST. To test this idea studies on water confined to MCM-41 with different pore sizes and fillings are in progress.

  12. 209Bi NMR in heavy-electron system YbBiPt

    International Nuclear Information System (INIS)

    Reyes, A.P.; Le, L.P.; Heffner, R.H.; Ahrens, E.T.; Fisk, Z.; Canfield, P.C.

    1994-01-01

    Bismuth NMR Knight shift and spin lattice relaxation rate 1/T 1 are reported between 35--325K in the low-carrier heavy fermion system YbBiPt. The Knight shift is strongly temperature dependent and negative. Its temperature dependence tracks the bulk susceptibility with a hyperfine coupling constant A hf = -7.89 kOe/μB. At low temperatures 1/T 1 exhibits a dramatic increase, such that the average 4f spin correlation time τ f shows a crossover behavior at about 75K. The rate 1/τ f is proportional to temperature, but with a different proportionality constant above and below about 75K. The linear temperature dependence is consistent with non-interacting 4f local moments which are relaxed via Korringa-type scattering with the conduction electrons. Below 75K, we infer that the reduced thermal excitation of a higher crystal-field multiplet is responsible for the dramatic decrease in the rate of 4f relaxation

  13. 13C NMR and relaxation studies of the nanomagnet Mn12-acetate

    Science.gov (United States)

    Achey, Randall M.; Kuhns, Philip L.; Reyes, Arneil P.; Moulton, William G.; Dalal, Naresh S.

    2001-08-01

    The nanomagnet [Mn12O12(CH3COO)16(H2O)4].2CH3COOH.4H2O, also known as Mn12, has been synthesized with 13C labeling at the CH3 groups, and investigated by 13C NMR at fields up to 23 T. Using oriented samples, it is possible to resolve four distinct 13C peaks at room temperature, located on both sides of the unshifted Larmor frequency. These peaks were assigned to the four hyperfine-shifted, magnetically inequivalent sets of 13CH3 groups in the Mn12 lattice, based on a comparison with the crystal structure and point-dipole and spin-density calculations. These results establish that the unpaired electron spin density of the S=10 system in this cluster extends over the entire molecular framework, not just the core. These results are discussed in relationship to inelastic neutron scattering measurements. The temperature and field dependence of the 13C nuclear-spin-lattice-relaxation time T1 on the least shifted peak was measured. A single weakly field-dependent minimum at about 60 K is observed in the temperature dependence of the measured T1. The relaxation mechanism responsible for the T1 minimum is ascribed mainly to hindered rotation of the methyl group of the acetate ligand at higher temperature, and to electronic spin fluctuations at lower temperature.

  14. Li dynamics in carbon-rich polymer-derived SiCN ceramics probed by NMR

    Science.gov (United States)

    Baek, Seung-Ho; Reinold, Lukas; Graczyk-Zajac, Magdalena; Riedel, Ralf; Hammerath, Franziska; Buechner, Bernd; Grafe, Hajo

    2014-03-01

    We report 7Li, 29Si, and 13C NMR studies of two different carbon-rich SiCN ceramics SiCN-1 and SiCN-3 derived from the preceramic polymers polyphenylvinylsilylcarbodiimide and polyphenylvinylsilazane, respectively. From the spectral analysis of the three nuclei at room temperature, we find that only the 13C spectrum is strongly influenced by Li insertion/extraction, suggesting that carbon phases are the major electrochemically active sites for Li storage. Temperature and Larmor frequency (ωL) dependences of the 7Li linewidth and spin-lattice relaxation rates T1-1 are described by an activated law with the activation energy EA of 0.31 eV and the correlation time τ0 in the high temperature limit of 1.3 ps. The 3 / 2 power law dependence of T1-1 on ωL which deviates from the standard Bloembergen, Purcell, and Pound (BPP) model implies that the Li motion on the μs timescale is governed by continuum diffusion mechanism rather than jump diffusion. On the other hand, the rotating frame relaxation rate T1ρ-1 results suggest that the slow motion of Li on the ms timescale may be affected by complex diffusion and/or non-diffusion processes.

  15. Monovacancy paramagnetism in neutron-irradiated graphite probed by 13C NMR.

    Science.gov (United States)

    Zhang, Zhi Tao; Xu, C; Dmytriieva, Daryna; Molatta, Sebastian; Wosnitza, J; Wang, Y T; Helm, Manfred; Zhou, Shengqiang; Kuehne, Hannes

    2017-09-18

    We report on the magnetic properties of monovacancy defects in neutron-irradiated graphite, probed by $^{13}$C nuclear magnetic resonance spectroscopy. The bulk paramagnetism of the defect moments is revealed by the temperature dependence of the NMR frequency shift and spectral linewidth, both of which follow a Curie behavior, in agreement with measurements of the macroscopic magnetization. Compared to pristine graphite, the fluctuating hyperfine fields generated by the defect moments lead to an enhancement of the $^{13}$C nuclear spin-lattice relaxation rate $1/T_{1}$ by about two orders of magnitude. With an applied magnetic field of 7.1 T, the temperature dependence of $1/T_{1}$ below about 10 K can well be described by a thermally activated form, $1/T_{1}\\propto\\exp(-\\Delta/k_{B}T)$, yielding a singular Zeeman energy of ($0.41\\pm0.01$) meV, in excellent agreement with the sole presence of polarized, non-interacting defect moments. © 2017 IOP Publishing Ltd.

  16. Non-polymeric asymmetric binary glass-formers. II. Secondary relaxation studied by dielectric, 2H NMR, and 31P NMR spectroscopy

    Science.gov (United States)

    Pötzschner, B.; Mohamed, F.; Bächer, C.; Wagner, E.; Lichtinger, A.; Bock, D.; Kreger, K.; Schmidt, H.-W.; Rössler, E. A.

    2017-04-01

    We investigate the secondary (β-) relaxations of an asymmetric binary glass former consisting of a spirobichroman derivative (SBC; Tg = 356 K) as the high-Tg component and the low-Tg component tripropyl phosphate (TPP; Tg = 134 K). The main relaxations are studied in Paper I [B. Pötzschner et al., J. Chem. Phys. 146, 164503 (2017)]. A high Tg contrast of ΔTg = 222 K is put into effect in a non-polymeric system. Component-selective studies are carried out by combining results from dielectric spectroscopy (DS) for mass concentrations cTPP ≥ 60% and those from different methods of 2H and 31P NMR spectroscopy. In the case of NMR, the full concentration range (10% ≤ cTPP ≤ 100%) is covered. The neat components exhibit a β-relaxation (β1 (SBC) and β2 (TPP)). The latter is rediscovered by DS in the mixtures for all concentrations with unchanged time constants. NMR spectroscopy identifies the β-relaxations as being alike to those in neat glasses. A spatially highly restricted motion with angular displacement below ±10° encompassing all molecules is involved. In the low temperature range, where TPP shows the typical 31P NMR echo spectra of the β2-process, very similar spectral features are observed for the (deuterated) SBC component by 2H NMR, in addition to its "own" β1-process observed at high temperatures. Apparently, the small TPP molecules enslave the large SBC molecules to perform a common hindered reorientation. The temperature dependence of the spin-lattice relaxation time of both components is the same and reveals an angular displacement of the SBC molecules somewhat smaller than that of TPP, though the time constants τβ2 are the same. Furthermore, T1(T) of TPP in the temperature region of the β2-process is absolutely the same as in the mixture TPP/polystyrene investigated previously. It appears that the manifestations of the β-process introduced by one component are essentially independent of the second component. Finally, at cTPP ≤ 20% one

  17. NMR studies at high magnetic fields of LiVGe_2O_6, a quasi one-dimensional spin S=1 system

    Science.gov (United States)

    Vonlanthen, P.; Tanaka, K. B.; Clark, W. G.; Gavilano, J. L.; Ott, H. R.; Millet, P.; Mila, F.; Kuhns, P.; Reyes, A. P.; Moulton, W. G.

    2001-03-01

    We report ^7Li NMR studies of LiVGe_2O_6, a quasi one-dimensional spin S=1 system. Our measurements include NMR spectra, the spin-lattice relaxation rate, T_1-1, and the spin-spin relaxation rate, T_2-1, obtained at magnetic fields (B) of 9 and 23 T and temperatures (T) over the range 1.8 - 300 K. The 9 T NMR spectra show a continuous transfer of spectral weight from a paramagnetic phase to an antiferromagnetic one in a narrow temperature range of about 2 K around the transition temperature TN ≈ 25 K. Both phases coexist in this range. Below 10 K, well into the antiferromagnetic phase, the T_1-1 measurements are consistent with electron spin excitations across an energy gap (Δ) with Δ/k_B≈ 14 K at 9 T and 11 K at about 23 T; i.e., applying a large B slightly reduces Δ. Changing B from 9 to 23 T increases TN by 1 K. Thus, TN is influenced only marginally by B up to 23 Tesla. The UCLA part of the work was supported by NSF Grants DMR-9705369 and DMR-0072524.

  18. Copper NMR and hole depletion in the normal state of Y1-xPrxBa2Cu3O7

    International Nuclear Information System (INIS)

    MacLaughlin, D.E.; Reyes, A.P.; Takigawa, M.; Hammel, P.C.; Heffner, R.H.; Thompson, J.D.; Crow, J.E.

    1990-01-01

    Normal-state copper NMR spectra and spin-lattice relaxation rates 1/T 1 have been measured in the planar cuprate system YBa 2 Cu 3 O 7 . With Pr doping the Knight shift K decreases and develops a temperature dependence at both plane and chain sites. Analysis of the bulk susceptibility and NMR data indicate that pair breaking and hole depletion both take part in the suppression of the superconducting transition temperature T c . The Knight shift behavior resembles that in oxygen-deficient YBa 2 Cu 3 O 7-y , as does the temperature dependence of 1/T 1 for plane Cu sites and magnetic field perpendicular to the c axis. This agreement leads to a consistent picture of the role of antiferromagnetic fluctuations in these materials. An analysis of the data in the framework of the phenomenological theory of Millis, Monien, and Pines is given. In the end compound PrBa 2 Cu 3 O 7 the NMR signal from plane Cu sites indicates antiferromagnetic (AF) ordering at a Neel temperature ∼280 K, and in the AF state yields an internal field similar to those found in AF YBa 2 Cu 3 O 6 and La 2 CuO 4 . 32 refs., 7 figs

  19. sup 5 sup 9 Co NMR spectroscopy and relaxation in the metamagnetic system Y sub 1 sub - sub x Gd sub x Co sub 3

    CERN Document Server

    Reis, M S; García, F; Takeuchi, A Y; Guimarães, A P

    2000-01-01

    We studied the nuclear magnetic resonance (NMR) in intermetallic compounds of the series Y sub 1 sub - sub x Gd sub x Co sub 3. We found spectra exhibiting four lines, corresponding to four magnetic sites of these compounds. However, the number of lines and their widths are strongly dependent on the radiofrequency (RF) power level, a fact that may help to explain some of the discrepancies found in the NMR literature on these compounds. From the dependence of the NMR spectra with the RF power we concluded that the site labeled 18h presents the largest local magnetic anisotropy. No significant changes are observed on the value of the hyperfine fields at each site as a function of the Gd concentration x, and that is explained in terms of the statistical distribution of Gd magnetic ions in the lattice. On the contrary, the spin-lattice and spin-spin relaxation rates, 1/T sub 1 and 1/T sub 2 , measured at each line, are remarkably dependent on the concentration. 1/T sub 2 exhibits a prominent peak at x approx 0.25...

  20. Characterization of polyurethane/organophilic montmorillonite nanocomposites by low field NMR; Caracterizacao de nanocompositos de poliuretano/montmorilonita organofilica por RMN de baixo campo

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Marcos Anacleto da [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Laboratorio de Nanocompositos Polimericos; Tavares, Maria I.B.; Nascimento, Suelen A.M.; Rodrigues, Elton J. da R [Universidade Federal do Rio de Janeiro (NUCAT/PEQ/COPPE/UFRJ), RJ (Brazil). Laboratorio de Nanocompositos Polimericos

    2012-07-01

    Polyurethanes are important and versatile materials, mainly due to some of their properties, such as high resistance to abrasion and tearing, excellent absorption of mechanical shocks and good flexibility and elasticity. However, they have some drawbacks as well, such as low thermal stability and barrier properties. To overcome these disadvantages, various studies have been conducted involving organophilic polyurethane/montmorillonite nanocomposites. The investigation of the structure of polyurethane/clay nanocomposites has mainly been done by X-ray diffraction (XRD) and transmission electron microscopy (TEM). In this work, PU/clay nanocomposite films obtained by solution intercalation were studied. The nanocomposites were characterized by XRD and low-field nuclear magnetic resonance (LF-NMR). The LF-NMR measurements, with determination of the spin-lattice relaxation time of the hydrogen nucleus, supplied important information about the molecular dynamics of these nanocomposites. The X-ray diffraction measurements validated the results found by NMR. The thermal stability of the material was also determined by thermogravimetric analysis (TGA) under an inert atmosphere. A slight improvement in this stability was observed in the nanocomposite in comparison with polyurethane (author)

  1. Cotton fibers encapsulated with homo- and block copolymers: synthesis by the atom transfer radical polymerization grafting-from technique and solid-state NMR dynamic investigations.

    Science.gov (United States)

    Castelvetro, Valter; Geppi, Marco; Giaiacopi, Simone; Mollica, Giulia

    2007-02-01

    Cotton fibers were modified by surface-initiated atom transfer radical polymerization of ethyl acrylate (EA) followed by copolymerization with styrene. Either ethyl 2-bromopropionate as a sacrificial free initiator or Cu(II) as a deactivator was used to optimize the EA grafting yield and to preserve the livingness of the chain ends for the subsequent growth of a poly(styrene) (PSty) block from the poly(ethyl acrylate) (PEA) grafts. The polymer-encapsulated cotton fibers were analyzed by Fourier transform infrared spectroscopy, scanning electron microscopy, differential scanning calorimetry (DSC), thermogravimetric analysis, and solid-state NMR (high-resolution 13C cross-polarization magic angle spinning, 1H spin-lattice relaxation times, and 1H free induction decay analysis NMR). The latter allowed the detection of the dynamic modifications associated with the presence of homo- and block copolymer grafts. In particular, the results of the DSC and NMR investigations suggest a heterogeneous morphology of the g-PEA-b-PSty grafted skin, which could be described as an inner layer of g-PEA sandwiched between the semicrystalline cellulose of the core fiber and the high glass transition temperature PSty of the covalently linked outer layer. Such morphology results in a reduced molecular mobility of the PEA chains.

  2. A new approach to the silica gel surface : characterization of different surface regions by 29Si magic angle spinning NMR relaxation parameters and consequences for quantification of silica gels by NMR: characterization of different surface regions by silicon-29 magic angle spinning NMR relaxation parameters and consequences for quantification of silica gels by NMR

    NARCIS (Netherlands)

    Pfleiderer, B.; Albert, K.; Bayer, E.; Ven, van de L.J.M.; Haan, de J.W.; Cramers, C.A.M.G.

    1990-01-01

    Native and some monofunctionally derivatized silica gels have been investigated by 29Si CP MAS NMR spectroscopy with pulse and with cross-polarization (CP) excitation. Contact time variation experiments for some native materials yield results for the siloxane (Q4)g roups which cannot be described

  3. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    International Nuclear Information System (INIS)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G.; Boffo, Elisangela F.; Figueira, Glyn M.

    2012-01-01

    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, 1 H HR-MAS NMR and 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. Fluorine dynamics in BaF2 superionic conductors investigated by NMR

    OpenAIRE

    Gumann, Patryk

    2008-01-01

    In this work the dynamics of fluorine in solid-state electrolytes having BaF2-structure was investigated using three different NMR-methods: field cycling relaxometry, lineshape analysis, and static field gradient NMR. For this purpose a pure BaF2 crystal, as well as crystals doped with trivalent impurities (LaF3), were studied as a function of temperature. The main goal of this investigation was to utilize the structure information provided by neutron scattering and MAS NMR data in order to s...

  6. 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)

  7. 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)

  8. 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

  9. 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 striki...

  10. Magnetic and structural properties of an octanuclear Cu(II) S=1/2 mesoscopic ring: Susceptibility and NMR measurements

    Energy Technology Data Exchange (ETDEWEB)

    Lascialfari, A. [Department of Physics ' ' A. Volta' ' and Unita INFM, University of Pavia, Via Bassi 6, I-27100 Pavia, (Italy); Jang, Z. H. [Ames Laboratory and Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Borsa, F. [Department of Physics ' ' A. Volta' ' and Unita INFM, University of Pavia, Via Bassi 6, I-27100 Pavia, (Italy); Ames Laboratory and Department of Physics and Astronomy, Iowa State University, Ames, Iowa 50011 (United States); Gatteschi, D. [Department of Chemistry, University of Florence, Via Maragliano 77, I-50144 Florence, (Italy); Cornia, A. [Department of Chemistry, University of Modena, Via Campi 183, I-41100 Modena, (Italy); Rovai, D. [Department of Chemistry, University of Florence, Via Maragliano 77, I-50144 Florence, (Italy); Caneschi, A. [Department of Chemistry, University of Florence, Via Maragliano 77, I-50144 Florence, (Italy); Carretta, P. [Department of Physics ' ' A. Volta' ' and Unita INFM, University of Pavia, Via Bassi 6, I-27100 Pavia, (Italy)

    2000-03-01

    Magnetic susceptibility, {sup 1}H NMR and {sup 63}Cu NMR-NQR experiments on two slightly different species of the molecular S=1/2 antiferromagnetic (AF) ring Cu8, [Cu{sub 8}(dmpz){sub 8}(OH){sub 8}]{center_dot}2C{sub 5}H{sub 5}N (Cu8P) and [Cu{sub 8}(dmpz){sub 8}(OH){sub 8}]{center_dot}2C{sub 5}H{sub 5}NO{sub 2} (Cu8N), are presented. The magnetic energy levels are calculated exactly for an isotropic Heisenberg model Hamiltonian in zero magnetic field. From the magnetic susceptibility measurements we estimate the AF exchange coupling constant J{approx}1000 K and the resulting gap {delta}{approx}500 K between the S{sub T}=0 ground state and the S{sub T}=1 first excited state. The {sup 63,65}Cu NQR spectra indicate the presence of four crystallographically inequivalent copper nuclei in each ring. From the combination of the {sup 63}Cu NQR spectra and of the {sup 63}Cu NMR spectra at high magnetic field, we estimate the quadrupole coupling constant v{sub Q} of each site and the average asymmetry parameter {eta} of the electric-field gradient tensor. The nuclear spin-lattice relaxation rate (NSLR) decreases exponentially on decreasing temperature for all nuclei investigated. The gap parameter extracted from {sup 63}Cu NQR-NSLR is the same as for the susceptibility while a smaller value is obtained from the {sup 63}Cu NMR-NSLR in an external magnetic field of 8.2 T. (c) 2000 The American Physical Society.

  11. Lectures on pulsed NMR

    International Nuclear Information System (INIS)

    Pines, A.

    1988-08-01

    These lectures discuss some recent developments in pulsed NMR, emphasizing fundamental principles with selected illustrative applications. Major topics covered include multiple-quantum spectroscopy, spin decoupling, the interaction of spins with a quantized field, adiabatic rapid passage, spin temperature and statistics of cross-polarization, coherent averaging, and zero field NMR. 32 refs., 56 figs

  12. Lectures on pulsed NMR

    International Nuclear Information System (INIS)

    Pines, A.

    1986-09-01

    These lectures discuss some recent developments in pulsed NMR, emphasizing fundamental principles with selected illustrative applications. Major topics covered include multiple-quantum spectroscopy, spin decoupling, the interaction of spins with a quantized field, adiabatic rapid passage, spin temperature and statistics of cross-polarization, coherent averaging, and zero field NMR. 55 figs

  13. Catalyst surface characterized by high magnetic field NMR; Kojiba NMR ni yoru shokubai hyomen no kansatsu

    Energy Technology Data Exchange (ETDEWEB)

    Sato, S. [Chiba University, Chiba (Japan). Faculty of Engineering

    1997-08-01

    This paper introduces studies performed by the authors on observation of surface of solid catalysts by means of solid NMR measurement using the high-speed MAS technology which uses a high magnetic field device. In the studies, a device with 14.1T (resonant frequency of proton at 600 MHz) was used to conduct CP-MAS NMR measurement on {sup 29}Si to identify bonding of silica carrier in a fixed aluminum chloride catalyst. As a result, it was verified that the surface structure of aluminum chloride species deposited on the silica carrier turns to a structure in which AlCl2 species of a monomeric substance is bonded with a surface hydroxyl group and fixed in four- or five-orientation. When adjusted at low temperatures, an Al2Cl5 structure is formed, which is fixed as a dimeric substance with AlCl3 oriented in the AlCl2 species. It is conceived that the Al2Cl5 species has higher electrophilicity than the AlCl2 species as a result of AlCl3 oriented in AlCl2, whereas the hydroxyl group on the silica surface oriented with the Al2Cl5 species dissociates, discharging protons, thus showing strong acidity. 18 refs., 8 figs., 2 tabs.

  14. Dynamics and interactions of ibuprofen in cyclodextrin nanosponges by solid-state NMR spectroscopy

    Directory of Open Access Journals (Sweden)

    Monica Ferro

    2017-01-01

    Full Text Available 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.

  15. NMR characterization of simulated Hanford low-activity waste glasses and its use in understanding waste form chemical durability

    International Nuclear Information System (INIS)

    Darab, J.G.; Linehan, J.C.; McGrail, B.P.

    1999-01-01

    Magic Angle Spinning Nuclear Magnetic Resonance (MAS-NMR) spectroscopy has been used to characterize the structural and chemical environments of B, Al, and Si in model Hanford low-activity waste glasses. The average 29 Si NMR peak position was found to systematically change with changing glass composition and structure. From an understanding of the structural roles of Al and B obtained from MAS-NMR experiments, the authors first developed a model that reliably predicts the distribution of structural units and the average 29 Si chemical shift value, δ, based purely on glass composition. A product consistency test (PCT) was used to determine the normalized elemental release (NL) from the prepared glasses. Comparison of the NMR and PCT data obtained from sodium boro-aluminosilicate glasses indicates that a rudimentary exponential relationship exists between the 29 Si chemical shift value, and the boron NL value

  16. Bentonite pore structure based on SAXS, chloride exclusion and NMR studies

    International Nuclear Information System (INIS)

    Muurinen, A.; Carlsson, T.

    2013-11-01

    Water-saturated bentonite is planned to be used in many countries as an important barrier component in high-level nuclear waste (HLW) repositories. Knowledge about the microstructure of the bentonite and the distribution of water between interlayer and non-interlayer pores is important for modelling of long-term processes. In this work the microstructure of water-saturated samples prepared from Na montmorillonite, Ca-montmorillonite, sodium bentonite MX-80 and calcium bentonite Deponit CaN were studied with nuclear magnetic resonance (NMR) and small-angle xray scattering spectroscopy (SAXS). The sample dry densities ranged between 0.3 and 1.6 g/cm 3 . The NMR technique was used to get information about the volumes of different water types in the bentonite samples. The results were obtained using 1H NMR spin-lattice T 1ρ relaxation time measurements using the short inter-pulse method. The interpretation of the NMR results was made by fitting distributions of exponentials to observed decay curves. The SAXS measurements were used to get information about the size distribution of the interlayer distance of montmorillonite. The chloride porosity measurements and Donnan exclusion calculations were used together with the SAXS results for evaluation of the bentonite microstructure. The NMR studies and SAXS studies coupled with Cl porosity measurements provided very similar pictures of how the porewater is divided in interlayer and non-interlayer water in MX-80 bentonite. In the case where MX-80 of a dry density 1.6 g/cm 3 was equilibrated with 0.1 M NaCl solution, the results indicated an interlayer porosity of 30 % and non-interlayer porosity of 12 %. The interlayer space mainly contained two water layers but also spaces with more water layers were present. The average size of the non-interlayer pores was evaluated to be 120 - 150 A. From the montmorillonite surface area 98 % was interlayer and 2 % non-interlayer. Evaluation of the interlayer and non

  17. Multinuclear (27Al, 29Si, 47,49Ti) solid-state NMR of titanium substituted zeolite USY.

    Science.gov (United States)

    Ganapathy, S; Gore, K U; Kumar, Rajiv; Amoureux, Jean-Paul

    2003-01-01

    Multinuclear solid-state NMR spectroscopy, employing 29Si MAS,27Al MAS/3Q-MAS and (47,49)Ti wide-line experiments, has been used for the structural characterization of titanium substituted ultra-stable zeolite Y (Ti-USY). 27Al MAS experiments show the presence of aluminum in four (Al(IV)), five (Al(V)), and six (Al(VI)) coordination, whereas the multiplicity within Al(IV) and Al(VI) is revealed by 27Al 3Q-MAS experiments. Two different tetrahedral and octahedral Al environments are resolved and their isotropic chemical shifts (delta(CS)) and second-order quadrupole interaction parameters (P(Q)) have been determined by a graphical analysis of the 3Q-MAS spectra. The emergence of signal with higher intensity at -101 ppm in the 29Si MAS spectrum of Ti-USY samples indicates the possible occurrence of Q4(3Si,1Ti) type silicon environments due to titanium substitution in the faujasite framework. High-field (11.74T) operation, using a probehead specially designed to handle a large sample volume, has enabled the acquisition of 47,49Ti static spectra and identification of the titanium environment in the zeolite. The chemical shielding and electric field gradient tensors for the titanium environment in the zeolite have been determined by a computer simulation of the quadrupolar broadened static 47,49Ti NMR spectra.

  18. 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.

  19. An NMR relaxometry and gravimetric study of gelatin-free aqueous polyacrylamide dosimeters

    International Nuclear Information System (INIS)

    Babic, Steven; Schreiner, L John

    2006-01-01

    In conformal radiation therapy, a high dose of radiation is given to a target volume to increase the probability of cure, and care is taken to minimize the dose to surrounding healthy tissue. The techniques used to achieve this are very complicated and the precise verification of the resulting three-dimensional (3D) dose distribution is required. Polyacrylamide gelatin (PAG) dosimeters with magnetic resonance imaging and optical computed tomography scanning provide the required 3D dosimetry with high spatial resolution. Many basic studies have characterized these chemical dosimeters that polymerize under irradiation. However, the investigation of the fundamental properties of the radiation-induced polymerization in PAG dosimeters is complicated by the presence of the background gelatin matrix. In this work, a gelatin-free model system for the study of the basic radiation-induced polymerization in PAG dosimeters has been developed. Experiments were performed on gelatin-free dosimeters, named aqueous polyacrylamide (APA) dosimeters, containing equal amounts of acrylamide and N,N'-methylene-bisacrylamide. The APA dosimeters were prepared with four different total monomer concentrations (2, 4, 6 and 8% by weight). Nuclear magnetic resonance (NMR) spin-spin and spin-lattice proton relaxation measurements at 20 MHz, and gravimetric analyses performed on all four dosimeters, show a continuous degree of polymerization over the dose range of 0-25 Gy. The developed NMR model explains the relationship observed between the relaxation data and the amount of crosslinked polymer formed at each dose. This model can be extended with gelatin relaxation data to provide a fundamental understanding of radiation-induced polymerization in the conventional PAG dosimeters

  20. Pulsed NMR studies of crosslinking and entanglements in high molecular weight linear polydimethylsiloxanes

    International Nuclear Information System (INIS)

    Folland, R.; Charlesby, A.

    1977-01-01

    Pulsed NMR studies of proton spin relaxation are used to investigate both radiation-induced cross linking and entanglements in three high molecular weight linear polydimethylsiloxanes (Msub(w) = 26,000, 63,000 and 110,000). Particular emphasis is placed on the spin-spin relaxation since this is determined by the slower relative translational motions of the polymer chains and hence profoundly affected by the presence of intermolecular couplings such as crosslinks or entanglements. The spin-lattice relaxation times, T 1 , are determined by the fast anisotropic chain rotations and are rather insensitive to such intermolecular couplings. The spin-spin relaxation in these materials is represented by a double exponential decay involving two time constants, Tsub(2S) and Tsub(2L). The shorter component, Tsub(2S), is attributed to network material, which may be either of a dynamic form arising from temporary entanglements or of a permanent nature due to crosslinks. The concentration of entanglements depends on the initial molecular weight of the sample whereas the concentration of crosslinks is a function of the radiation dose. The longer component, Tsub(2L), is attributed to the non-network molecules. On the time scale of the NMR measurements the entanglements are shown to act in the same way as crosslinks. The variation of the relative proportions of network and non-network material with dose is shown to be accounted for by using standard gelation theory when allowance is made for the initial effective crosslink density due to entanglements. The analysis provides a value for the average molecular weight per entanglement point of 27,000 +- 1000 which is consistent with the critical molecular weight for entanglements of 29,000. The dependences of Tsub(2S) and Tsub(2L) on dose and molecular weight are also discussed in terms of the molecular motion. (author)

  1. Ab initio random structure searching of organic molecular solids: assessment and validation against experimental data† †Electronic supplementary information (ESI) available: Results of similarity analysis between the 11 structures of lowest energy obtained in the AIRSS calculations and the reported structures of form III and form IV of m-ABA; unit cell parameters and volumes for all structures considered; comparison of 2θ values derived from the unit cell parameters of different structural models representing form III of m-ABA; Le Bail fitting of the experimental powder XRD pattern of form IV of m-ABA recorded at 70 K using, as the initial structural model, the reported crystal structure following geometry optimization; table of calculated (GIPAW) absolute isotropic NMR shieldings; simulated powder XRD data for the considered structures after precise geometry optimization; experimental 1H MAS NMR spectra of forms III and IV. (pdf) The calculated and experimental data for this study are provided as a supporting dataset from WRAP, the Warwick Research Archive Portal at http://wrap.warwick.ac.uk/91884. See DOI: 10.1039/c7cp04186a

    Science.gov (United States)

    Zilka, Miri; Dudenko, Dmytro V.; Hughes, Colan E.; Williams, P. Andrew; Sturniolo, Simone; Franks, W. Trent; Pickard, Chris J.

    2017-01-01

    This paper explores the capability of using the DFT-D ab initio random structure searching (AIRSS) method to generate crystal structures of organic molecular materials, focusing on a system (m-aminobenzoic acid; m-ABA) that is known from experimental studies to exhibit abundant polymorphism. Within the structural constraints selected for the AIRSS calculations (specifically, centrosymmetric structures with Z = 4 for zwitterionic m-ABA molecules), the method is shown to successfully generate the two known polymorphs of m-ABA (form III and form IV) that have these structural features. We highlight various issues that are encountered in comparing crystal structures generated by AIRSS to experimental powder X-ray diffraction (XRD) data and solid-state magic-angle spinning (MAS) NMR data, demonstrating successful fitting for some of the lowest energy structures from the AIRSS calculations against experimental low-temperature powder XRD data for known polymorphs of m-ABA, and showing that comparison of computed and experimental solid-state NMR parameters allows different hydrogen-bonding motifs to be discriminated. PMID:28944393

  2. Functional studies using NMR

    International Nuclear Information System (INIS)

    McCready, V.R.; Leach, M.O.; Sutton; Ell, P.

    1986-01-01

    The object of this book is to discuss and evaluate an area of Nuclear Magnetic Resonance which to date has been less emphasized than it might be, namely the use of NMR for functional studies. The book commences with a discussion of the areas in which the NMR techniques might be needed due to deficiencies in other techniques. The physics of NMR especially relating to functional measurement are then explained. Technical factors in producing functional images are discussed and the use of paramagnetic substances for carrying out flow studies are detailed. Particular attention is paid to specific studies in the various organs. The book ends with a survey of imaging in each organ and the relation of NMR images to other techniques such as ultrasound, nuclear medicine and X-rays

  3. Functional studies using NMR

    International Nuclear Information System (INIS)

    McCready, V.R.; Leach, M.; Ell, P.J.

    1987-01-01

    This volume is based on a series of lectures delivered at a one-day teaching symposium on functional and metabolic aspects of NMR measurements held at the Middlesex Hospital Medical School on 1st September 1985 as a part of the European Nuclear Medicine Society Congress. Currently the major emphasis in medical NMR in vivo is on its potential to image and display abnormalities in conventional radiological images, providing increased contrast between normal and abnormal tissue, improved definition of vasculature, and possibly an increased potential for differential diagnosis. Although these areas are undeniably of major importance, it is probable that NMR will continue to complement conventional measurement methods. The major potential benefits to be derived from in vivo NMR measurements are likely to arise from its use as an instrument for functional and metabolic studies in both clinical research and in the everyday management of patients. It is to this area that this volume is directed

  4. NMR of unfolded proteins

    Indian Academy of Sciences (India)

    Unknown

    2005-01-03

    Jan 3, 2005 ... covering all the systems, so far discovered.5,7,8,12. With the increasing ... Structural investigations on proteins by NMR are, currently ... rapid analysis of unfolded proteins. ...... and hence help in design of drugs against them.

  5. Theory of NMR probe design

    International Nuclear Information System (INIS)

    Schnall, M.D.

    1988-01-01

    The NMR probe is the intrinsic part of the NMR system which allows transmission of a stimulus to a sample and the reception of a resulting signal from a sample. NMR probes are used in both imaging and spectroscopy. Optimal probe design is important to the production of adequate signal/moise. It is important for anyone using NMR techniques to understand how NMR probes work and how to optimize probe design

  6. PROPAGANDA POLITIK PARTAI GERINDRA DALAM GAME MAS GARUDA PADA PEMILU 2014 (Analisis Deskriptif Game Online Mas Garuda

    Directory of Open Access Journals (Sweden)

    Angga Satrya Putra

    2016-03-01

    Full Text Available The purpose of this study was to determine how the meaning of the look and content of the online game “Garuda Mas”. This game contains aspects of politically charged designations so that it can become a propaganda technique. The subject of this study is the game “Garuda Mas” which has been input on social media Facebook.Methods of data collection using documentary and literature. Data analysis using descriptive techniques. Data validity checking techniques using triangulation source.The results showed that the game “MAS GARUDA” can form the perspective of the players against Mas Garuda as a superhero figure hopes the Indonesian people who are able to overcome all the problems that exist in Indonesia. This game is a form of creative campaigns using propaganda techniques inserted in the game that has the power to change the mindset of every player. Change of mindset occurs because the player did not have an opportunity to think critically on aspects marking contained in the game. By indirectly the players will feel the emotional of this game and assume characterizations “Garuda Mas” in this game is a truth that can be believed.Keywords: Descriptive, Online Games, Mas Garuda, Partai Gerindra

  7. NMR and Electrochemical Investigation of the Transport Properties of Methanol and Water in Nafion and Clay-Nanocomposites Membranes for DMFCs

    Directory of Open Access Journals (Sweden)

    Vincenzo Baglio

    2012-06-01

    Full Text Available Water and methanol transport behavior, solvents adsorption and electrochemical properties of filler-free Nafion and nanocomposites based on two smectite clays, were investigated using impedance spectroscopy, DMFC tests and NMR methods, including spin-lattice relaxation and pulsed-gradient spin-echo (PGSE diffusion under variable temperature conditions. Synthetic (Laponite and natural (Swy-2 smectite clays, with different structural and physical parameters, were incorporated into the Nafion for the creation of exfoliated nanocomposites. Transport mechanism of water and methanol appears to be influenced from the dimensions of the dispersed platelike silicate layers as well as from their cation exchange capacity (CEC. The details of the NMR results and the effect of the methanol solution concentration are discussed. Clays particles, and in particular Swy-2, demonstrate to be a potential physical barrier for methanol cross-over, reducing the methanol diffusion with an evident blocking effect yet nevertheless ensuring a high water mobility up to 130 °C and for several hours, proving the exceptional water retention property of these materials and their possible use in the DMFCs applications. Electrochemical behavior is investigated by cell resistance and polarization measurements. From these analyses it is derived that the addition of clay materials to recast Nafion decreases the ohmic losses at high temperatures extending in this way the operating range of a direct methanol fuel cell.

  8. Ion conduction mechanisms and thermal properties of hydrated and anhydrous phosphoric acids studied with 1H, 2H, and 31P NMR.

    Science.gov (United States)

    Aihara, Yuichi; Sonai, Atsuo; Hattori, Mineyuki; Hayamizu, Kikuko

    2006-12-14

    To understand the behaviors of phosphoric acids in fuel cells, the ion conduction mechanisms of phosphoric acids in condensed states without free water and in a monomer state with water were studied by measuring the ionic conductivity (sigma) using AC impedance, thermal properties, and self-diffusion coefficients (D) and spin-lattice relaxation times (T1) with multinuclear NMR. The self-diffusion coefficient of the protons (H+ or H3O+), H2O, and H located around the phosphate were always larger than the diffusion coefficients of the phosphates and the disparity increased with increasing phosphate concentration. The diffusion coefficients of the samples containing D2O paralleled those in the protonated samples. Since the 1H NMR T1 values exhibited a minimum with temperature, it was possible to determine the correlation times and they were found to be of nanosecond order for a distance of nanometer order for a flip. The agreement of the ionic conductivities measured directly and those calculated from the diffusion coefficients indicates that the ion conduction obeys the Nernst-Einstein equation in the condensed phosphoric acids. The proton diffusion plays a dominant role in the ion conduction, especially in the condensed phosphoric acids.

  9. sup 7 sup 5 As NQR/NMR study of successive phase transitions and energy gap formation in Kondo semiconductor CeRhAs

    CERN Document Server

    Matsumura, M; Takabatake, T; Tsuji, S; Tou, H; Sera, M

    2003-01-01

    sup 7 sup 5 As NQR/NMR studies were performed to investigate the successive phase transitions found recently, the gap formation and their interplay in a Kondo semiconductor CeRhAs. NQR/NMR spectra in their respective phases change, reflecting lattice modulation modes, q sub 1 = (0, 1/2, 1/2), q sub 2 = (0, 1/3, 1/3) and q sub 3 = (1/3, 0, 0). In particular for well-resolved three NQR lines corresponding to the q sub 3 mode in the lowest temperature phase, the nuclear spin-lattice relaxation rate (T sub 1 T) sup - sup 1 shows an activation type T-dependence, suggesting a gap opening over the entire Fermi surface, in contrast to the V-shaped gap in isostructural CeNiSn and CeRhSn. The evaluated gap of 272 K and the bandwidth of about 4000 K are one order of magnitude larger than those in CeNiSn and CeRhSb. A lattice modulation forms a gap different from the V-shaped gap. (author)

  10. Water speciation in sodium silicate glasses (quenched melts): A comprehensive NMR study

    Science.gov (United States)

    Xue, X.; Kanzaki, M.; Eguchi, J.

    2012-12-01

    Dissolution mechanism of water is an important factor governing how the dissolved water affects the physical and thermodynamic properties of silicate melts and glasses. Our previous studies have demonstrated that 1H MAS NMR in combination with 29Si-1H and 27Al-1H double-resonance NMR experiments is an effective approach for unambiguously differentiating and quantifying different water species in quenched silicate melts (glasses). Several contrasting dissolution mechanisms have been revealed depending on the melt composition: for relatively polymerized melts, the formation of SiOH/AlOH species (plus molecular H2O) and depolymerization of the network structure dominate; whereas for depolymerized Ca-Mg silicate melts, free OH (e.g. MgOH) become increasingly important (cf. [1]). The proportion of free OH species has been shown to decrease with both increasing melt polymerization (silica content) and decreasing field strength of the network modifying cations (from Mg to Ca). Our previous 1H and 29Si MAS NMR results for hydrous Na silicate glasses of limited compositions (Na2Si4O9 and Na2Si2O5) were consistent with negligible free OH (NaOH) species and depolymerizing effect of water dissolution [2]. On the other hand, there were also other studies that proposed the presence of significant NaOH species in hydrous glasses near the Na2Si2O5 composition. The purpose of this study is apply the approach of combined 1H MAS NMR and double-resonance (29Si-1H and 23Na-1H) NMR to gain unambiguous evidence for the OH speciation in Na silicate glasses (melts) as a function of composition. Hydrous Na silicate glasses containing mostly ≤ 1 wt% H2O for a range of Na/Si ratios from 0.33 to 1.33 have been synthesized by rapidly quenching melts either at 0.2 GPa using an internally heated gas pressure vessel or at 1 GPa using a piston cylinder high-pressure apparatus. NMR spectra have been acquired using a 9.4 T Varian Unity-Inova spectrometer. The 29Si and 1H chemical shifts are

  11. {sup 119}Sn NMR investigations on superconducting Ca{sub 3}Ir{sub 4}Sn{sub 13}

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, Rajib; Brueckner, Felix; Guenther, Marco; Klauss, Hans-Henning [IFP, TU Dresden (Germany); Petrovic, Cedomir; Wang, Kefeng [CMPMS, BNL, Upton, NY (United States); Luetkens, Hubertus; Biswas, Pabitra; Morenzoni, Elvezio; Amato, Alex [PSI, Villigen (Switzerland)

    2014-07-01

    Ca{sub 3}Ir{sub 4}Sn{sub 13} was found to exhibit superconducting transition with T{sub c} ∼ 7 K. It received considerable attention due to the possible coexistence of superconductivity and ferromagnetic spin fluctuation as well as the three-dimensional charge density wave (CDW) from the superlattice transition. While thermal, transport, and thermodynamic characterization of Ca{sub 3}Ir{sub 4}Sn{sub 13} single crystals suggest that it is a weakly correlated nodeless superconductor, recent μSR investigation reveals that the electron-phonon pairing interaction is in the strong-coupling limit. Here we present {sup 119}Sn NMR investigations on Ca{sub 3}Ir{sub 4}Sn{sub 13} polycrystalline samples and discuss the symmetry of the superconducting order parameter together with the normal state properties. Our preliminary results of spin-lattice relaxation rate (1/T{sub 1}) indicate that this is a BCS superconductor with weak-coupling limit.

  12. Synthesis, characterization, and solid-state NMR investigation of organically modified bentonites and their composites with LDPE.

    Science.gov (United States)

    Borsacchi, Silvia; Sudhakaran, Umayal; Geppi, Marco; Ricci, Lucia; Liuzzo, Vincenzo; Ruggeri, Giacomo

    2013-07-23

    Polymer/clay nanocomposites show remarkably improved properties (mechanical properties, as well as decreased gas permeability and flammability, etc.) with respect to their microscale counterparts and pristine polymers. Due to the substantially apolar character of most of the organic polymers, natural occurring hydrophilic clays are modified into organophilic clays with consequent increase of the polymer/clay compatibility. Different strategies have been developed for the preparation of nanocomposites with improved properties, especially aimed at achieving the best dispersion of clay platelets in the polymer matrix. In this paper we present the preparation and characterization of polymer/clay nanocomposites composed of low-density polyethylene (LDPE) and natural clay, montmorillonite-containing bentonite. Two different forms of the clay have been considered: the first, a commercial organophilic bentonite (Nanofil 15), obtained by exchanging the natural cations with dimethyldioctadecylammonium (2C18) cations, and the second, obtained by performing a grafting reaction of an alkoxysilane containing a polymerizable group, 3-(trimethoxysilyl)propyl methacrylate (TSPM), onto Nanofil 15. Both the clays and LDPE/clay nanocomposites were characterized by thermal, FT-IR, and X-ray diffraction techniques. The samples were also investigated by means of (29)Si, (13)C, and (1)H solid-state NMR, obtaining information on the structural properties of the modified clays. Moreover, by exploiting the effect of bentonite paramagnetic (Fe(3+)) ions on proton spin-lattice relaxation times (T1's), useful information about the extent of the polymer-clay dispersion and their interfacial interactions could be obtained.

  13. 1.48 GHz (34.8 T) ^1H NMR measurements of SDW fluctuations in (TMTSF)_2PF_6

    Science.gov (United States)

    Clark, W. G.; Vonlanthen, P.; Goto, A.; Tanaka, K. B.; Alavi, B.; Kuhns, P.; Reyes, A. P.; Moulton, W. G.

    2001-03-01

    We report ^1H spin-lattice relaxation rate (T_1-1) measurements that probe the spin-density-wave (SDW) fluctuations in the quasi 1-d system (TMTSF)_2PF6 up to 1.48 GHz (34.8 T) in the NHMFL hybrid magnet. In the critical regime above the SDW transition near 12 K, T_1-1 has no frequency dependence and the angular dependence of T_1-1 attributed to the spin-flop condition in the ordered phase is absent. These results indicate that amplitude fluctuations of the SDW drive T_1-1 in the critical regime and that the SDW critical fluctuation correlation time is <1× 10-10 s. Somewhat below the transition, T_1-1 continues the decrease with increasing NMR frequency observed at lower frequencies. We attribute it to the power spectrum of the SDW phason fluctuations. The dependence of T_1-1 upon the field orientation in this phase reflects the spin-flop condition, but with parameters that are different from the expected ones. The UCLA part of this work was supported by NSF Grants DMR-9705369 and DMR-0072524.

  14. Nematic fluctuations in iron arsenides NaFeAs and LiFeAs probed by 75As NMR

    Science.gov (United States)

    Toyoda, Masayuki; Kobayashi, Yoshiaki; Itoh, Masayuki

    2018-03-01

    75As NMR measurements have been made on single crystals to study the nematic state in the iron arsenides NaFeAs, which undergoes a structural transition from a high-temperature (high-T ) tetragonal phase to a low-T orthorhombic phase at Ts=57 K and an antiferromagnetic transition at TN=42 K, and LiFeAs having a superconducting transition at Tc=18 K. We observe the in-plane anisotropy of the electric field gradient η even in the tetragonal phase of NaFeAs and LiFeAs, showing the local breaking of tetragonal C4 symmetry. Then, η is found to obey the Curie-Weiss (CW) law as well as in Ba (Fe1-xCox) 2As2 . The good agreement between η and the nematic susceptibility obtained by electronic Raman spectroscopy indicates that η is governed by the nematic susceptibility. From comparing η in NaFeAs and LiFeAs with η in Ba (Fe1-xCox) 2As2 , we discuss the carrier-doping dependence of the nematic susceptibility. The spin contribution to nematic susceptibility is also discussed from comparing the CW terms in η with the nuclear spin-lattice relaxation rate divided by temperature 1 /T1T . Finally, we discuss the nematic transition in the paramagnetic orthorhombic phase of NaFeAs from the in-plane anisotropy of 1 /T1T .

  15. NMR relaxation in natural soils: Fast Field Cycling and T1-T2 Determination by IR-MEMS

    Science.gov (United States)

    Haber-Pohlmeier, S.; Pohlmeier, A.; Stapf, S.; van Dusschoten, D.

    2009-04-01

    Soils are natural porous media of highest importance for food production and sustainment of water resources. For these functions, prominent properties are their ability of water retainment and transport, which are mainly controlled by pore size distribution. The latter is related to NMR relaxation times of water molecules, of which the longitudinal relaxation time can be determined non-invasively by fast-field cycling relaxometry (FFC) and both are obtainable by inversion recovery - multi-echo- imaging (IR-MEMS) methods. The advantage of the FFC method is the determination of the field dependent dispersion of the spin-lattice relaxation rate, whereas MRI at high field is capable of yielding spatially resolved T1 and T2 times. Here we present results of T1- relaxation time distributions of water in three natural soils, obtained by the analysis of FFC data by means of the inverse Laplace transformation (CONTIN)1. Kaldenkirchen soil shows relatively broad bimodal distribution functions D(T1) which shift to higher relaxation rates with increasing relaxation field. These data are compared to spatially resolved T1- and T2 distributions, obtained by IR-MEMS. The distribution of T1 corresponds well to that obtained by FFC.

  16. {sup 23}Na nuclear magnetic resonance study of the structure and dynamic of natrolite

    Energy Technology Data Exchange (ETDEWEB)

    Paczwa, Mateusz; Olszewski, Marcin; Sergeev, Nikolaj [Szczecin Univ. (Poland). Inst. of Physics; Sapiga, Aleksej A.; Sapiga, Aleksej V. [Taurida National V.I. Vernadsky Univ., Simferopol, Crimea (Ukraine)

    2015-07-01

    The temperature dependences of nuclear magnetic resonance (NMR) and magic angle spinning (MAS) NMR spectra of {sup 23}Na nuclei in natrolite (Na{sub 2}Al{sub 2}Si{sub 3}O{sub 10} . 2H{sub 2}O) have been studied. The temperature dependences of the spin-lattice relaxation times T{sub 1} in natrolite have also been studied. It has been shown that the spin-lattice relaxation of the {sup 23}Na is governed by the electric quadrupole interaction with the crystal electric field gradients modulated by translational motion of H{sub 2}O molecules in the natrolite pores. The dipolar interactions with paramagnetic impurities become significant as a relaxation mechanism of the {sup 23}Na nuclei only at low temperature (<270 K).

  17. Hexagonal ice in pure water and biological NMR samples

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Thomas; Gath, Julia; Hunkeler, Andreas; Ernst, Matthias, E-mail: maer@ethz.ch [ETH Zurich, Physical Chemistry (Switzerland); Böckmann, Anja, E-mail: a.bockmann@ibcp.fr [UMR 5086 CNRS, Université de Lyon 1, Institut de Biologie et Chimie des Protéines (France); Meier, Beat H., E-mail: beme@ethz.ch [ETH Zurich, Physical Chemistry (Switzerland)

    2017-01-15

    Ice, in addition to “liquid” water and protein, is an important component of protein samples for NMR spectroscopy at subfreezing temperatures but it has rarely been observed spectroscopically in this context. We characterize its spectroscopic behavior in the temperature range from 100 to 273 K, and find that it behaves like pure water ice. The interference of magic-angle spinning (MAS) as well as rf multiple-pulse sequences with Bjerrum-defect motion greatly influences the ice spectra.

  18. Characterization of zeolites by magic-angle-spinning NMR

    International Nuclear Information System (INIS)

    Brunner, E.; Ernst, H.; Freude, D.; Hunger, M.; Pfeifer, H.

    1988-01-01

    Magic-angle-spinning nuclear magnetic resonance (MAS NMR) has been used to study structure defects in TPA/ZSM-5, the dealumination process caused by hydrothermal treatment and acid leaching of zeolites, the influence of Lewis sites upon water as a probe molecule, the boron incorporation into the ZSM-5 framework, and the acid sites and structure defects in SAPO-5. The nuclei under study are 1 H, 11 B, 27 Al, 29 Si, and 31 P. 24 refs.; 7 figs.; 1 table

  19. 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

  20. 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...

  1. Microprocessorized NMR measurement

    International Nuclear Information System (INIS)

    Rijllart, A.

    1984-01-01

    An MC68000 CAMAC microprocessor system for fast and accurate NMR signal measurement will be presented. A stand-alone CAMAC microprocessor system (MC68000 STAC) with a special purpose interface sweeps a digital frequency synthesizer and digitizes the NMR signal with a 16-bit ADC of 17 μs conversion time. It averages the NMR signal data over many sweeps and then transfers it through CAMAC to a computer for calculation of the signal parameters. The computer has full software control over the timing and sweep settings of this signal averager, and thus allows optimization of noise suppression. Several of these processor systems can be installed in the same crate for parallel processing, and the flexibility of the STAC also allows easy adaptation to other applications such as transient recording or phase-sensitive detection. (orig.)

  2. 139La and 63Cu NMR investigation of charge order in La2CuO4 +y (Tc=42 K)

    Science.gov (United States)

    Imai, T.; Lee, Y. S.

    2018-03-01

    We report 139La and 63Cu NMR investigation of the successive charge order, spin order, and superconducting transitions in superoxygenated La2CuO4 +y single crystal with stage-4 excess oxygen order at Tstage≃290 K. We show that the stage-4 order induces tilting of CuO6 octahedra below Tstage, which in turn causes 139La NMR line broadening. The structural distortion continues to develop far below Tstage, and completes at Tcharge≃60 K, where charge order sets in. This sequence is reminiscent of the the charge-order transition in Nd codoped La1.88Sr0.12CuO4 that sets in once the low-temperature tetragonal phase is established. We also show that the paramagnetic 63Cu NMR signals are progressively wiped out below Tcharge due to enhanced low-frequency spin fluctuations in charge-ordered domains, but the residual 63Cu NMR signals continue to exhibit the characteristics expected for optimally doped superconducting CuO2 planes. This indicates that charge order in La2CuO4 +y does not take place uniformly in space. In addition, unlike the typical second-order magnetic phase transitions, low-frequency Cu spin fluctuations as probed by 139La nuclear spin-lattice relaxation rate do not exhibit critical divergence at Tspin(≃Tc ) =42 K. These findings, including the spatially inhomogeneous nature of the charge-ordered state, are qualitatively similar to the case of La1.885Sr0.115CuO4 [Imai et al., Phys. Rev. B 96, 224508 (2017), 10.1103/PhysRevB.96.224508 and Arsenault et al., Phys. Rev. B 97, 064511 (2018), 10.1103/PhysRevB.97.064511], but both charge and spin order take place more sharply in the present case.

  3. C-13 NMR spectra of all-trans-N-retinylidene-n-butylamine as an analogue of the Schiff base linkage compound in visual pigment

    Energy Technology Data Exchange (ETDEWEB)

    Tokito, Y; Inoue, Y; Chujo, R [Tokyo Inst. of Tech. (Japan). Faculty of Science; Miyoshi, Y

    1975-01-01

    In the process of visual excitation, a visual pigment, rhodopsin, plays a role of a photoreceptor, and it has been known that the first step in the process is the photoisomerization of the rhodopsin visual chromophore. The bathochromic shift has been regarded as the result of the formation of Schiff base linkage of retinal with opsin. In this study, C-13 NMR spectra were obtained for the analogue of the compound with Schiff base linkage in the visual pigment, and the chemical shift change for going from all trans-retinal to all trans-N-retinylidene-n-butylamine (NRB) was discussed. Further, the effect of N protonation in NRB was examined as the reflection of the function of visual pigment. The compound with Schiff base linkage of all trans-retinal with n-butylamine, namely NRB, was used. The nuclear magnetic resonance (NMR) spectra of carbon-13 Fourier transformation were obtained for this sample at natural abundance with a JNM PS-100 spectrometer. In the C-13 FT NMR spectrum of NRB, besides eight peaks in the C-13 NMR of all trans-retinal, four peaks were observed in higher field region. They originated from the portion of n-butylamine in the compound with Schiff base linkage. The peaks in lower field region were assigned to eleven conjugated polyene carbons by the measurement of spin-lattice relaxation time and shift. The chemical shift change for going from retinal to NRB is shown. It is concluded that the ..pi..-electrons in polyene chains are considerably delocalized by the collapse of bond alteration in the retinal forming Schiff base linkage.

  4. Unusual spin frozen state in a frustrated pyrochlore system NaCaCo{sub 2}F{sub 7} as observed by NMR

    Energy Technology Data Exchange (ETDEWEB)

    Sarkar, R.; Brueckner, F.; Klauss, H.H. [IFP, TU Dresden (Germany); Krizan, J.W.; Cava, R.J. [Department of Chemistry, Princeton University, Princeton, NJ (United States)

    2016-07-01

    We present {sup 23}Na -and {sup 19}F NMR results on the magnetically frustrated pyrochlore NaCaCo{sub 2}F{sub 7} with a frustration index of f = θ{sub CW}/T{sub f} ∝ 56. Recent neutron scattering experiments proposed XY like antiferromagnetic spin clusters at low energies in NaCaCo{sub 2}F{sub 7}. {sup 23}Na NMR -spectra reveal the presence of two magnetically non equivalent Na sites in conjunction with the local Co{sup 2+} spin structure. Below 3.6 K both the {sup 23}Na -and {sup 19}F spectra broaden due to the formation of static spin correlations. A huge reduction of the {sup 19}F -and {sup 23}Na NMR signal intensity hints at a quasi-static field distribution in NaCaCo{sub 2}F{sub 7} in this regime. The {sup 19}F spin-lattice relaxation rate {sup 19}(1/T{sub 1}) exhibits a peak at around 2.9 K, at the same temperature range where ac and dc susceptibility data show a broad maximum. The character of the spin fluctuation appears to be isotropic. The overall temperature dependence of {sup 19}(1/T{sub 1}) can be described by the BPP theory considering a fluctuating hyperfine field with an autocorrelation function. The correlation time of the autocorrelation function exhibits an activation behavior further indicating the spin-frozen state. While the present NMR studies suggest the spin frozen state at low temperatures, μSR investigations however reveal the presence of so called persistent spin dynamics down to 20 mK implying an exotic ground state in NaCaCo{sub 2}F{sub 7}.

  5. Fourier transform NMR

    International Nuclear Information System (INIS)

    Hallenga, K.

    1991-01-01

    This paper discusses the concept of Fourier transformation one of the many precious legacies of the French mathematician Jean Baptiste Joseph Fourier, essential for understanding the link between continuous-wave (CW) and Fourier transform (FT) NMR. Although in modern FT NMR the methods used to obtain a frequency spectrum from the time-domain signal may vary greatly, from the efficient Cooley-Tukey algorithm to very elaborate iterative least-square methods based other maximum entropy method or on linear prediction, the principles for Fourier transformation are unchanged and give invaluable insight into the interconnection of many pairs of physical entities called Fourier pairs

  6. 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; Yamasaki, Shizuo; Takahashi, Rui; Asakura, Tetsuo

    2010-01-01

    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

  7. International symposium on NMR spectroscopy

    International Nuclear Information System (INIS)

    The publication consists of 32 papers and presentations from the field of NMR spectroscopy applications submitted to the International Symposium on NMR Spectroscopy held at Smolenice between 29 Sep and 3 Oct, 1980. (B.S.)

  8. 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.

  9. 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. Copyright © 2016 John Wiley & Sons, Ltd.

  10. NMR studies of chemical structural variation of insoluble organic matter from different carbonaceous chondrite groups

    Science.gov (United States)

    Cody, George D.; Alexander, Conel M. O.'D.

    2005-02-01

    Solid-state 1H and 13C Nuclear Magnetic Resonance (NMR) spectroscopic experiments have been performed on isolated meteoritic Insoluble Organic Matter (IOM) spanning four different carbonaceous chondrite meteorite groups; a CR2 (EET92042), a CI1 (Orgueil), a CM2 (Murchison), and the unique C2 meteorite, Tagish Lake. These solid state NMR experiments reveal considerable variation in bulk organic composition across the different meteorite group's IOM. The fraction of aromatic carbon increases as CR2 meteorite groups. Single pulse (SP) 13C magic angle spinning (MAS) NMR experiments reveal the presence of nanodiamonds with an apparent concentration ranking in the IOM of CR2 IOM of all four meteoritic IOM fractions are highly substituted. Fast spinning SP 1H MAS NMR spectral data combined with other NMR experimental data reveal that the average hydrogen content of sp 3 bonded carbon functional groups is low, requiring a high degree of aliphatic chain branching in each IOM fraction. The variation in chemistry across the meteorite groups is consistent with alteration by low temperature chemical oxidation. It is concluded that such chemistry principally affected the aliphatic moieties whereas the aromatic moieties and nanodiamonds may have been largely unaffected.

  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. Solid-state 29Si NMR and FTIR analyses of lignin-silica coprecipitates

    DEFF Research Database (Denmark)

    Cabrera Orozco, Yohanna; Cabrera, Andrés; Larsen, Flemming Hofmann

    2016-01-01

    When agricultural residues are processed to ethanol, lignin and silica are some of the main byproducts. Separation of these two products is difficult and the chemical interactions between lignin and silica are not well described. In the present study, the effect of lignin-silica complexing has been...... investigated by characterizing lignin and silica coprecipitates by FTIR and solid state NMR. Silica particles were coprecipitated with three different lignins, three lignin model compounds, and two silanes representing silica-in-lignin model compounds. Comparison of 29Si SP/MAS NMR spectra revealed differences...

  13. 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

    for the C-S-H phase formed during hydration. It will be demonstrated that Al3+ and flouride guest-ions in the anhydrous and hydrated calcium silicates can be studied in detail by 27Al and 19F MAS NMR, thereby providing information on the local structure and the mechanisms for incorporation of these ions......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......- and second-coordination spheres of the spin nucleus under investigation while it is less sensitive to long-range order. Thus, crystalline as well as amorphous phases can be detected in a quantitative manner by solid-state NMR. In particular the structure of the calcium-silicate-hydrate (C-S-H) phase have...

  14. 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 the vegetative growth stage had little effect on the parameters investigated. For the first time, H-1 HR-MAS NMR spectra of grains taken during grain-filling were analysed by an advanced multiway model. In addition to the results from the chemical protein analysis and the H-1 HR-MAS NMR spectra of single kernels...... was to examine the implications of different drought treatments on the protein fractions in grains of winter wheat using H-1 nuclear magnetic resonance spectroscopy followed by chemometric analysis. Triticum aestivum L. cv. Vinjett was studied in a semi-field experiment and subjected to drought episodes either...... 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...

  15. The MAS Six Years in Power in Bolivia

    Directory of Open Access Journals (Sweden)

    Ton Salman

    2012-04-01

    Full Text Available Review Essay of:– The Rise of Evo Morales and the MAS, by Sven Harten. London/New York: Zed Books, 2011.– Evo Morales and the Movimiento al Socialismo in Bolivia; The First Term in Context, edited by Adrian J. Pearce. London, Institute for the Study of the Americas, 2011.– El estado de derecho como tiranía, by Luis Tapia. La Paz: CIDES/UMSA, 2011.– From Rebellion to Reform in Bolivia: Class Struggle, Indigenous Liberation and the Politics of Evo Morales, by Jeffery R. Webber. Chicago: Haymarket Books, 2011.– La democracia desde los márgenes: Transformaciones en el campo político boliviano, by María Teresa Zegada, with Claudia Arce, Gabriela Canedo and Alber Quispe. La Paz: Muela del Diablo Editores/CLACSO, 2011.

  16. 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

  17. 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.

  18. 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 There are a few traditional methods of analysing the chemical properties of cellulose I. Some of these methods include the Permanganate number determination, which is used to obtain the lignin content of the pulp [12]. The acid insoluble lignin content... – Fundamental Aspects 88 [10] Fengel D, Wegener G. Wood Chemistry, Ultrastructure, Reactions, Walter de Gruyter; 1984. [11] Uhlmann T. Ullmann's encyclopedia of industrial chemistry. Paper and Pulp. 1991; 18 (A). [12] Permanganate number of pulp, Tappi T...

  19. 31P-NMR spectroscopy in measurements of physiological parameters and response to therapy of human melanoma xenografts

    International Nuclear Information System (INIS)

    Olsen, Dag Rune

    1999-01-01

    The aim of the study was to investigate whether ''31P-NMR spectroscopy can be utilized in prediction and monitoring of response to therapy or tumours. The specific aims were: 1) To investigate possible correlations between on the one hand bio energetics status, phospholipids resonance ratios, intracellular pH and phosphorus T 1 s and on the other hand tumour blood supply and oxygenation, tumour proliferation and necrotic fraction across tumour lines. 2) Reveal possible correlations between changes in tumour bio energetics status and phosphorus T 1 s and the changes in tumour blood flow, tumour oxygenation and necrotic fraction. 3) To investigate whether irradiation and hyperthermia treatment of tumours affect bio energetics status and phosphorus T 1 s. 4) To identify the tumour physiological factors that is effected by the treatment and influence the bio energetics status and phosphorus T 1 s. The results are presented in 8 papers with titles: 1)''31P-nuclear magnetic resonance spectroscopy in vivo of six human melanoma zeno graft lines: Tumour bio energetic status and blood supply. 2) ''31P NMR spectroscopy studies of phospholipid metabolism in human melanoma xenograft lines differing in rate of tumour cell proliferation. 3) ''31P-nuclear magnetic resonance spectroscopy in vivo of four human melanoma xenograft lines: Spin-lattice relaxation times. 4) Effect of melanin on phosphorus T 1 s in human melanoma xenografts studied by ''31P MRS 5) Spin-lattice relaxation time of inorganic phosphate in human tumour xenografts measured in vivo by ''31P-magnetic resonance spectroscopy influence of oxygen tension. 6) Effects of hyperthermia on bio energetic status and phosphorus T 1 s in human melanoma xenografts monitored by ''31P-MRS. 7) Monitoring of tumour reoxygenation following irradiation by ''31P magnetic resonance spectroscopy an experimental study of human melanoma xenografts. 8) Radiation-induced changes in phosphorus T 1 values in human melanoma xenografts studied

  20. Solid state NMR studies for a new carbonization process with high temperature preheating

    Science.gov (United States)

    Saito, Koji; Hatakeyama, Moriaki; Komaki, Ikuo; Katoh, Kenji

    2002-01-01

    A new carbonization process with rapid preheating and coke discharging at medium temperature has been developed in Japan. The result of this process shows that even when no or slightly coking coal is by 50 wt% the coking property is improved and a coking coke with cold strength usable at blast furnace can be manufactured with the new carbonization process. The mechanism of the coking property improvement was examined by coal properties using mainly solid state NMR ( 1H CRAMPS and 13C SPE/MAS, CP/MAS) and NMR imaging (single point imaging, in-situ imaging). It has been clarified that the molecular structure of coal is relaxed by the rapid heating treatment and, in addition, there is a close relation between hydrogen bonding and relaxation of the molecular structure of coal.

  1. Investigation of new NMR methods for structural and dynamic studies in the liquid state

    International Nuclear Information System (INIS)

    Desvaux, H.

    1993-01-01

    After a short presentation of the NMR fundements, three new methods of spin -lattice relaxation in liquids are reported. (1) The method consists of measuring the steady-state nuclear magnetization under strong off-resonance rf irradiation as a function of the angle θ between external field and effective field. For purely dipolar relaxation between homonuclear spins under isotropic Brownian molecular rotation, this variation yields the value of the local correlation time. A departure from the theoretical shape reveals the existence of complex motions or complex relaxation mechanisms. These results have been verified by experimental illustrations. Some numerical simulations have been performed for studying the effects of the distribution of chemical shift and for studying the coherence of the local correlation time concept. (2) The improvements of a modified ROESY experiment are discussed. The use of a time-modulated strong off-resonances rf irradiation permits to suppress totally the problems of the NOESY (suppression of cross-relaxation peaks for molecules where ωτ c ≅ 1.1) and of the ROESY (HOHAHA transfer and angular dispersion due to the chemical shift distribution). The angle θ defined previously can be used as a constraint: either to obtain a ratio of the cross over direct dipolar relaxation rates independent on the correlation time value, or to observe the sole chemical exchange. (3) The difference of the relaxation rates of the coherences at zero and two quanta is always exactly the cross relaxation rates measured by the NOESY experiment. The experimental illustration is presented

  2. The effects of bone on proton NMR relaxation times of surrounding liquids

    Science.gov (United States)

    Davis, C. A.; Genant, H. K.; Dunham, J. S.

    1986-01-01

    Preliminary attempts by our group at UCSF to assess fat content of vertebral marrow in the lumbar spine using relaxation time information demonstrated that the presence of trabecular bone affects relaxation times. The objective of this work was a thorough study of the effects of bone on NMR relaxation characteristics of surrounding liquids. Trabecular bone from autopsy specimens was ground up and sifted into a series of powders with graded densities ranging from 0.3 gm/cc to 0.8 gm/cc. Each powder was placed first in n-saline and then in cottonseed oil. With spectroscopy, spin-lattice relaxation times (T1) and effective spin-spin relaxation times (T2*) were measured for each liquid in each bone powder. As bone density and surface to volume ratio increased, T1 decreased faster for saline than for oil. T2* decreased significantly for both water and oil as the surface to volume ratio increased. It was concluded that effects of water on T1 could be explained by a surface interaction at the bone/liquid interface, which restricted rotational and translational motion of nearby molecules. The T1s of oil were not affected since oil molecules are nonpolar, do not participate in significant intermolecular hydrogen bonding, and therefore would not be expected to interact strongly with the bone surface. Effects on T2* could be explained by local magnetic field inhomogeneities created by discontinuous magnetic susceptibility near the bone surface. These preliminary results suggest that water in contact with trabecular bone in vivo will exhibit shortened relaxation times.

  3. Gadolinium-Encapsulating Iron Oxide Nanoprobe as Activatable NMR/MRI Contrast Agent

    Science.gov (United States)

    Santra, Santimukul; Jativa, Samuel D.; Kaittanis, Charalambos; Normand, Guillaume; Grimm, Jan; Perez, J. Manuel

    2012-01-01

    Herein we report a novel gadolinium-encapsulating iron oxide nanoparticle-based activatable NMR/MRI nanoprobe. In our design, Gd-DTPA is encapsulated within the polyacrylic acid (PAA) polymer coating of a superparamagnetic iron oxide nanoparticle (IO-PAA) yielding a composite magnetic nanoprobe (IO-PAA-Gd-DTPA) with quenched longitudinal spin-lattice magnetic relaxation (T1). Upon release of the Gd-DTPA complex from the nanoprobe's polymeric coating in acidic media, an increase in the T1 relaxation rate (1/T1) of the composite magnetic nanoprobe was observed, indicating a dequenching of the nanoprobe with a corresponding increase in the T1-weighted MRI signal. When a folate-conjugated nanoprobe was incubated in HeLa cells, a cancer cell line overexpressing folate receptors, an increase in the 1/T1 signal was observed. This result suggests that upon receptor-mediated internalization, the composite magnetic nanoprobe degraded within the cell's lysosome acidic (pH = 5.0) environment, resulting in an intracellular release of Gd-DTPA complex with subsequent T1 activation. No change in T1 was observed when the Gd-DTPA complex was chemically conjugated on the surface of the nanoparticle's polymeric coating or when encapsulated in the polymeric coating of a non-magnetic nanoparticle. These results confirmed that the observed (T1) quenching of the composite magnetic nanoprobe is due to the encapsulation and close proximity of the Gd ion to the nanoparticles superparamagnetic iron oxide (IO) core. In addition, when an anticancer drug (Taxol) was co-encapsulated with the Gd-DTPA within the folate receptor targeting composite magnetic nanoprobe, the T1 activation of the probe coincide with the rate of drug release and corresponding cytotoxic effect in cell culture studies. Taken together, these results suggest that our activatable T1 nanoagent could be of great importance for the detection of acidic tumors and assessment of drug targeting and release by MRI. PMID:22809405

  4. Possible quadrupolar nematic phase in the frustrated spin chain LiCuSbO4: An NMR investigation

    Science.gov (United States)

    Bosiočić, M.; Bert, F.; Dutton, S. E.; Cava, R. J.; Baker, P. J.; Požek, M.; Mendels, P.

    2017-12-01

    The frustrated one-dimensional quantum magnet LiCuSbO4 is a rare realization of the J1-J2 spin chain model with an easily accessible saturation field, formerly estimated at 12 T. Exotic multipolar nematic phases were theoretically predicted in such compounds just below the saturation field, but without unambiguous experimental observation so far. In this paper we present extensive experimental research on the compound in a wide temperature (30 mK to 300 K) and field (0-13.3 T) range by muon spin rotation (μ SR ), 7Li nuclear magnetic resonance (NMR), and magnetic susceptibility (SQUID). μ SR experiments in zero magnetic field demonstrate the absence of long-range 3D ordering down to 30 mK. Together with former heat capacity data [Dutton et al., Phys. Rev. Lett. 108, 187206 (2012), 10.1103/PhysRevLett.108.187206], magnetic susceptibility measurements suggest a short-range-correlated vector chiral phase in the field range 0-4 T. At the intermediate-field values (5-12 T), the system enters a 3D-ordered spin density wave phase with 0.75 μB per copper site at lowest temperatures (125 mK), estimated by NMR. At still higher field, the magnetization is found to be saturated above 13 T where the spin lattice T1-1 relaxation reveals a spin gap estimated at 3.2(2) K. We narrow down the possibility of observing a multipolar nematic phase to the range 12.5-13 T.

  5. NMR evidence for spin fluctuations in underdoped LaO{sub 1-x}F{sub x}FeAs

    Energy Technology Data Exchange (ETDEWEB)

    Hammerath, Franziska; Grafe, Hans-Joachim; Lang, Guillaume; Behr, Guenter; Werner, Jochen; Buechner, Bernd [Leibniz-Institut fuer Festkoerper- und Werkstoffforschung, Dresden (Germany); Paar, Dalibor [Department of Physics, Faculty of Science, University of Zagreb (Croatia)

    2012-07-01

    We present {sup 75}As Nuclear Magnetic Resonance (NMR) measurements on the iron-based superconductor LaO{sub 1-x}F{sub x}FeAs with 0 {<=} x {<=} 0.1, covering a broad range of the phase diagram from magnetically-ordered to optimally-doped superconducting samples. For underdoped samples (x=0.05,x=0.075) the {sup 75}As NMR spin-lattice relaxation rate (T{sub 1}T){sup -1} shows a Curie-Weiss-like increase at intermediate temperatures, indicating the slowing down of spin fluctuations. However, a simple Curie-Weiss fit fails to describe (T{sub 1}T){sup -1}(T) above 250 K and the occurrence of a peak in (T{sub 1}T){sup -1} slightly above T{sub c}. Instead, the data can be well described by considering a BPP-model for fluctuating magnetic fields in combination with a doping-independent linear temperature dependence at high temperature. At optimal doping (x=0.1) spin fluctuations are suppressed and only the linear contribution to (T{sub 1}T){sup -1} is left. This stands in contrast to other pnictides, such as Ba(Fe{sub 1-x}Co{sub x}As){sub 2} and Ba(FeAs{sub 1-x}P{sub x}){sub 2}. Our analysis is consistent with charge carrier localization in underdoped LaO{sub 1-x}F{sub x}FeAs as seen by means of resistivity measurements.

  6. 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.

  7. Synthesis and NMR characterization of SAPO-35 from non-aqueous systems using hexamethyleneimine template

    International Nuclear Information System (INIS)

    Venkatathri, N.

    2005-01-01

    SAPO-35 was synthesized using hexamethyleneimine template in non-aqueous systems. X-ray diffraction and scanning electron micrograph analysis shows the synthesized sample is pure and well crystalline. Presence of four stages (1.6%, 0.8%, 7.8% and 8.4%) of weight loss is observed by TG/DTA analysis. FT-IR analysis in the framework region shows the presence of tetrahedral T-O-T vibrations is similar to the other known aluminophosphate molecular sieves. FT-IR spectrum in the -OH region shows stretching vibrations at 3631, 3604 and 3580 cm -1 can be assigned to OH groups in bigger cages near S6R, in bigger cages near D6R and those actually confined inside the D6R, respectively. The spectra for the as-synthesized sample show a single symmetrical 27 Al MAS NMR line at δ = 36.26 indicating the presence of a single tetrahedral aluminium species. Where as 29 Si and 31 P MAS NMR shows the presence of two peaks in both at (-89.9 and -95.15 ppm) and (-34.01 and -40.45 ppm) due to the Si substitution of P present in two different locations in double 6 ring (D6R) and in single 6 ring (S6R). 27 Al 3Q-MAS NMR shows two peaks for environmentally different tetrahedral aluminium atoms. This is the first time we are showing such a fact which is not observable using ordinary MAS NMR

  8. Angiotensin-(1-7)/Mas axis integrity is required for the expression of object recognition memory.

    Science.gov (United States)

    Lazaroni, Thiago L N; Raslan, Ana Cláudia S; Fontes, Walkiria R P; de Oliveira, Marilene L; Bader, Michael; Alenina, Natalia; Moraes, Márcio F D; Dos Santos, Robson A; Pereira, Grace S

    2012-01-01

    It has been shown that the brain has its own intrinsic renin-angiotensin system (RAS) and angiotensin-(1-7) (Ang-(1-7)) is particularly interesting, because it appears to counterbalance most of the Ang II effects. Ang-(1-7) exerts its biological function through activation of the G-protein-coupled receptor Mas. Interestingly, hippocampus is one of the regions with higher expression of Mas. However, the role of Ang-(1-7)/Mas axis in hippocampus-dependent memories is still poorly understood. Here we demonstrated that Mas ablation, as well as the blockade of Mas in the CA1-hippocampus, impaired object recognition memory (ORM). We also demonstrated that the blockade of Ang II receptors AT1, but not AT2, recovers ORM impairment of Mas-deficient mice. Considering that high concentrations of Ang-(1-7) may activate AT1 receptors, nonspecifically, we evaluate the levels of Ang-(1-7) and its main precursors Ang I and Ang II in the hippocampus of Mas-deficient mice. The Ang I and Ang II levels are unaltered in the whole hipocampus of MasKo. However, Ang-(1-7) concentration is increased in the whole hippocampus of MasKo mice, as well as in the CA1 area. Taken together, our findings suggest that the functionality of the Ang-(1-7)/Mas axis is essential for normal ORM processing. Copyright © 2011 Elsevier Inc. All rights reserved.

  9. NMR study of the molecular nanomagnet [Fe8(N3C6H15)6O2(OH)12]·[Br8·9H2O] in the high-spin magnetic ground state

    International Nuclear Information System (INIS)

    Furukawa, Y.; Kumagai, K.; Lascialfari, A.; Aldrovandi, S.; Borsa, F.; Sessoli, R.; Gatteschi, D.

    2001-01-01

    The magnetic molecular cluster [Fe 8 (N 3 C 6 H 15 ) 6 O 2 (OH) 12 ] 8+ [Br 8 ·9H 2 O] 8- , in short Fe8, has been investigated at low temperature by 1 H-NMR and relaxation measurements. Some measurements of 2 D-NMR in partially deuterated Fe8 clusters will also be reported. Upon decreasing temperature the NMR spectra display a very broad and structured signal which is the result of the internal local fields at the proton sites due to the local moments of the Fe(III) ions in the total S=10 magnetic ground state. The proton and deuteron NMR spectra have been analyzed and the different resonance peaks have been attributed to the different proton groups in the molecule. The simulation of the spectra by using a dipolar hyperfine field and the accepted model for the orientation of the Fe(III) local moments do not agree with the experiments even when the magnitude of the local Fe(III) moments is allowed to vary. It is concluded that a positive contact hyperfine interaction of the same order of magnitude as the dipolar interaction is present for all proton sites except the water molecules. The temperature and magnetic field dependence of the nuclear spin-lattice relaxation rate is ascribed to the fluctuations of the local Fe(III) moments, which follow rigidly the fluctuations of the total ground state magnetization of the nanomagnet. By using a simple model already utilized for the Mn12 cluster, we derive the value of the spin phonon coupling constant which determines the lifetime broadening of the different magnetic quantum number m substates of the S=10 ground state. It is shown that the lifetime broadening decreases rapidly on lowering the temperature. When the lifetime becomes longer than the reciprocal of the frequency shift of the proton lines a structure emerges in the NMR spectrum reflecting the ''frozen'' local moment configuration

  10. Structural Characterization of MAO and Related Aluminum Complexes. 1. Solid-State 27 Al NMR with Comparison to EFG Tensors from ab Initio Molecular Orbital Calculations

    Energy Technology Data Exchange (ETDEWEB)

    Bryant, Pamela L.; Harwell, Chris; Mrse, Anthony A.; Emery, Earl F.; Gan, Zhedong; Caldwell, Tod; Reyes, Arneil P.; Kuhns, Philip; Hoyt, David W.; Simeral, Larry S.; Hall, Randall W.; Butler, Leslie G.

    2001-11-07

    Aminato and propanolato aluminum clusters with 3-, 4-, and 6-coordinate aluminum sites are studied with three 27Al NMR techniques optimized for large 27Al Quadrupole coupling constants: field-swept, frequency-stepped, and high-field MAS NMR. The 27Al quadrupole coupling constants and asymmetry parameters of molecular species, both experimental and derived from ab initio molecular orbital calculations, are correlated with structure.

  11. NMR, water and plants

    International Nuclear Information System (INIS)

    As, H. van.

    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 other body fluids in human and animals. The method is based on a pulse sequence of equidistant π pulses in combination with a linear magnetic field gradient. (Auth.)

  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. Magnetic structure and spin dynamics of the ground state of the molecular cluster Mn12O12 acetate studied by 55Mn NMR

    International Nuclear Information System (INIS)

    Furukawa, Y.; Watanabe, K.; Kumagai, K.; Borsa, F.; Gatteschi, D.

    2001-01-01

    55 Mn nuclear magnetic resonance (NMR) measurements have been carried out in an oriented powder sample of Mn12 acetate at low temperature (1.4--3 K) in order to investigate locally the static and dynamic magnetic properties of the molecule in its high-spin S=10 ground state. We report the observation of three 55 MnNMR lines under zero external magnetic field. From the resonance frequency and the width of the lines we derive the internal hyperfine field and the quadrupole coupling constant at each of the three nonequivalent Mn ion sites. From the field dependence of the spectrum we obtain a direct confirmation of the standard picture, in which spin moments of Mn 4+ ions (S=3/2) of the inner tetrahedron are polarized antiparallel to that of Mn 3+ ions (S=2) of the outer ring with no measurable canting from the easy axis up to an applied field of 6 T. It is found that the splitting of the 55 Mn-NMR lines when a magnetic field is applied at low temperature allows one to monitor the off-equilibrium population of the molecules in the different low lying magnetic states. The measured nuclear spin-lattice relaxation time T 1 strongly depends on temperature and magnetic field. The behavior could be fitted well by considering the local-field fluctuations at the nuclear 55 Mn site due to the thermal reorientation of the total S=10 spin of the molecule. From the fit of the data one can derive the product of the spin-phonon coupling constant times the mean-square value of the fluctuating hyperfine field. The two constants could be estimated separately by making some assumptions. The comparison of the mean-square fluctuation from relaxation with the static hyperfine field from the spectrum suggests that nonuniform terms (q≠0) are important in describing the spin dynamics of the local Mn moments in the ground state

  14. NMR and NQR study of the electronic and structural properties of Al-Cu-Fe and Al-Cu-Ru quasicrystals

    International Nuclear Information System (INIS)

    Shastri, A.; Borsa, F.; Torgeson, D.R.; Shield, J.E.; Goldman, A.I.

    1994-01-01

    27 Al and 63,65 Cu NMR is reported for powdered stable Al-Cu-Fe and Al-Cu-Ru icosahedral quasicrystals and crystalline approximants, and for an Al-Pd-Mn single-grain quasicrystal. 27 Al NQR spectra at 4.2 K were observed in Al-Cu-Fe and Al-Cu-Ru samples. From quadrupole-perturbed NMR spectra at different magnetic fields, and from zero-field NQR spectra, a wide distribution of local electric-field gradient (EFG) tensor components and principal-axis-system orientations was found at the Al site. A model EFG calculation based on a 1/1 Al-Cu-Fe approximant successfully explained the observed NQR spectra. The average local gradient is largely determined by the p-electron wave function at the Al site, while the width of the distribution is due to EFG lattice contribution. Comparison of 63 Cu and 27 Al NMR shows the EFG distribution at the two sites is similar, but the electronic contribution to the EFG is considerably smaller at the Cu site, in agreement with a more s-type wave function of the conduction electrons. Overall spread of EFG values is well reproduced by calculation based on the approximant. However, the experimental spectra indicate a much larger number of nonequivalent sites when compared with the simulated NQR spectra based on the 1/1 approximant. The short-range, local chemical order is well represented by the approximant, but differences in coordination must be included at intermediate range in the quasicrystal. Measured 27 Al Knight shift, magnetic susceptibility, and nuclear spin-lattice relaxation time as a function of temperature indicate reduced density of states at the Fermi level by a factor of 7 or 8 from the value in Al metal, consistent with the notion of a pseudogap for these quasicrystals. No differences in measured parameters were detected as a function of composition of the quasicrystalline alloys

  15. The microscopic NMR probe in chiral magnets. Zero field-, field-modulated- and Skyrmion- states in FeGe and MnSi

    Energy Technology Data Exchange (ETDEWEB)

    Baenitz, Michael; Yasuoka, Hiroshi; Majumder, Mayukh; Khuntia, Panchanan; Schmidt, Marcus [MPI for the Chemical Physics of Solids, Dresden (Germany); Witt, Sebastian; Krellner, Cornelius [Goethe University, Frankfurt am Main (Germany)

    2016-07-01

    Cubic FeGe is a prototype B20 chiral magnet (T{sub c} = 280 K) which allows to study chiral correlations directly ''on-site'' via the{sup 57}Fe nucleus because of its S=1/2 nuclear spin interacting only with the electron spin moment. NMR provides the static and dynamic staggered local magnetization M{sub Q} through the hyperfine field (H{sub hf}) and the spin lattice relaxation rate (SLRR = 1/T{sub 1}). Measurements were performed on randomly oriented {sup 57}Fe enriched FeGe single crystals between 2-300 K. Helical-, conical- and field-polarized-states could be clearly identified and spin dynamics of each phase was investigated. MnSi single crystals and {sup 29}Si enriched MnSi polycrystals were studied by {sup 29}Si-NMR (S=1/2) in the ordered state (T{sub c} = 29 K) and above. The T- and H- dependence of H{sub hf} and SLRR was investigated in great detail for both FeGe and MnSi.The {sup 29}Si-NMR lines in MnSi are narrow and H{sub hf}-values obtained are smaller than in FeGe. Our results are in general accordance with the extended SCR theory for itinerant helical magnets, although the theory does not include the symmetry breaking in the B20 structure and the multi-band nature. For FeGe correlations are complex due to its more localized magnetism.

  16. Distributed Cooperation Solution Method of Complex System Based on MAS

    Science.gov (United States)

    Weijin, Jiang; Yuhui, Xu

    To adapt the model in reconfiguring fault diagnosing to dynamic environment and the needs of solving the tasks of complex system fully, the paper introduced multi-Agent and related technology to the complicated fault diagnosis, an integrated intelligent control system is studied in this paper. Based on the thought of the structure of diagnostic decision and hierarchy in modeling, based on multi-layer decomposition strategy of diagnosis task, a multi-agent synchronous diagnosis federation integrated different knowledge expression modes and inference mechanisms are presented, the functions of management agent, diagnosis agent and decision agent are analyzed, the organization and evolution of agents in the system are proposed, and the corresponding conflict resolution algorithm in given, Layered structure of abstract agent with public attributes is build. System architecture is realized based on MAS distributed layered blackboard. The real world application shows that the proposed control structure successfully solves the fault diagnose problem of the complex plant, and the special advantage in the distributed domain.

  17. 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.

  18. PEMANFAATAN TANAMAN ATRAKTAN MENGENDALIKAN HAMA KEONG MAS PADI

    Directory of Open Access Journals (Sweden)

    Ameilia Zuliyanti Siregar

    2018-01-01

    In Indonesia, many plantation as use as beneficial plants. This study aims to obtain an effective formula that can be used as a biopesticide to control snail pests during the vegetative phase from May to July 2017 using random non-factorial methods at two rice planting locations in the Village Lae parira, Dairi, North Sumatra. Design with 6 treatments and 3 replicates (ie control, neem leaves (Azadirachta indica, tobacco leaf (Nicotiana tabacum, sweet potato leaf (Manihot glaziovii, noni fruit, Morinda citrifolia, and betel nut (Areca catechu and papaya (Carica papaya as an eco-friendly herbaceous and biopesticide. Based on the study recorded in sampling for 7 days with 6 treatments had significant effect on the percentage affected by the clump of rice attacked and the percentage of death. Pearson correlation value recorded percentage of death and percentage of impacted  showed a very significant relationship. Neem is the best biopesticide in controlling mollusicides, followed by betel nuts, tobacco, poisonous yams and noni. Death of 100% snail mas will prevent damage to the clump of rice plants Dairi, North Sumatra. All biopesticide treatments were tested to control snail pests in rice plants that will increase agicultural productivity in maintaining food security in Dairi, North Sumatra.

  19. Magic Angle Spinning NMR Metabolomics

    Energy Technology Data Exchange (ETDEWEB)

    Zhi Hu, Jian

    2016-01-01

    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.

  20. NMR in clinical practice

    International Nuclear Information System (INIS)

    Smith, F.W.

    1987-01-01

    The development of NMR for clinical use has been complicated by a number of controversies, the largest of these being the question of what is the optimum field strength for proton imaging. Many workers believe that diagnostically useful images can only be produced at high field strength (i.e. 0.5 - 2.0 T), where in fact diagnostically useful images are made using field strengths of as low as 0.02 T. Because the method is more complex than X-ray CT, which relies on the measurement of only one parameter, tissue density, many new users have difficulty in selecting the correct imaging pulse sequence to provide the most useful image for diagnosis. NMR imaging pulse sequence may be selected to produce images of the proton density, T/sub 1/ or T/sub 2/ signals, or combinations of them. When this facility is used, images which are T/sub 1/ or T/sub 2/ weighted can be selected. Inversion-recovery sequences are more appropriate for imaging the abdomen where by selecting a short TR interval the signal from subcutaneous fat, which is the major cause of image artefact in abdominal imaging, is suppressed thereby improving image quality. The use of surface receiver coils, which are applied closely to the area of the body being examined is becoming more widespread and is of particular value when examining the orbits, facial structures, neck, breast, spine and limbs. The use of these coils together with a discussion of patient selection for NMR imaging, image interpretation and data storage follow

  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. Copyright © 2015 John Wiley & Sons, Ltd.

  2. Electronic correlations in the hole-doped superconductor RbFe{sub 2}As{sub 2} probed via {sup 75}As NMR

    Energy Technology Data Exchange (ETDEWEB)

    Molatta, S.; Wosnitza, J. [Hochfeld-Magnetlabor Dresden (HLD), Helmholtz-Zentrum Dresden-Rossendorf (Germany); TU Dresden (Germany); DFG, GRK-1621 (Germany); Zhang, Z.; Dmytriieva, D.; Kuehne, H. [Hochfeld-Magnetlabor Dresden (HLD), Helmholtz-Zentrum Dresden-Rossendorf (Germany); Khim, S.; Grafe, H.J. [IFW Dresden (Germany); Wurmehl, S.; Buechner, B. [TU Dresden (Germany); DFG, GRK-1621 (Germany); IFW Dresden (Germany)

    2016-07-01

    We will present latest {sup 75}As NMR data in the normal state of the stoichiometric superconductor RbFe{sub 2}As{sub 2}. This will be put into context to known results for the heavily hole-doped compound KFe{sub 2}As{sub 2}. The static and dynamic magnetic correlations were probed via measurements of the Knight shift and nuclear spin-lattice relaxation rate in a wide temperature range from 0.3 to 300 K. Although neither a magnetic nor a structural transition were observed down to lowest temperatures, the very close proximity of the ground state to a magnetic instability is indicated by a pronounced Curie-Weiss-like behavior of spin fluctuations. At around 100 K, we find a maximum of the Knight shift and a changing exponent of the temperature-dependent relaxation rate. This is phenomenologically similar to the case of KFe{sub 2}As{sub 2} and was proposed to stem from a incoherence-coherence crossover mechanism of electronic correlations.

  3. Glycosphingolipids: 2H NMR study of the influence of carbohydrate headgroup structure on ceramide acyl chain behavior in glycolipid-phospholipid bilayers

    International Nuclear Information System (INIS)

    Fenske, D.B.; Jarrell, H.C.; Hamilton, K.; Florio, E.; Barber, K.R.; Grant, C.W.M.

    1991-01-01

    Galactosyl- and glucosylceramide, globoside, and dihydrolactosylceramide, bearing [2,2- 2 H 2 ]stearic acid, have been studied at a concentration of 10 mol % in bilayers of dimyristoylphosphatidylcholine by 2 H NMR. The quadrupolar splittings Δv Q of the C2 deuterons were measured at several temperatures in the range of 30-60 degree C. Spin-lattice relaxation times T 1 of C2 deuterons were determined in the same temperature range for all lipids but globoside. T 1 values for the GlcCer and GalCer systems increased with temperature, indicating that the motions responsible for relaxation were in the short correlation time regime. T 1 for deuterons at the acyl chain C2-position of LaCer was observed to decrease with increasing temperature, indicating that the motion(s) dominating relaxation are in the long correlation time regime. Thus the mobility of the acyl chain at the 2-position is reduced in the LacCer with respect to GlcCer and GalCer

  4. Glycosphingolipids: sup 2 H NMR study of the influence of carbohydrate headgroup structure on ceramide acyl chain behavior in glycolipid-phospholipid bilayers

    Energy Technology Data Exchange (ETDEWEB)

    Fenske, D.B.; Jarrell, H.C. (National Research Council of Canada, Ottawa, Ontario (Canada)); Hamilton, K.; Florio, E.; Barber, K.R.; Grant, C.W.M. (Univ. of Western Ontario, London (Canada))

    1991-05-07

    Galactosyl- and glucosylceramide, globoside, and dihydrolactosylceramide, bearing (2,2-{sup 2}H{sub 2})stearic acid, have been studied at a concentration of 10 mol % in bilayers of dimyristoylphosphatidylcholine by {sup 2}H NMR. The quadrupolar splittings {Delta}v{sub Q} of the C2 deuterons were measured at several temperatures in the range of 30-60{degree}C. Spin-lattice relaxation times T{sub 1} of C2 deuterons were determined in the same temperature range for all lipids but globoside. T{sub 1} values for the GlcCer and GalCer systems increased with temperature, indicating that the motions responsible for relaxation were in the short correlation time regime. T{sub 1} for deuterons at the acyl chain C2-position of LaCer was observed to decrease with increasing temperature, indicating that the motion(s) dominating relaxation are in the long correlation time regime. Thus the mobility of the acyl chain at the 2-position is reduced in the LacCer with respect to GlcCer and GalCer.

  5. NMR investigation of charge fluctuations in the charge-density-wave (CDW) system Rb_0.3MoO_3

    Science.gov (United States)

    Tanaka, K. B.; Vonlanthen, P.; Clark, W. G.; Kriza, G.; Moulton, W. G.; Kuhns, P.; Reyes, A. P.

    2001-03-01

    We report measurements of the spin-lattice relaxation rate (T_1-1), the spin-spin relaxation rate (T_2-1), and NMR spectra of ^85Rb and ^87Rb in Rb_0.3MoO3 for the temperature (T) range 5-300 K at 9 T and 23 T. The ratio of T_1-1 for ^85Rb and ^87Rb shows that for all T, the dominant coupling for T_1-1 is quadrupolar; i.e., it is driven by charge fluctuations. Prior work assumed that in the metallic phase above 182 K, the relaxation was via magnetic coupling to conduction electrons. Another surprising result is the absence of a strong variation of T_1-1 across the CDW-broadened spectrum. Such a variation is expected for relaxation by thermal CDW phason fluctuations. Our high field measurements also show very little frequency dependence for T_1-1. The observed T-variation of T_1-1 displays five different regimes, which will be presented and discussed. The UCLA part of the work was supported by NSF Grants DMR-9705369 and DMR-0072524.

  6. Magnetic excitation and local magnetic susceptibility of the excitonic insulator Ta2NiSe5 investigated by 77Se NMR

    Science.gov (United States)

    Li, Shang; Kawai, Shunsuke; Kobayashi, Yoshiaki; Itoh, Masayuki

    2018-04-01

    77Se NMR measurements were made on polycrystalline and single-crystalline samples to elucidate local magnetic susceptibility and magnetic excitation of Ta2NiSe5 , which is proposed to undergo an exciton condensation accompanied by a structural transition at Tc=328 K . We determine the 77Se Knight shift tensors for the three Se sites and analyze their anisotropy based on the site symmetry. The temperature dependence of the Knight shift is discussed on the basis of spin and orbital susceptibilities calculated for two-chain and two-dimensional three-band models. The large fraction of the Se 4 p orbital polarization due to the mixing between Ni 3 d and Se 4 p orbitals is estimated from the analysis of the transferred hyperfine coupling constant. Also the nuclear spin-lattice relaxation rate 1 /T1 is found not to show a coherent peak just below Tc and to obey the thermally activated temperature dependence with a spin gap energy of 1770 ±40 K . This behavior of 1 /T1 monitors the exciton condensation as proposed by the theoretical study of 1 /T1 based on the three-chain Hubbard model for the excitonic insulator.

  7. Ferromagnetic quantum critical fluctuations and anomalous coexistence of ferromagnetism and superconductivity in UCoGe revealed by Co-NMR and NQR studies

    International Nuclear Information System (INIS)

    Ohta, Tetsuya; Nakai, Yusuke; Ihara, Yoshihiko; Ishida, Kenji; Deguchi, Kazuhiko; Sato, Noriaki K.; Satoh, Isamu

    2008-01-01

    Co nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) studies were carried out for the recently discovered UCoGe, in which the ferromagnetic and superconducting (SC) transitions are reported to occur at T Curie - 3 K and T S - 0.8 K, in order to investigate the coexistence of ferromagnetism and superconductivity as well as the normal-state and SC properties from a microscopic point of view. From the nuclear spin-lattice relaxation rate 1/T 1 and Knight-shift measurements, we confirm that ferromagnetic fluctuations that possess a quantum critical character are present above T Curie and also the occurrence of a ferromagnetic transition at 2.5 K in our polycrystalline sample. The magnetic fluctuations in the normal state show that UCoGe is an itinerant ferromagnet similar to ZrZn 2 and YCo 2 . The onset SC transition is identified at T S - 0.7 K, below which 1/T 1 arising from 30% of the volume fraction starts to decrease due to the opening of the SC gap. This component of 1/T 1 , which follows a T 3 dependence in the temperature range 0.3-0.1 K, coexists with the magnetic components of 1/T 1 showing a √T dependence below T S . From the NQR measurements in the SC state, we suggest that the self-induced vortex state is realized in UCoGe. (author)

  8. Spin lattice coupling in multiferroic hexagonal YMnO3

    Indian Academy of Sciences (India)

    phonon and spin waves involving deviations out of the spiral magnetic plane. This ... collimations were used to fully benefit from the focusing effects. ... following spin Hamiltonian based on the Heisenberg model H = JSiSj − hSini +. DSz i Sz.

  9. Spin-lattice effects in selected antiferromagnetic materials

    Czech Academy of Sciences Publication Activity Database

    Zherlitsyn, S.; Yasin, S.; Wosnitza, J.; Zvyagin, A.A.; Andreev, Alexander V.; Tsurkan, V.

    2014-01-01

    Roč. 40, č. 2 (2014), s. 123-133 ISSN 1063-777X R&D Projects: GA ČR GAP204/12/0150 Grant - others:AVČR(CZ) M100101203 Keywords : low-dimensional spin systems * frustrated chromium spinels * spin-strain interaction * uranium -based compounds Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.786, year: 2014

  10. Spin-orbit and spin-lattice coupling

    International Nuclear Information System (INIS)

    Bauer, Gerrit E.W.; Ziman, Timothy; Mori, Michiyasu

    2014-01-01

    We pursued theoretical research on the coupling of electron spins in the condensed matter to the lattice as mediated by the spin-orbit interaction with special focus on the spin and anomalous Hall effects. (author)

  11. The realization of Majorana fermions in Kitaev Quantum Spin Lattice

    Science.gov (United States)

    Do, Seung-Hwan; Park, Sang-Youn; Yoshitake, Junki; Nasu, Joji; Motome, Yukitoshi; Kwon, Y. S.; Adroja, D. T.; Voneshen, D.; Park, J.-H.; Choi, Kwang-Yong; Ji, Sungdae

    The Kitaev honeycomb lattice is envisioned as an ideal host for Majorana fermions that are created out of the spin liquid background. Combining specific heat and neutron scattering experiments with theoretical calculations, here, we establish a hitherto unparalleled spin fractionalization to two species of Majorana fermions in the Kitaev material α-RuCl3. The specific heat data unveil a two-stage release of magnetic entropy by (R/2)ln2 and the T-linear dependence at intermediate temperatures. Our inelastic neutron scattering measurements further corroborate two distinct characters of fractionalized excitations: an Y-like, dispersive, magnetic continuum at higher energies and a dispersionless excitation at low energies around the Brillouin zone center. These dual features are well described by a Ferromagnetic Kitaev model, providing a smoking gun proof of the itinerant and localized Majorana fermions emergent in Kitaev magnets.

  12. A Hybrid Solid-State NMR and Electron Microscopy Structure-Determination Protocol for Engineering Advanced para-Crystalline Optical Materials

    NARCIS (Netherlands)

    Thomas, Brijith; Rombouts, Jeroen; Oostergetel, Gert T.; Gupta, Karthick B.S.S.; Buda, Francesco; Lammertsma, Koop; Orru, Romano; de Groot, Huub J.M.

    2017-01-01

    Hybrid magic-angle spinning (MAS) NMR spectroscopy and TEM were demonstrated for de novo structure determination of para-crystalline materials with a bioinspired fused naphthalene diimide (NDI)–salphen–phenazine prototype light-harvesting compound. Starting from chiral building blocks with C2

  13. High-resolution magic angle spinning (1)H NMR spectroscopy of metabolic changes in rabbit lens after treatment with dexamethasone combined with UVB exposure

    Czech Academy of Sciences Publication Activity Database

    Seather, O.; Risa, O.; Čejková, Jitka; Krane, J.; Midelfart, A.

    2004-01-01

    Roč. 242, - (2004), s. 1000-1007 ISSN 0721-832X R&D Projects: GA ČR GA304/03/0419 Institutional research plan: CEZ:AV0Z5008914 Keywords : HR-MAS 1H NMR Subject RIV: FF - HEENT, Dentistry Impact factor: 1.513, year: 2004

  14. Chemical structure changes in coals after low-temperature oxidation and demineralization by acid treatment as revealed by high resolution solid state 13C NMR

    International Nuclear Information System (INIS)

    Tekely, P.; Nicole, D.; Delpuech, J.-J.; Totino, E.; Muller, J.F.

    1987-01-01

    13 C CP/MAS NMR has been used for characterization of chemical structure changes in coals after low-temperature oxidation and prolonged demineralization by acid treatment. In both cases the changes take place mainly in the aliphatic part of coal molecules. 21 refs.; 3 figs.; 2 tabs

  15. Evaluation of thermoplastic starch/MMT nanocomposites by nuclear magnetic resonance (NMR)

    International Nuclear Information System (INIS)

    Schlemmer, D.; Rodrigues, Tiago C.A.F.; Resck, I.S.; Sales, M.J.A.

    2010-01-01

    Starch has been studied for replace petrochemical plastics for short shelf life. However, the starch films have limitations: sensitivity to moisture and poor mechanical strength. This can be improved by incorporating loads such as montmorillonite, forming nanocomposites. Nanocomposites were prepared with 1, 3, 5 and 10% of montmorillonite, using vegetable oils of Brazilian Cerrado as plasticizers. The NMR spectra of oils are similar, but the intensities of the signals varying with the proportion of fatty acids. The molar mass of the oils was also calculated by NMR. The spectrum of CP/MAS 13 C NMR for starch presented a duplet in 97 and 98 ppm, on the amorphous domains of C-1, indicating a crystal type A. The spectra of the nanocomposites are similar to those of starch and oils. No new peaks appear, suggesting that there are no strong chemical bonds between components. (author)

  16. E/Z MAS: An easy-to-use computerized materials control and accountability system

    International Nuclear Information System (INIS)

    Anderson, L.K.; Boor, M.G.; Hurford, J.M.; Landry, R.P.; Martinez, B.J.; Solem, A.M.; Whiteson, R.; Zardecki, A.

    1998-01-01

    Nuclear facilities that handle and process nuclear materials are required to track their nuclear holdings and to keep adequate records that manage and control the inventory of those holdings. The complexity of a system that does this job is directly proportional to the complexity of the facility's operations. This paper describes an approach to computerized materials protection, control, and accountability (MPC and A) that was introduced by Los Alamos National Laboratory (LANL) in the fall of 1997. This new system, E/Z MAS, is the latest addition to the LANL suite of computerized MPC and A tools, which also includes the CoreMAS system. E/Z MAS was initially designed to address the needs of those facilities that have small to modest MPC and A needs but has been expanded to provide full functionality for any facility. The system name, E/Z MAS, reflects the system's easy-to-use characteristics, which include ease of installation and ease of software maintenance. Both CoreMAS and E/Z MAS have been provided to facilities in the Former Soviet Union to assist them in implementing a computerized MPC and A system that meets their needs. In this paper the authors will address the functionality of CoreMAS and E/Z MAS, and an argument in favor of intranet-based material control and accountability will be advanced

  17. Evidence for Heterodimerization and Functional Interaction of the Angiotensin Type 2 Receptor and the Receptor MAS

    DEFF Research Database (Denmark)

    Leonhardt, Julia; Villela, Daniel C.; Teichmann, Anke

    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 in...

  18. Characterization of Two Distinct Amorphous Forms of Valsartan by Solid-State NMR.

    Science.gov (United States)

    Skotnicki, Marcin; Apperley, David C; Aguilar, Juan A; Milanowski, Bartłomiej; Pyda, Marek; Hodgkinson, Paul

    2016-01-04

    Valsartan (VAL) is an antihypertensive drug marketed in an amorphous form. Amorphous materials can have different physicochemical properties depending on preparation method, thermal history, etc., but the nature of such materials is difficult to study by diffraction techniques. This study characterizes two different amorphous forms of valsartan (AR and AM) using solid-state NMR (SSNMR) as a primary investigation tool, supported by solution-state NMR, FT-IR, TMDSC, and dissolution tests. The two forms are found to be clearly distinct, with a significantly higher level of structural arrangement in the AR form, as observed in (13)C, (15)N, and (1)H SSNMR. (13)C and (15)N NMR indicates that the fully amorphous material (AM) contains an approximately equal ratio of cis-trans conformers about the amide bond, whereas the AR form exists mainly as one conformer, with minor conformational "defects". (1)H ultrafast MAS NMR shows significant differences in the hydrogen bonding involving the tetrazole and acid hydrogens between the two materials, while (15)N NMR shows that both forms exist as a 1,2,3,4-tetrazole tautomer. NMR relaxation times show subtle differences in local and bulk molecular mobility, which can be connected with the glass transition, the stability of the glassy material, and its response to aging. Counterintuitively the fully amorphous material is found to have a significantly lower dissolution rate than the apparently more ordered AR material.

  19. Application of NMR Spectroscopy in the Analysis of Petroleum Derivatives and Products

    Directory of Open Access Journals (Sweden)

    Parlov Vuković, J.

    2012-11-01

    Full Text Available Complex chemical composition and physical properties of oil and fuel make their complete cha racterization very difficult. Components present in oil and oil products differ in structure, size, po larity and functionality. The presence and structure of specific hydrocarbons in final products depend on the processing procedure and type of the fuel. In order to predict or improve fuel pro perties it is necessary to determine its composition. Thus, new and more sophisticated analytical methods and procedures are constantly being developed. NMR spectroscopy plays a significant role in analysis and identification of complex hydrocarbon mixtures of petroleum and petroleum products. In this review, we describe the application of NMR spectroscopy for analyzing gasoline and diesel fuels. Hence, by using NMR spectroscopy it is possible to determine gasoline composition and presence of benzene and oxygenates, as well as some important physical characteristics of gasoli ne such as the research octane number. An application of different NMR techniques made it pos sible to characterize diesel fuels and middle oil distillates from various refineries. Data so obtained can be used in combination with statistical methods to predict fuel properties and to monitor pro- duction processes in the petroleum industry. NMR spectroscopy has proven useful in analysis of FAME which has recently been used as an ecologically acceptable alternative fuel. Furthermore, techniques such as CP/MAS for characterization of solid state oil-geochemical samples are inclu- ded. Also, possibilities of using NMR spectroscopy in the analysis of polymeric additives are di- scussed.

  20. Structural analysis of alanine tripeptide with antiparallel and parallel beta-sheet structures in relation to the analysis of mixed beta-sheet structures in Samia cynthia ricini silk protein fiber using solid-state NMR spectroscopy.

    Science.gov (United States)

    Asakura, Tetsuo; Okonogi, Michi; Nakazawa, Yasumoto; Yamauchi, Kazuo

    2006-05-10

    The structural analysis of natural protein fibers with mixed parallel and antiparallel beta-sheet structures by solid-state NMR is reported. To obtain NMR parameters that can characterize these beta-sheet structures, (13)C solid-state NMR experiments were performed on two alanine tripeptide samples: one with 100% parallel beta-sheet structure and the other with 100% antiparallel beta-sheet structure. All (13)C resonances of the tripeptides could be assigned by a comparison of the methyl (13)C resonances of Ala(3) with different [3-(13)C]Ala labeling schemes and also by a series of RFDR (radio frequency driven recoupling) spectra observed by changing mixing times. Two (13)C resonances observed for each Ala residue could be assigned to two nonequivalent molecules per unit cell. Differences in the (13)C chemical shifts and (13)C spin-lattice relaxation times (T(1)) were observed between the two beta-sheet structures. Especially, about 3 times longer T(1) values were obtained for parallel beta-sheet structure as compared to those of antiparallel beta-sheet structure, which could be explicable by the difference in the hydrogen-bond networks of both structures. This very large difference in T(1) becomes a good measure to differentiate between parallel or antiparallel beta-sheet structures. These differences in the NMR parameters found for the tripeptides may be applied to assign the parallel and antiparallel beta-sheet (13)C resonances in the asymmetric and broad methyl spectra of [3-(13)C]Ala silk protein fiber of a wild silkworm, Samia cynthia ricini.

  1. Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Mingxue

    2013-02-26

    Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T{sub 1}) and rotating frame (T{sub 1{rho}}) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of {sup 1}H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T{sub 1} and T{sub 1{rho}} relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T{sub 1{rho}} in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

  2. Investigation of a polymer-dispersed liquid crystal system by NMR diffusometry and relaxometry

    International Nuclear Information System (INIS)

    Tang, Mingxue

    2013-01-01

    Polymer-dispersed liquid crystals (PDLCs) are polymer composites containing a dispersion of liquid crystal droplets in polymer networks. PDLCs have attracted much attention due to their unique properties and potential usage. The properties of PDLCs depend on the degree of phase separation and the size of liquid crystal droplets. To investigate the structure will help us to better understand and optimize PDLCs.The main aim of this PhD thesis was to investigate PDLCs by NMR techniques. Diffusion constants and spin-lattice relaxation times in the laboratory (T 1 ) and rotating frame (T 1ρ ) were measured for PDLCs as well as precursor mixtures based on the trifunctional monomer trimethylolpropane triacrylate (TMPTA) and the commercial nematic mixture E7. The variation of the main dipolar splitting of 1 H spectra with increasing temperature was analyzed to obtain the nematic-to-isotropic phase transition temperature and the nematic order parameter of E7 and, for comparison, the nematic liquid crystal 5CB.Diffusion constants in TMPTA/E7 mixtures, measured by pulsed-field gradient NMR, increase for both E7 and TMPTA as the mass fraction of E7 increases, due to the lower viscosity of E7. E7 in the PDLC diffuses more slowly than in the bulk because of the hindrance by the polymer matrix. T 1 and T 1ρ relaxation times in the liquid or liquid-crystalline phases of TMPTA and bulk E7 are higher than in the PDLC and the pure polymer, due to the lower mobility in the polymer samples. T 1ρ in the PDLC is even shorter than in the pure polymer, indicating an anti-softening effect caused by E7 molecules. In bulk E7, the well-ordered rod-like molecules exhibit a unique H-C dipolar coupling, which leads to oscillations in the cross-polarization curve. However, in the PDLC, the anchoring effect at the boundary between the polymer and LC droplets disturbs the molecular order resulting in a smooth cross polarization curve.

  3. 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.

  4. NMR spectroscopy and drug development

    International Nuclear Information System (INIS)

    Craik, D.; Munro, S.

    1990-01-01

    The use of nuclear magnetic resonance (NMR) spectroscopy for structural and conformational studies on drug molecules, the three-dimensional investigation of proteins structure and their interactions with ligands are discussed. In-vivo NMR studies of the effects of drugs on metabolism in perfused organs and whole animals are also briefly presented. 5 refs., ills

  5. NMR in pulsed magnetic field

    KAUST Repository

    Abou-Hamad, Edy; Bontemps, P.; Rikken, Geert L J A

    2011-01-01

    Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

  6. NMR imaging of osteoarticular pathology

    International Nuclear Information System (INIS)

    Frocrain, L.; Duvauferrier, R.; Gagey, N.

    1987-01-01

    NMR imaging is assuming an increasingly important role in the diagnosis of osteo-articular disorders. Semiological descriptions of the mean pathological disorders of the locomotor system are presented. Some investigation strategies are proposed to compare NMR imaging with other imaging techniques in various pathological states [fr

  7. Nuclear magnetic resonance (NMR) tomography

    International Nuclear Information System (INIS)

    Skalpe, I.O.

    1984-01-01

    A brief survey of the working principle of the NMR technique in diagnostical medicine is given. Its clinical usefulness for locating tumors, diagnosing various other diseases, such as some mental illnesses and multiple sclerosis, and its possibilities for studying biochemical processes in vivo are mentioned. The price of NMR image scanners and the problems of the strong magnetic field around the machines are mentioned

  8. NMR imaging studies of coal

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Z.R.; Zhang, P.Z.; Ding, G.L.; Li, L.Y.; Ye, C.H. [University of Science and Technology, Beijing (China). Dept. of Chemistry

    1996-06-01

    The permeation transportation and swelling behavior of solvents into coal are investigated by NMR imaging using pyridine-d{sub 5} and acetone-d{sub 6}. Images of coal swollen with deuterated solvents illuminate proton distributions of mobile phases within the coal macromolecular networks. More information about the chemical and physical structure of coal can be obtained using NMR imaging techniques.

  9. NMR in pulsed magnetic field

    KAUST Repository

    Abou-Hamad, Edy

    2011-09-01

    Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

  10. Structural Biology: Practical NMR Applications

    CERN Document Server

    Teng, Quincy

    2005-01-01

    This textbook begins with an overview of NMR development and applications in biological systems. It describes recent developments in instrument hardware and methodology. Chapters highlight the scope and limitation of NMR methods. While detailed math and quantum mechanics dealing with NMR theory have been addressed in several well-known NMR volumes, chapter two of this volume illustrates the fundamental principles and concepts of NMR spectroscopy in a more descriptive manner. Topics such as instrument setup, data acquisition, and data processing using a variety of offline software are discussed. Chapters further discuss several routine stategies for preparing samples, especially for macromolecules and complexes. The target market for such a volume includes researchers in the field of biochemistry, chemistry, structural biology and biophysics.

  11. Fundamentals of Protein NMR Spectroscopy

    CERN Document Server

    Rule, Gordon S

    2006-01-01

    NMR spectroscopy has proven to be a powerful technique to study the structure and dynamics of biological macromolecules. Fundamentals of Protein NMR Spectroscopy is a comprehensive textbook that guides the reader from a basic understanding of the phenomenological properties of magnetic resonance to the application and interpretation of modern multi-dimensional NMR experiments on 15N/13C-labeled proteins. Beginning with elementary quantum mechanics, a set of practical rules is presented and used to describe many commonly employed multi-dimensional, multi-nuclear NMR pulse sequences. A modular analysis of NMR pulse sequence building blocks also provides a basis for understanding and developing novel pulse programs. This text not only covers topics from chemical shift assignment to protein structure refinement, as well as the analysis of protein dynamics and chemical kinetics, but also provides a practical guide to many aspects of modern spectrometer hardware, sample preparation, experimental set-up, and data pr...

  12. Solid-state 27Al and 29Si NMR characterization of hydrates formed in calcium aluminate-silica fume mixtures

    International Nuclear Information System (INIS)

    Pena, P.; Rivas Mercury, J.M.; Aza, A.H. de; Turrillas, X.; Sobrados, I.; Sanz, J.

    2008-01-01

    Partially deuterated Ca 3 Al 2 (SiO 4 ) y (OH) 12-4y -Al(OH) 3 mixtures, prepared by hydration of Ca 3 Al 2 O 6 (C 3 A), Ca 12 Al 14 O 33 (C 12 A 7 ) and CaAl 2 O 4 (CA) phases in the presence of silica fume, have been characterized by 29 Si and 27 Al magic-angle spinning-nuclear magnetic resonance (MAS-NMR) spectroscopies. NMR spectroscopy was used to characterize anhydrous and fully hydrated samples. In hydrated compounds, Ca 3 Al 2 (OH) 12 and Al(OH) 3 phases were detected. From the quantitative analysis of 27 Al NMR signals, the Al(OH) 3 /Ca 3 Al 2 (OH) 12 ratio was deduced. The incorporation of Si into the katoite structure, Ca 3 Al 2 (SiO 4 ) 3-x (OH) 4x , was followed by 27 Al and 29 Si NMR spectroscopies. Si/OH ratios were determined from the quantitative analysis of 27 Al MAS-NMR components associated with Al(OH) 6 and Al(OSi)(OH) 5 environments. The 29 Si NMR spectroscopy was also used to quantify the unreacted silica and amorphous calcium aluminosilicate hydrates formed, C-S-H and C-A-S-H for short. From 29 Si NMR spectra, the amount of Si incorporated into different phases was estimated. Si and Al concentrations, deduced by NMR, transmission electron microscopy, energy dispersive spectrometry, and Rietveld analysis of both X-ray and neutron data, indicate that only a part of available Si is incorporated in katoite structures. - Graphical abstract: Transmission electron micrograph of CaAl 2 O 4 -microsilica mixture hydrated at 90 deg. C for 31 days showing a cubic Ca 3 Al 2.0±0.2 (SiO 4 ) 0.9±0.2 (OH) 1.8 crystal surrounded by unreacted amorphous silica spheres

  13. 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.

  14. Crystal structure and tautomerism of Pigment Yellow 138 determined by X-ray powder diffraction and solid-state NMR

    DEFF Research Database (Denmark)

    Gumbert, Silke D.; Körbitzer, Meike; Alig, Edith

    2016-01-01

    The crystal structure of C.I. Pigment Yellow 138 was determined from X-ray powder diffraction data using real-space methods with subsequent Rietveld refinements. The tautomeric state was investigated by solid-state 1D and 2D multinuclear NMR experiments. In the crystals, the compound exhibits...... the NH-tautomer with a hydrogen atom situated at the nitrogen of the quinoline moiety. Direct evidence of the presence of the NH-tautomer is provided by 1H–14N HMQC solid-state NMR at very fast MAS. Solid-state dispersion-corrected density functional theory calculations with BLYP-D3 confirm...

  15. 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 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.

  16. Two dimensional solid state NMR

    International Nuclear Information System (INIS)

    Kentgens, A.P.M.

    1987-01-01

    This thesis illustrates, by discussing some existing and newly developed 2D solid state experiments, that two-dimensional NMR of solids is a useful and important extension of NMR techniques. Chapter 1 gives an overview of spin interactions and averaging techniques important in solid state NMR. As 2D NMR is already an established technique in solutions, only the basics of two dimensional NMR are presented in chapter 2, with an emphasis on the aspects important for solid spectra. The following chapters discuss the theoretical background and applications of specific 2D solid state experiments. An application of 2D-J resolved NMR, analogous to J-resolved spectroscopy in solutions, to natural rubber is given in chapter 3. In chapter 4 the anisotropic chemical shift is mapped out against the heteronuclear dipolar interaction to obtain information about the orientation of the shielding tensor in poly-(oxymethylene). Chapter 5 concentrates on the study of super-slow molecular motions in polymers using a variant of the 2D exchange experiment developed by us. Finally chapter 6 discusses a new experiment, 2D nutation NMR, which makes it possible to study the quadrupole interaction of half-integer spins. 230 refs.; 48 figs.; 8 tabs

  17. NMR-CT in muscular disorders. Muscle T/sub 1/ values in Duchenne muscular dystrophy carriers

    Energy Technology Data Exchange (ETDEWEB)

    Matsumura, Kiichiro; Nakano, Imaharu; Fukuda, Nobuo; Ikehira, Hiroo; Tateno, Yukio

    1987-02-01

    Proton NMR-CT (magnetic field strength 0.1 Tesla, resonant frequency 4.5 MHz) was performed in 10 normal females and 19 Duchenne muscular dystrophy (DMD) carriers. The mean age was 39 +- 12 years for the normal females and 42 +- 6 years for the DMD carriers. In DMD carriers, there were 4 definite, 4 probable, and 11 possible carriers. T/sub 1/ (spin-lattice relaxation time) image was obtained for a slice at the buttock, mid-thigh and calf levels respectively. T/sub 1/ values were measured for the medial portion of the gluteus maximus, the vastus lateralis of the quadriceps femoris, and the gastrocnemius. The bound water fraction (BWF) was calculated from Fullerton's equation based on the fast proton diffusion model. The following results were obtained: (1) In normal females, muscle T/sub 1/ value was highest in the gastrocnemius and lowest in the gluteus maximus. (2) In DMD carriers, T/sub 1/ values of the gluteus maximus and quadriceps femoris were significantly higher than those of the normal females. There was, however, no significant difference in T/sub 1/ value of the gastrocnemius between DMD carriers and normal females. (3) In DMD carriers, BWFs of the gluteus maximus and quadriceps femoris were significantly lower than those of the normal females. (4) In DMD carriers, no significant correlation was observed between the muscle T/sub 1/ values and the serum creatine phosphokinase values. Increased tissue water content in the lower parts of the body due to gravity is considered to be the primary cause of the high T/sub 1/ value in the gastrocnemius of normal females. The presence of the degenerating muscle fibers are presumed responsible for the high T/sub 1/ value and low BWF in the proximal muscles of DMD carriers.

  18. NMR-CT in muscular disorders. Muscle T/sub 1/ values in Duchenne muscular dystrophy carriers

    Energy Technology Data Exchange (ETDEWEB)

    Matsumura, Kiichiro; Nakano, Imaharu; Fukuda, Nobuo; Ikehira, Hiroo; Tateno, Yukio

    1987-02-01

    Proton NMR-CT (magnetic field strength 0.1 Tesla, resonant frequency 4.5 MHz) was performed in 10 normal females and 19 Duchenne muscular dystrophy (DMD) carriers. The mean age was 39 +- 12 years for the normal females and 42 +- 6 years for the DMD carriers. In DMD carriers, there were 4 definite, 4 probable, and 11 possible carriers. T/sub 1/ (spin-lattice relaxation time) image was obtained for a slice at the buttock, mid-thigh and calf levels respectively. T/sub 1/ values were measured for the medial portion of the gluteus maximus, the vastus lateralis of the quadriceps femoris, and the gastrocnemius. The bound water fraction (BWF) was calculated from Fullerton's equation based on the fast proton diffusion model. The following results were obtained: (1) In normal females, muscle T/sub 1/ value was highest in the gastrocnemius and lowest in the gluteus maximus. (2) In DMD carriers, T/sub 1/ values of the gluteus maximus and quadriceps femoris were significantly higher than those of the normal females. There was, however, no significant difference in T/sub 1/ value of the gastrocnemius between DMD carriers and normal females. (3) In DMD carriers, BWFs of the gluteus maximus and quadriceps femoris were significantly lower than those of the normal females. (4) In DMD carriers, no significant correlation was observed between the muscle T/sub 1/ values and the serum creatine phosphokinase values. Increased tissue water content in the lower parts of the body due to gravity is considered to be the primary cause of the high T/sub 1/ value in the gastrocnemius of normal females. The presence of the degenerating muscle fibers are presumed responsible for the high T/sub 1/ value and low BWF in the proximal muscles of DMD carriers.

  19. Mixed micelles of polyethylene glycol (23) lauryl ether with ionic surfactants studied by proton 1D and 2D NMR.

    Science.gov (United States)

    Gao, Hong-Chang; Zhao, Sui; Mao, Shi-Zhen; Yuan, Han-Zhen; Yu, Jia-Yong; Shen, Lian-Fang; Du, You-Ru

    2002-05-01

    (1)H NMR chemical shift, spin-lattice relaxation time, spin-spin relaxation time, self-diffusion coefficient, and two-dimensional nuclear Overhauser enhancement (2D NOESY) measurements have been used to study the nonionic-ionic surfactant mixed micelles. Cetyl trimethyl ammonium bromide (CTAB) and sodium dodecyl sulfate (SDS) were used as the ionic surfactants and polyethylene glycol (23) lauryl ether (Brij-35) as the nonionic surfactant. The two systems are both with varying molar ratios of CTAB/Brij-35 (C/B) and SDS/Brij-35 (S/B) ranging from 0.5 to 2, respectively, at a constant concentration of 6 mM for Brij-35 in aqueous solutions. Results give information about the relative arrangement of the surfactant molecules in the mixed micelles. In the former system, the trimethyl groups attached to the polar heads of the CTAB molecules are located between the first oxy-ethylene groups next to the hydrophobic chains of Brij-35 molecules. These oxy-ethylene groups gradually move outward from the hydrophobic core of the mixed micelle with an increase in C/B in the mixed solution. In contrast to the case of the CTAB/Triton X-100 system, the long flexible hydrophilic poly oxy-ethylene chains, which are in the exterior part of the mixed micelles, remain coiled, but looser, surrounding the hydrophobic core. There is almost no variation in conformation of the hydrophilic chains of Brij-35 molecules in the mixed micelles of the SDS/Brij-35 system as the S/B increases. The hydrophobic chains of both CTAB and SDS are co-aggregated with Brij-35, respectively, in their mixed micellar cores.

  20. nmr spectroscopic study and dft calculations of giao nmr shieldings

    African Journals Online (AJOL)

    Preferred Customer

    3Department of Physics, Arts and Science Faculty, Dumlupinar University, Kütahya, ... 1H, 13C NMR chemical shifts and 1JCH coupling constants of .... then estimated using the corresponding TMS shieldings calculated in advance at the same.

  1. NMR-based milk metabolomics

    DEFF Research Database (Denmark)

    Sundekilde, Ulrik; Larsen, Lotte Bach; Bertram, Hanne Christine S.

    2013-01-01

    and processing capabilities of bovine milk is closely associated to milk composition. Metabolomics is ideal in the study of the low-molecular-weight compounds in milk, and this review focuses on the recent nuclear magnetic resonance (NMR)-based metabolomics trends in milk research, including applications linking...... compounds. Furthermore, metabolomics applications elucidating how the differential regulated genes affects milk composition are also reported. This review will highlight the recent advances in NMR-based metabolomics on milk, as well as give a brief summary of when NMR spectroscopy can be useful for gaining...

  2. Annual reports on NMR spectroscopy

    CERN Document Server

    Webb, Graham A; McCarthy, M J

    1995-01-01

    Over recent years, no other technique has grown to such importance as that of NMR spectroscopy. It is used in all branches of science where precise structural determination is required and where the nature of interactions and reactions in solution is being studied. Annual Reports on NMR Spectroscopy has established itself as a means for the specialist and non-specialist alike to become familiar with new applications of the technique in all branches of chemistry, including biochemistry, and pharmaceutics. This volume focuses on theoretical aspects of NMR nuclear shielding and on applications of

  3. Pressure dependence of coherence-incoherence crossover behavior in KFe2As2 observed by resistivity and 75As-NMR/NQR

    Science.gov (United States)

    Wiecki, P.; Taufour, V.; Chung, D. Y.; Kanatzidis, M. G.; Bud'ko, S. L.; Canfield, P. C.; Furukawa, Y.

    2018-02-01

    We present the results of 75As nuclear magnetic resonance (NMR), nuclear quadrupole resonance (NQR), and resistivity measurements in KFe2As2 under pressure (p ). The temperature dependence of the NMR shift, nuclear spin-lattice relaxation time (T1), and resistivity show a crossover between a high-temperature incoherent, local-moment behavior and a low-temperature coherent behavior at a crossover temperature (T*). T* is found to increase monotonically with pressure, consistent with increasing hybridization between localized 3 d orbital-derived bands with the itinerant electron bands. No anomaly in T* is seen at the critical pressure pc=1.8 GPa where a change of slope of the superconducting (SC) transition temperature Tc(p ) has been observed. In contrast, Tc(p ) seems to correlate with antiferromagnetic spin fluctuations in the normal state as measured by the NQR 1 /T1 data, although such a correlation cannot be seen in the replacement effects of A in the A Fe2As2 (A =K , Rb, Cs) family. In the superconducting state, two T1 components are observed at low temperatures, suggesting the existence of two distinct local electronic environments. The temperature dependence of the short T1 s indicates a nearly gapless state below Tc. On the other hand, the temperature dependence of the long component 1 /T1 L implies a large reduction in the density of states at the Fermi level due to the SC gap formation. These results suggest a real-space modulation of the local SC gap structure in KFe2As2 under pressure.

  4. Smoke, Clouds and Radiation Brazil NASA ER-2 Moderate Resolution Imaging Spectrometer (MODIS) Airborne Simulator (MAS) Data

    Data.gov (United States)

    National Aeronautics and Space Administration — SCARB_ER2_MAS data are Smoke, Clouds and Radiation Brazil (SCARB) NASA ER2 Moderate Resolution Imaging Spectrometer (MODIS) Airborne Simulator (MAS)...

  5. 48 CFR 538.270 - Evaluation of multiple award schedule (MAS) offers.

    Science.gov (United States)

    2010-10-01

    ... SERVICES ADMINISTRATION SPECIAL CATEGORIES OF CONTRACTING FEDERAL SUPPLY SCHEDULE CONTRACTING Establishing and Administering Federal Supply Schedules 538.270 Evaluation of multiple award schedule (MAS) offers... determining the Government's price negotiation objectives, consider the following factors: (1) Aggregate...

  6. β-NMR sample optimization

    CERN Document Server

    Zakoucka, Eva

    2013-01-01

    During my summer student programme I was working on sample optimization for a new β-NMR project at the ISOLDE facility. The β-NMR technique is well-established in solid-state physics and just recently it is being introduced for applications in biochemistry and life sciences. The β-NMR collaboration will be applying for beam time to the INTC committee in September for three nuclei: Cu, Zn and Mg. Sample optimization for Mg was already performed last year during the summer student programme. Therefore sample optimization for Cu and Zn had to be completed as well for the project proposal. My part in the project was to perform thorough literature research on techniques studying Cu and Zn complexes in native conditions, search for relevant binding candidates for Cu and Zn applicable for ß-NMR and eventually evaluate selected binding candidates using UV-VIS spectrometry.

  7. NMR Studies of Polymer Nanocomposites

    National Research Council Canada - National Science Library

    Greenbaum, Steve

    2001-01-01

    .... The primary tool is pulsed field gradient NMR. A static field gradient method was developed which makes possible variable pressure diffusion measurement, and the application to the important fuel cell membrane NAFION constitute the first results...

  8. Integrative NMR for biomolecular research

    International Nuclear Information System (INIS)

    Lee, Woonghee; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L.

    2016-01-01

    NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download_packages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

  9. Integrative NMR for biomolecular research

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Woonghee, E-mail: whlee@nmrfam.wisc.edu; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L., E-mail: markley@nmrfam.wisc.edu [University of Wisconsin-Madison, National Magnetic Resonance Facility at Madison and Biochemistry Department (United States)

    2016-04-15

    NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download{sub p}ackages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

  10. Interpretations of NMR images

    International Nuclear Information System (INIS)

    Shi, J.Z.; McFarland, W.D.; Chen, S.S.; Sadhu, V.K.

    1986-01-01

    Two color display schemes are generally considered in medical images: pseudo-color and color composite. Psuedo-color technique maps the intensity means of a single monochrome image into a three dimensional color space, the gray level is thus replaced by the assigned color. Such a psuedo-color assignment is somewhat arbitrary but may be advantageous if the monochrome image is composed of simple intensity patterns. A good example of psuedo-color application is in nuclear medicine: The change of gray levels can be simply determined and the isocounts from two regions with different surroundings can be readily recognized. However, the use of psuedo-color in CT or MR imaging is controversial because it does not give additional information and may exaggerate insignificant gray scale differences. The color composite technique maps three parametric image data into a three dimensional color space, and thus three monochrome images are merged to form a single color image. The color composite technique increases the number of ways information can be displayed and provides both quantitative and qualitative data about the object or event represented. This paper describes the application of color composite in NMR images

  11. Microfabricated inserts for magic angle coil spinning (MACS wireless NMR spectroscopy.

    Directory of Open Access Journals (Sweden)

    Vlad Badilita

    Full Text Available This article describes the development and testing of the first automatically microfabricated probes to be used in conjunction with the magic angle coil spinning (MACS NMR technique. NMR spectroscopy is a versatile technique for a large range of applications, but its intrinsically low sensitivity poses significant difficulties in analyzing mass- and volume-limited samples. The combination of microfabrication technology and MACS addresses several well-known NMR issues in a concerted manner for the first time: (i reproducible wafer-scale fabrication of the first-in-kind on-chip LC microresonator for inductive coupling of the NMR signal and reliable exploitation of MACS capabilities; (ii improving the sensitivity and the spectral resolution by simultaneous spinning the detection microcoil together with the sample at the "magic angle" of 54.74° with respect to the direction of the magnetic field (magic angle spinning - MAS, accompanied by the wireless signal transmission between the microcoil and the primary circuit of the NMR spectrometer; (iii given the high spinning rates (tens of kHz involved in the MAS methodology, the microfabricated inserts exhibit a clear kinematic advantage over their previously demonstrated counterparts due to the inherent capability to produce small radius cylindrical geometries, thus tremendously reducing the mechanical stress and tearing forces on the sample. In order to demonstrate the versatility of the microfabrication technology, we have designed MACS probes for various Larmor frequencies (194, 500 and 700 MHz testing several samples such as water, Drosophila pupae, adamantane solid and LiCl at different magic angle spinning speeds.

  12. Dynamic Nuclear Polarization enhanced NMR at 187 GHz/284 MHz using an Extended Interaction Klystron amplifier.

    Science.gov (United States)

    Kemp, Thomas F; Dannatt, Hugh R W; Barrow, Nathan S; Watts, Anthony; Brown, Steven P; Newton, Mark E; Dupree, Ray

    2016-04-01

    A Dynamic Nuclear Polarisation (DNP) enhanced solid-state Magic Angle Spinning (MAS) NMR spectrometer which uses a 187 GHz (corresponding to (1)H NMR frequency of 284 MHz) Extended Interaction Klystron (EIK) amplifier as the microwave source is briefly described. Its performance is demonstrated for a biomolecule (bacteriorhodopsin), a pharmaceutical, and surface functionalised silica. The EIK is very compact and easily incorporated into an existing spectrometer. The bandwidth of the amplifier is sufficient that it obviates the need for a sweepable magnetic field, once set, for all commonly used radicals. The variable power (CW or pulsed) output from the EIK is transmitted to the DNP-NMR probe using a quasi-optic system with a high power isolator and a corrugated waveguide which feeds the microwaves into the DNP-NMR probe. Curved mirrors inside the probe project the microwaves down the axis of the MAS rotor, giving a very efficient system such that maximum DNP enhancement is achieved with less than 3 W output from the microwave source. The DNP-NMR probe operates with a sample temperature down to 90K whilst spinning at 8 kHz. Significant enhancements, in excess of 100 for bacteriorhodopsin in purple membrane (bR in PM), are shown along with spectra which are enhanced by ≈25 with respect to room temperature, for both the pharmaceutical furosemide and surface functionalised silica. These enhancements allow hitherto prohibitively time consuming experiments to be undertaken. The power at which the DNP enhancement in bR in PM saturates does not change significantly between 90K and 170 K even though the enhancement drops by a factor of ≈11. As the DNP build up time decreases by a factor 3 over this temperature range, the reduction in T1n is presumably a significant contribution to the drop in enhancement. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

  13. MAS Integration and Controllership Effectiveness: Evidence of a Preparer-User Perception Gap

    OpenAIRE

    Weißenberger, Barbara E.; Angelkort, Hendrik; Holthoff, Gero

    2012-01-01

    Recent evidence suggests that managers establish a positive link between management accounting system (MAS) integration and controllership effectiveness, which is fully mediated by the perceived consistency of financial language. Our paper extends this research by analyzing whether controllers have similar perceptions on MAS design. Testing a series of multi-group structural equation models, we find evidence for a preparer-user perception gap with respect to the mediating impact of a consiste...

  14. NMR characterization of thin films

    Science.gov (United States)

    Gerald II, Rex E.; Klingler, Robert J.; Rathke, Jerome W.; Diaz, Rocio; Vukovic, Lela

    2010-06-15

    A method, apparatus, and system for characterizing thin film materials. The method, apparatus, and system includes a container for receiving a starting material, applying a gravitational force, a magnetic force, and an electric force or combinations thereof to at least the starting material, forming a thin film material, sensing an NMR signal from the thin film material and analyzing the NMR signal to characterize the thin film of material.

  15. NMR imaging of cerebral infarction

    International Nuclear Information System (INIS)

    Takusagawa, Yoshihiko; Yamaoka, Naoki; Doi, Kazuaki; Okada, Keisei

    1987-01-01

    One hundred and five patients with cerebral infarction were studied by nuclear magnetic resonance (NMR) CT (resistive type of magnet with strength of 0.1 tesla) and X-ray CT. Pulse sequences used saturation recovery (Tr = 600 mSec), Inversion recovery (Tr = 500 mSec, Td = 300 mSec) and spin echo (Tr = 1500 mSec, Te = 40, 80, 120, 160 mSec). Fifteen cases were examined by NMR-CT within 24 hours from onset. Proton NMR imaging could not detect cerebral ischemia as early as 2 hours after onset, but except could detect the lesions in Se image the area of cerebral infarct 3 hours after onset. After 5 hours from onset image changes in SE were evident and corresponded to the area of cerebral infarct, but image changes in IR could not fully delineate the infarcted area. NMR images of 41 year-old woman with cerebral embolism by MCA trunck occlusion associated with mitral stenosis were presented, and NMR-CT was examined 10 hours, 9th and 43th days after episode of MCA occlusion. Sixty patents (64 times) with lacunar infarction were studied by NMR-CT and X-ray CT. The inversion recovery images were used mainly for detection of lesions and comparison with X-ray CT. In 160 lesions which were detected by NMR-CT or X-ray CT, could 156 lesions be detected by NMR-CT and 78 lesions by X-ray CT. Inversion recovery images were more useful for detection of lacunes than X-ray CT. Calculated T1 and T2 values prolonged with time course from onset. (author)

  16. Optical pumping and xenon NMR

    International Nuclear Information System (INIS)

    Raftery, M.D.

    1991-11-01

    Nuclear Magnetic Resonance (NMR) spectroscopy of xenon has become an important tool for investigating a wide variety of materials, especially those with high surface area. The sensitivity of its chemical shift to environment, and its chemical inertness and adsorption properties make xenon a particularly useful NMR probe. This work discusses the application of optical pumping to enhance the sensitivity of xenon NMR experiments, thereby allowing them to be used in the study of systems with lower surface area. A novel method of optically-pumping 129 Xe in low magnetic field below an NMR spectrometer and subsequent transfer of the gas to high magnetic field is described. NMR studies of the highly polarized gas adsorbed onto powdered samples with low to moderate surface areas are now possible. For instance, NMR studies of optically-pumped xenon adsorbed onto polyacrylic acid show that xenon has a large interaction with the surface. By modeling the low temperature data in terms of a sticking probability and the gas phase xenon-xenon interaction, the diffusion coefficient for xenon at the surface of the polymer is determined. The sensitivity enhancement afforded by optical pumping also allows the NMR observation of xenon thin films frozen onto the inner surfaces of different sample cells. The geometry of the thin films results in interesting line shapes that are due to the bulk magnetic susceptibility of xenon. Experiments are also described that combine optical pumping with optical detection for high sensitivity in low magnetic field to observe the quadrupoler evolution of 131 Xe spins at the surface of the pumping cells. In cells with macroscopic asymmetry, a residual quadrupolar interaction causes a splitting in the 131 Xe NMR frequencies in bare Pyrex glass cells and cells with added hydrogen

  17. NMR characterization of thin films

    Science.gov (United States)

    Gerald, II, Rex E.; Klingler, Robert J.; Rathke, Jerome W.; Diaz, Rocio; Vukovic, Lela

    2008-11-25

    A method, apparatus, and system for characterizing thin film materials. The method, apparatus, and system includes a container for receiving a starting material, applying a gravitational force, a magnetic force, and an electric force or combinations thereof to at least the starting material, forming a thin film material, sensing an NMR signal from the thin film material and analyzing the NMR signal to characterize the thin film of material.

  18. Paraffin molecule mobility in channel clathrates of urea on spectroscopic NMR relaxation data

    CERN Document Server

    Kriger, Y G; Chekhova, G N

    2001-01-01

    The temperature dependences of the protons spin-lattice relaxation time (T sub I) in the channel clathrates of urea with paraffins are measured. The data on the T sub I are interpreted within the frames of the model of the paraffins molecules and their fragments orientation in the clathrate channels. The dynamics peculiarities are connected with the disproportion effects of these compounds

  19. Manganese-55 NMR and relaxation in single crystals of manganese(12)-Ac and analogs

    Science.gov (United States)

    Harter, Andrew

    This dissertation presents the first single crystal 55Mn NMR characterization of three compounds related to Mn12-acetate [Mn12O12(O2CCH3)16(H 2O)4]·2CH3COOH·4H2O (henceforth Mn12-Ac) that have come to be known as Single-Molecule Magnets (SMMs). This study was undertaken because they exhibit novel phenomena such as quantum mechanical tunneling of their magnetization (QTM), the origin of which is still not fully understood, and also because they have the potential to form elements of magnetic memory storage at the molecular dimensions. The investigations herein involve studies related to both the bonding as well as spin-dynamics in these compounds to much higher precision than in earlier work. These experiments were made possible by the design of a high frequency goniometer probe and a 3He temperature facility. The first single crystal NMR of any Mn12-based molecule was conducted on [Mn12O12(O2CCH2Br) 16(H2O)4]·4CH2Cl2 (Mn12-BrAc). Its 55Mn NMR spectrum, field dependence, angular dependence, and spin-lattice relaxation time (T 1) measurements were conducted. Most importantly, data are presented that (a) confirm the alteration of the magnetic core of these molecules when the samples are crushed into powder (a practice used in earlier studies), (b) show the presence of transverse hyperfine fields at the nuclear site, and (c) do not yield any evidence of temperature independent relaxation below 1 K, suggesting that QTM is not the dominant relaxation mechanism at these temperatures, in contrast to earlier studies. Data from single crystals of Mn12-Ac, the most studied SMM, concur with previous x-ray findings in that isomers are present. Such detailed information was not obtainable with powder samples. T 1-1 measurements over 400 mK--1 K indicate the existence of an energy barrier, in this case ˜1.65 K, which does not fit the current understanding of the electronic energy diagram. This value supports an earlier, yet unexplained observation of such a level by inelastic

  20. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

    International Nuclear Information System (INIS)

    Thurber, Kent R.; Tycko, Robert

    2014-01-01

    We report solid state 13 C and 1 H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, 1 H and cross-polarized 13 C NMR signals from 15 N, 13 C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T 1e is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations

  1. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves.

    Science.gov (United States)

    Thurber, Kent R; Tycko, Robert

    2014-05-14

    We report solid state (13)C and (1)H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, (1)H and cross-polarized (13)C NMR signals from (15)N,(13)C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T1e is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations.

  2. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

    Energy Technology Data Exchange (ETDEWEB)

    Thurber, Kent R., E-mail: thurberk@niddk.nih.gov; Tycko, Robert [Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, Maryland 20892-0520 (United States)

    2014-05-14

    We report solid state {sup 13}C and {sup 1}H nuclear magnetic resonance (NMR) experiments with magic-angle spinning (MAS) on frozen solutions containing nitroxide-based paramagnetic dopants that indicate significant perturbations of nuclear spin polarizations without microwave irradiation. At temperatures near 25 K, {sup 1}H and cross-polarized {sup 13}C NMR signals from {sup 15}N,{sup 13}C-labeled L-alanine in trinitroxide-doped glycerol/water are reduced by factors as large as six compared to signals from samples without nitroxide doping. Without MAS or at temperatures near 100 K, differences between signals with and without nitroxide doping are much smaller. We attribute most of the reduction of NMR signals under MAS near 25 K to nuclear spin depolarization through the cross-effect dynamic nuclear polarization mechanism, in which three-spin flips drive nuclear polarizations toward equilibrium with spin polarization differences between electron pairs. When T{sub 1e} is sufficiently long relative to the MAS rotation period, the distribution of electron spin polarization across the nitroxide electron paramagnetic resonance lineshape can be very different from the corresponding distribution in a static sample at thermal equilibrium, leading to the observed effects. We describe three-spin and 3000-spin calculations that qualitatively reproduce the experimental observations.

  3. Sine-squared shifted pulses for recoupling interactions in solid-state NMR

    Science.gov (United States)

    Jain, Mukul G.; Rajalakshmi, G.; Equbal, Asif; Mote, Kaustubh R.; Agarwal, Vipin; Madhu, P. K.

    2017-06-01

    Rotational-Echo DOuble-Resonance (REDOR) is a versatile experiment for measuring internuclear distance between two heteronuclear spins in solid-state NMR. At slow to intermediate magic-angle spinning (MAS) frequencies, the measurement of distances between strongly coupled spins is challenging due to rapid dephasing of magnetisation. This problem can be remedied by employing the pulse-shifted version of REDOR known as Shifted-REDOR (S-REDOR) that scales down the recoupled dipolar coupling. In this study, we propose a new variant of the REDOR sequence where the positions of the π pulses are determined by a sine-squared function. This new variant has scaling properties similar to S-REDOR. We use theory, numerical simulations, and experiments to compare the dipolar recoupling efficiencies and the experimental robustness of the three REDOR schemes. The proposed variant has advantages in terms of radiofrequency field requirements at fast MAS frequencies.

  4. Medical applications of NMR imaging and NMR spectroscopy with stable isotopes. Summary

    Energy Technology Data Exchange (ETDEWEB)

    Matwiyoff, N.A.

    1983-01-01

    The current status of NMR imaging and NMR spectroscopy are summarized. For the most part examples from the March 1983 Puerto Rico symposium are used to illustrate the utility of NMR in medicine. 18 refs., 5 figs.

  5. Medical applications of NMR imaging and NMR spectroscopy with stable isotopes. Summary

    International Nuclear Information System (INIS)

    Matwiyoff, N.A.

    1983-01-01

    The current status of NMR imaging and NMR spectroscopy are summarized. For the most part examples from the March 1983 Puerto Rico symposium are used to illustrate the utility of NMR in medicine. 18 refs., 5 figs

  6. NMR and NQR studies of 5f-band metamagnetic UCoAl and UCo{sub 1-x}T{sub x}Al (T=Fe,Ni)

    Energy Technology Data Exchange (ETDEWEB)

    Kohori, Y. [Graduate School of Science and Technology, Chiba University, Chiba 263-8522 (Japan) and Department of Physics, Faculty of Science, Chiba University, Chiba 263-8522 (Japan)]. E-mail: kohori@faculty.chiba-u.jp; Fukazawa, H. [Graduate School of Science and Technology, Chiba University, Chiba 263-8522 (Japan); Department of Physics, Faculty of Science, Chiba University, Chiba 263-8522 (Japan); Iwamoto, Y. [Division of Cargo and Transportation Science, Kobe University, Kobe 658-0022 (Japan); Kohara, T. [Graduate School of Material Science, University of Hyogo, Hyogo 678-1297 (Japan); Andreev, A.V. [Institute of Physics, Academy of Sciences of the Czech Republic, Na Slovance 2, 18040 Prague 8 (Czech Republic); Sechovsky, V. [Department of Electronic Structures, Charles University, Ke Karlovu 5, 121 16 Prague 2 (Czech Republic)

    2006-05-01

    The 5f-band system UCoAl, which crystallizes in the hexagonal ZrNiAl-type structure, has the paramagnetic ground state. The magnetic fields H as low as 0.6T oriented along the c-axis induce the metamagnetic transition below 17K. In order to study the magnetic property of UCoAl, we performed {sup 27}Al and {sup 59}Co NMR/NQR measurements in UCoAl, UCo{sub 0.98}Fe{sub 0.02}Al and UCo{sub 0.95}Ni{sub 0.05}Al single crystals. The substitution of Fe stabilizes the ferromagnetic state, and that of Ni stabilizes the paramagnetic state. The nuclear spin-lattice relaxation rate 1/T{sub 1} obtained with the crystal c-axis perpendicular to H is nearly six times larger than the 1/T{sub 1} with the c-axis parallel to H, which reflects the anisotropy of the spin fluctuations of the system.

  7. Glassy spin freezing and NMR wipeout effect in the high-T{sub c} superconductor La{sub 1.90}Sr{sub 0.10}CuO{sub 4}: Critical discussion of the role of stripes

    Energy Technology Data Exchange (ETDEWEB)

    Julien, M.-H.; Campana, A.; Rigamonti, A.; Carretta, P.; Borsa, F.; Kuhns, P.; Reyes, A. P.; Moulton, W. G.; Horvatic, M.; Berthier, C. (and others)

    2001-04-01

    We report on {sup 139}La and {sup 63}Cu NMR/NQR measurements in the high-T{sub c} superconductor La{sub 1.90}Sr{sub 0.10}CuO{sub 4}, with T{sub c}=26.5 K. Spin fluctuations probed by {sup 139}La spin-lattice relaxation (T{sub 1}) continuously slow down on cooling through T{sub c}. We argue that spin freezing and superconductivity are bulk effects in this sample. Thus both phenomena have to coexist microscopically. The distribution of {sup 139}La T{sub 1} values at low temperature reveals a wide spread of spin fluctuation frequencies in CuO{sub 2} planes. A simple estimate shows that {sup 63}Cu nuclei at sites where electronic fluctuations are the slowest are not observable (wipeout effect) because relaxation times are too short. This means that the {sup 63}Cu NQR wipeout, observed in this sample, can be explained primarily by slow magnetic, rather than charge, fluctuations. The magnetic origin of the wipeout is still compatible with a connection between wipeout and charge order [as proposed by Hunt , Phys. Rev. Lett. 82, 4300 (1999)], but this connection is indirect. On the other hand, since the wipeout fraction is not an intensive quantity it cannot define a proper order parameter and cannot be used by itself as a criterion for the existence of a stripe phase.

  8. Glassy spin freezing and NMR wipeout effect in the high-Tc superconductor La1.90Sr0.10CuO4: Critical discussion of the role of stripes

    Science.gov (United States)

    Julien, M.-H.; Campana, A.; Rigamonti, A.; Carretta, P.; Borsa, F.; Kuhns, P.; Reyes, A. P.; Moulton, W. G.; Horvatić, M.; Berthier, C.; Vietkin, A.; Revcolevschi, A.

    2001-04-01

    We report on 139La and 63Cu NMR/NQR measurements in the high-Tc superconductor La1.90Sr0.10CuO4, with Tc=26.5 K. Spin fluctuations probed by 139La spin-lattice relaxation (T1) continuously slow down on cooling through Tc. We argue that spin freezing and superconductivity are bulk effects in this sample. Thus both phenomena have to coexist microscopically. The distribution of 139La T1 values at low temperature reveals a wide spread of spin fluctuation frequencies in CuO2 planes. A simple estimate shows that 63Cu nuclei at sites where electronic fluctuations are the slowest are not observable (wipeout effect) because relaxation times are too short. This means that the 63Cu NQR wipeout, observed in this sample, can be explained primarily by slow magnetic, rather than charge, fluctuations. The magnetic origin of the wipeout is still compatible with a connection between wipeout and charge order [as proposed by Hunt et al., Phys. Rev. Lett. 82, 4300 (1999)], but this connection is indirect. On the other hand, since the wipeout fraction is not an intensive quantity it cannot define a proper order parameter and cannot be used by itself as a criterion for the existence of a stripe phase.

  9. Local magnetic susceptibility, spin dynamics, and charge order in the quasi-one-dimensional conductor β -Li0.33V2O5 investigated by site-selective 51V NMR

    Science.gov (United States)

    Yamauchi, Ichihiro; Itoh, Masayuki; Yamauchi, Touru; Yamaura, Jun-Ichi; Ueda, Yutaka

    2017-11-01

    51V NMR measurements have been conducted on a single crystal of the quasi-one-dimensional conductor β -Li0.33V2O5 which undergoes a metal-insulator (MI) transition at TMI˜170 K. In the metallic phase, we obtain 51V Knight shift and electric field gradient tensors. From the analysis of the 51V Knight shifts, we find that the charge disproportionation appears even in the metallic state and the electronic structure is represented within a model of weakly coupled ladders containing two types of ladders with distinct carrier densities. Based on the 51V nuclear spin-lattice relaxation rate, we discuss the spin dynamics within the one-dimensional electron gas model. From the analysis of several nonmagnetic V5 + spectra observed in the insulating phase, we propose a possible charge-order pattern which has a superlattice modulation larger than those in other family members of β -A0.33V2O5 (A =Na and Ag). Finally, we discuss the A -ion dependence of the electronic structure, the charge disproportionation, and the charge order in β -A0.33V2O5 .

  10. Carbon-13 NMR of flavinoids

    International Nuclear Information System (INIS)

    Agrawal, P.K.

    1989-01-01

    The present book has been written with the objective of introducing the organic chemists with the conceptual and experimental basis required for interpretation of 13 C NMR spectra of a flavonoid and to a discussion of general usefulness of the technique in solving flavonoid structural problem. After a brief general introduction to the essential aspects of flavonoids and 13 C NMR spectroscopy, considerable emphasis has been placed in chapter 2 on the various experimental methods and the interpretation of spectral details which enable individual resonance lines to be associated with the appropriate carbons in a molecule. The whole bulk of the literature, published on 13 C NMR of flavonoids in the major journals upto 1986 alongwith some recent references of 1987 has been classified in several categories such as: flavonoids, isflavonoids, other flavonoids, flavonoid glycosides, chalconoids and flavanoids. Each category constitutes a chapter. Finally the last chapter is devoted largely to a discussion for the differentiation of various categories and subcategories of flavonoids and for the establishment of aromatic substitution pattern in these compounds. It should be emphasized that the book is a data book and only concerned with the actual analysis of 13 C NMR spectra, thus a reasonable familiarity with basic instrumentation of 13 C NMR and general pattern of nuclear chemical shifts has been assumed. (author). refs.; figs.; tabs

  11. Analysis of Hydroperoxides in solid Polyethylene by NMR and EPR Spectroscopy

    International Nuclear Information System (INIS)

    Assink, Roger A.; Celina, Mathias C.; Dunbar, Timothy D.; Alam, Todd M.; Clough, Roger Lee; Gillen, Kenneth T.

    2000-01-01

    The authors have shown that the hydroperoxide species in γ-irradiated 13 C-polyethylene can be directly observed by 13 C MAS NMR spectroscopy. The experiment was performed without the need for special sample preparation such as chemical derivatization or dissolution. Annealing experiments were employed to study the thermal decomposition of the hydroperoxide species and to measure an activation energy of 98 kJ/mol. EPR spectroscopy suggests that residual polyenyl and alkylperoxy radicals are predominantly trapped in interracial or crystalline regions, while the peroxy radicals observed after UV-photolysis of hydroperoxides are in amorphous regions

  12. Real time neutron diffraction and NMR of the Empress II glass-ceramic system.

    Science.gov (United States)

    O'Donnell, M D; Hill, R G; Karpukhina, N; Law, R V

    2011-10-01

    This study reports real time neutron diffraction on the Empress II glass-ceramic system. The commercial glass-ceramics was characterized by real time neutron diffraction, ³¹P and ²⁹Si solid-state MAS-NMR, DSC and XRD. On heating, the as-received glass ceramic contained lithium disilicate (Li₂Si₂O₅), which melted with increasing temperature. This was revealed by neutron diffraction which showed the Bragg peaks for this phase had disappeared by 958°C in agreement with thermal analysis. On cooling lithium metasilicate (Li₂SiO₃) started to form at around 916°C and a minor phase of cristobalite at around 852°C. The unit cell volume of both Li-silicate phases increased linearly with temperature at a rate of +17×10⁻³ ų.°C⁻¹. Room temperature powder X-ray diffraction (XRD) of the material after cooling confirms presence of the lithium metasilicate and cristobalite as the main phases and shows, in addition, small amount of lithium disilicate and orthophosphate. ³¹P MAS-NMR reveals presence of the lithiorthophosphate (Li₃PO₄) before and after heat treatment. The melting of lithium disilicate on heating and crystallisation of lithium metasilicate on cooling agree with endothermic and exotermic features respectively observed by DSC. ²⁹Si MAS-NMR shows presence of lithium disilicate phase in the as-received glass-ceramic, though not in the major proportion, and lithium metasilicate in the material after heat treatment. Both phases have significantly long T₁ relaxation time, especially the lithium metasilicate, therefore, a quantitative analysis of the ²⁹Si MAS-NMR spectra was not attempted. Significance. The findings of the present work demonstrate importance of the commercially designed processing parameters in order to preserve desired characteristics of the material. Processing the Empress II at a rate slower than recommended 60°C min⁻¹ or long isothermal hold at the maximal processing temperature 920°C can cause

  13. The flexibility of SIMPSON and SIMMOL for numerical simulations in solid-and liquid-state NMR spectroscopy

    International Nuclear Information System (INIS)

    Vosegaard, T.; Malmendal, A.; Nielsen, N.C.

    2002-01-01

    Addressing the need for numerical simulations in the design and interpretation of advanced solid- and liquid-state NMR experiments, we present a number of novel features for numerical simulations based on the SIMPSON and SIMMOL open source software packages. Major attention is devoted to the flexibility of these Tcl-interfaced programs for numerical simulation of NMR experiments being complicated by demands for efficient powder averaging, large spin systems, and multiple-pulse rf irradiation. These features are exemplified by fast simulation of second-order quadrupolar powder patterns using crystallite interpolation, analysis of rotary resonance triple-quantum excitation for quadrupolar nuclei, iterative fitting of MQ-MAS spectra by combination of SIMIPSON and MINUIT, simulation of multiple-dimensional PISEMA-type correlation experiments for macroscopically oriented membrane proteins, simulation of Hartman-Hahn polarization transfers in liquid-state NMR, and visualization of the spin evolution under complex composite broad-band excitation pulses. (author)

  14. Neuroprotective Mechanisms of the ACE2-Angiotensin-(1-7)-Mas Axis in Stroke

    DEFF Research Database (Denmark)

    Bennion, Douglas M; Haltigan, Emily; Regenhardt, Robert W

    2015-01-01

    The discovery of beneficial neuroprotective effects of the angiotensin converting enzyme 2-angiotensin-(1-7)-Mas axis [ACE2-Ang-(1-7)-Mas] in ischemic and hemorrhagic stroke has spurred interest in a more complete characterization of its mechanisms of action. Here, we summarize findings that desc......The discovery of beneficial neuroprotective effects of the angiotensin converting enzyme 2-angiotensin-(1-7)-Mas axis [ACE2-Ang-(1-7)-Mas] in ischemic and hemorrhagic stroke has spurred interest in a more complete characterization of its mechanisms of action. Here, we summarize findings...... that describe the protective role of the ACE2-Ang-(1-7)-Mas axis in stroke, along with a focused discussion on the potential mechanisms of neuroprotective effects of Ang-(1-7) in stroke. The latter incorporates evidence describing the actions of Ang-(1-7) to counter the deleterious effects of angiotensin II...... complete understanding of the mechanisms of action of Ang-(1-7) to elicit neuroprotection will serve as an essential step toward research into potential targeted therapeutics in the clinical setting....

  15. NMR investigation of coal extracts

    Energy Technology Data Exchange (ETDEWEB)

    Lang, I; Sebor, G [Ceskoslovenska Akademie Ved, Prague. Hornicky Ustav; Sebor, G Jr; Hajek, M; Mostecky, J [Vysoka Skola Chemicko-Technologicka, Prague (Czechoslovakia)

    1978-07-01

    Proton NMR spectroscopy was used for the evaluation of 10% coal extract solutions in deuterated pyridine. Four types of Czechoslovak coal were analyzed. Agreement was found between the aromaticity of coal extracts calculated from /sup 1/H NMR data using Brown's method and Ladner's and Williams' method and the characterization of an average molecule of the coal extract by the number of non-bridge carbon atoms of aromatic rings, by the overall number of aromatic ring carbon atoms and the number of aromatic rings, determined by the Williams and Ferris methods. The methods for calculating carbon distribution from /sup 1/H NMR data, however, contain some constants theoretically estimated or experimentally found using the method which still remain to be verified.

  16. Two-dimensional NMR spectrometry

    International Nuclear Information System (INIS)

    Farrar, T.C.

    1987-01-01

    This article is the second in a two-part series. In part one (ANALYTICAL CHEMISTRY, May 15) the authors discussed one-dimensional nuclear magnetic resonance (NMR) spectra and some relatively advanced nuclear spin gymnastics experiments that provide a capability for selective sensitivity enhancements. In this article and overview and some applications of two-dimensional NMR experiments are presented. These powerful experiments are important complements to the one-dimensional experiments. As in the more sophisticated one-dimensional experiments, the two-dimensional experiments involve three distinct time periods: a preparation period, t 0 ; an evolution period, t 1 ; and a detection period, t 2

  17. Effects of amantadine on the dynamics of membrane-bound influenza A M2 transmembrane peptide studied by NMR relaxation

    Energy Technology Data Exchange (ETDEWEB)

    Cady, Sarah D.; Hong Mei [Iowa State University, Department of Chemistry (United States)], E-mail: mhong@iastate.edu

    2009-09-15

    The molecular motions of membrane proteins in liquid-crystalline lipid bilayers lie at the interface between motions in isotropic liquids and in solids. Specifically, membrane proteins can undergo whole-body uniaxial diffusion on the microsecond time scale. In this work, we investigate the {sup 1}H rotating-frame spin-lattice relaxation (T{sub 1{rho}}) caused by the uniaxial diffusion of the influenza A M2 transmembrane peptide (M2TMP), which forms a tetrameric proton channel in lipid bilayers. This uniaxial diffusion was proved before by {sup 2}H, {sup 15}N and {sup 13}C NMR lineshapes of M2TMP in DLPC bilayers. When bound to an inhibitor, amantadine, the protein exhibits significantly narrower linewidths at physiological temperature. We now investigate the origin of this line narrowing through temperature-dependent {sup 1}H T{sub 1{rho}} relaxation times in the absence and presence of amantadine. Analysis of the temperature dependence indicates that amantadine decreases the correlation time of motion from 2.8 {+-} 0.9 {mu}s for the apo peptide to 0.89 {+-} 0.41 {mu}s for the bound peptide at 313 K. Thus the line narrowing of the bound peptide is due to better avoidance of the NMR time scale and suppression of intermediate time scale broadening. The faster diffusion of the bound peptide is due to the higher attempt rate of motion, suggesting that amantadine creates better-packed and more cohesive helical bundles. Analysis of the temperature dependence of ln (T{sub 1{rho}}{sup -1}) indicates that the activation energy of motion increased from 14.0 {+-} 4.0 kJ/mol for the apo peptide to 23.3 {+-} 6.2 kJ/mol for the bound peptide. This higher activation energy indicates that excess amantadine outside the protein channel in the lipid bilayer increases the membrane viscosity. Thus, the protein-bound amantadine speeds up the diffusion of the helical bundles while the excess amantadine in the bilayer increases the membrane viscosity.

  18. Escala de atitudes frente ao dinheiro (MAS: Teste de modelos e poder preditivo

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Pimentel

    2012-01-01

    Full Text Available The social importance attached to money and its role as an important motivator of behavior justifies the study of its psychosocial aspects. But there is a lack of studies concerning attitudinal or psychological aspects of money in Brazil. In order to encourage research in this context, the validity of the Money Attitudes Scale (MAS was tested using confirmatory factor approaches. Results supported a brief 16-items version of the scale and replicated the factor analytic pattern with satisfactory internal consistency for the factors of power, retention, distrust, and anxiety. Age differences were observed regarding money attitudes of power, and the predictive role of the MAS to account for consumer behavior was also confirmed. This version of the MAS shows evidences of factorial validity and reliability, justifying its use in future research.

  19. SIMPSON: A general simulation program for solid-state NMR spectroscopy

    Science.gov (United States)

    Bak, Mads; Rasmussen, Jimmy T.; Nielsen, Niels Chr.

    2011-12-01

    A computer program for fast and accurate numerical simulation of solid-state NMR experiments is described. The program is designed to emulate a NMR spectrometer by letting the user specify high-level NMR concepts such as spin systems, nuclear spin interactions, RF irradiation, free precession, phase cycling, coherence-order filtering, and implicit/explicit acquisition. These elements are implemented using the Tel scripting language to ensure a minimum of programming overhead and direct interpretation without the need for compilation, while maintaining the flexibility of a full-featured programming language. Basicly, there are no intrinsic limitations to the number of spins, types of interactions, sample conditions (static or spinning, powders, uniaxially oriented molecules, single crystals, or solutions), and the complexity or number of spectral dimensions for the pulse sequence. The applicability ranges from simple ID experiments to advanced multiple-pulse and multiple-dimensional experiments, series of simulations, parameter scans, complex data manipulation/visualization, and iterative fitting of simulated to experimental spectra. A major effort has been devoted to optimizing the computation speed using state-of-the-art algorithms for the time-consuming parts of the calculations implemented in the core of the program using the C programming language. Modification and maintenance of the program are facilitated by releasing the program as open source software (General Public License) currently at http://nmr.imsb.au.dk. The general features of the program are demonstrated by numerical simulations of various aspects for REDOR, rotational resonance, DRAMA, DRAWS, HORROR, C7, TEDOR, POST-C7, CW decoupling, TPPM, F-SLG, SLF, SEMA-CP, PISEMA, RFDR, QCPMG-MAS, and MQ-MAS experiments.

  20. Push-through Direction Injectin NMR Automation

    Science.gov (United States)

    Nuclear magnetic resonance (NMR) and mass spectrometry (MS) are the two major spectroscopic techniques successfully used in metabolomics studies. The non-invasive, quantitative and reproducible characteristics make NMR spectroscopy an excellent technique for detection of endogeno...

  1. Development of a generic, computerized nuclear material accountability system: NucMAS

    International Nuclear Information System (INIS)

    Cornell, M.D.; O'Leary, J.M.

    1987-01-01

    The application NucMAS provides basic computerized accountability functions for the Savannah River Plant (SRP) Separations Department Material Balance Areas (MBA's). These functions include data entry, data management, calculations, and report generation. NucMAS can be used both for routine reporting to the SRP central Material Control and Accounting (MC and A) system and for rapid ad hoc queries in emergency situations. The system is designed to work with any process handling one or more of the 17 accountable nuclear materials specified by the Department of Energy (DOE). It relies on user-supplied configuration data to drive data prompts, report headings, data validations, and calculations

  2. Structure resolution of Ba5Al3F19 and Iivestigation of fluorine ion dynamics by synchrotron powder diffraction, variable-temperature solid-state NMR, and quantum computations

    International Nuclear Information System (INIS)

    Martineau, C.; Fayon, F.; Suchomel, M.R.; Allix, M.; Massiot, D.; Taulelle, F.

    2011-01-01

    The room temperature structure of Ba 5 Al 3 F 19 has been solved using electron microscopy and synchrotron powder diffraction data. One-dimensional (1D) 27 Al and ultrafast magic-angle-spinning (MAS) 19 F NMR spectra have been recorded and are in agreement with the proposed structural model for Ba 5 Al 3 F 19 . The 19 F isotropic chemical shift and 27 Al quadrupolar parameters have been calculated using the CASTEP code from the experimental and density functional theory geometry-optimized structures. After optimization, the calculated NMR parameters of both the 19 F and 27 Al nuclei show improved consistency with the experimental values, demonstrating that the geometry optimization step is necessary to obtain more accurate and reliable structural data. This also enables a complete and unambiguous assignment of the 19 F MAS NMR spectrum of Ba 5 Al 3 F 19 . Variable-temperature 1D MAS 19 F NMR experiments have been carried out, showing the occurrence of fluorine ion mobility. Complementary insights were obtained from both two-dimensional (2D) exchange and 2D double-quantum dipolar recoupling NMR experiments, and a detailed analysis of the anionic motion in Ba 5 Al 3 F 19 is proposed, including the distinction between reorientational processes and chemical exchange involving bond breaking and re-formation.

  3. Characterization of new materials in chromatography and fuel cell development by modern NMR techniques; Charakterisierung neuer Materialien in der Chromatographie und Brennstoffzellen-Forschung mit Hilfe moderner NMR-Techniken

    Energy Technology Data Exchange (ETDEWEB)

    Schauff, S.

    2007-12-28

    New materials, suitable for the application in reversed phase liquid chromatography and fuel cell membranes, were characterized regarding their structure and dynamic properties using solid-state and suspended-state NMR spectroscopy. Both methods were found to be suitable to study the dynamic behaviour, the first to observe intrinsic mobilities of phosphonic acids, the second to monitor interaction processes taking place in a chromatography-like system. Several phosphonic acids, which are promising materials for high temperature fuel cell membranes, were investigated with respect to proton mobility and transport applying various solid-state NMR methods. In addition, water uptake and its effects on anhydride formation were studied on samples that were equilibrated with saturated salt solutions. For PVPA substantial, reversible anhydride formation was found, while MePA did not show condensation. These results show that the relation between hydrogen bond strength and proton mobility is complex. In particular, this work demonstrates that the application of simple 1D 1H and 2H NMR experiments provides easy access to information about proton/deuteron mobility on short time scales, needed for an identification of materials with high intrinsic proton conductivities. Stationary phases for reversed phase liquid chomatography were characterized by solid-state NMR spectroscopy, and their influence on different analytes was studied using suspendedstate HR-MAS NMR spectroscopy. Suspended-state HR-MAS NMR spectroscopy showed to be suitable to model the separation process of analytes on chromatographic sorbents. For this, the stationary phase was suspended in a solution of analyte dissolved in mobile phase. MePhSucc showed a peak doubling of the CH2 group in presence of monomeric C18 phase, leading to the coexistence of a narrow and a broadened peak. Thus, the dynamic interactions of MePhSucc towards the stationary phase, and under the influence of the mobile phase, could be

  4. Fourier transform n.m.r. spectroscopy

    International Nuclear Information System (INIS)

    Shaw, D.

    1976-01-01

    This book is orientated to techniques rather than applications. The basic theory of n.m.r. is dealt with in a unified approach to the Fourier theory. The middle section of the book concentrates on the practical aspects of Fourier n.m.r., both instrumental and experimental. The final chapters briefly cover general application of n.m.r., but concentrate strongly on those areas where Fourier n.m.r. can give information which is not available by conventional techniques

  5. NMR investigations of molecular dynamics

    Science.gov (United States)

    Palmer, Arthur

    2011-03-01

    NMR spectroscopy is a powerful experimental approach for characterizing protein conformational dynamics on multiple time scales. The insights obtained from NMR studies are complemented and by molecular dynamics (MD) simulations, which provide full atomistic details of protein dynamics. Homologous mesophilic (E. coli) and thermophilic (T. thermophilus) ribonuclease H (RNase H) enzymes serve to illustrate how changes in protein sequence and structure that affect conformational dynamic processes can be monitored and characterized by joint analysis of NMR spectroscopy and MD simulations. A Gly residue inserted within a putative hinge between helices B and C is conserved among thermophilic RNases H, but absent in mesophilic RNases H. Experimental spin relaxation measurements show that the dynamic properties of T. thermophilus RNase H are recapitulated in E. coli RNase H by insertion of a Gly residue between helices B and C. Additional specific intramolecular interactions that modulate backbone and sidechain dynamical properties of the Gly-rich loop and of the conserved Trp residue flanking the Gly insertion site have been identified using MD simulations and subsequently confirmed by NMR spin relaxation measurements. These results emphasize the importance of hydrogen bonds and local steric interactions in restricting conformational fluctuations, and the absence of such interactions in allowing conformational adaptation to substrate binding.

  6. PSYCHE Pure Shift NMR Spectroscopy.

    Science.gov (United States)

    Foroozandeh, Mohammadali; Morris, Gareth; Nilsson, Mathias

    2018-03-13

    Broadband homodecoupling techniques in NMR, also known as "pure shift" methods, aim to enhance spectral resolution by suppressing the effects of homonuclear coupling interactions to turn multiplet signals into singlets. Such techniques typically work by selecting a subset of "active" nuclear spins to observe, and selectively inverting the remaining, "passive", spins to reverse the effects of coupling. Pure Shift Yielded by Chirp Excitation (PSYCHE) is one such method; it is relatively recent, but has already been successfully implemented in a range of different NMR experiments. Paradoxically, PSYCHE is one of the trickiest of pure shift NMR techniques to understand but one of the easiest to use. Here we offer some insights into theoretical and practical aspects of the method, and into the effects and importance of the experimental parameters. Some recent improvements that enhance the spectral purity of PSYCHE spectra will be presented, and some experimental frameworks including examples in 1D and 2D NMR spectroscopy, for the implementation of PSYCHE will be introduced. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Measurement of backbone hydrogen-deuterium exchange in the type III secretion system needle protein PrgI by solid-state NMR

    Science.gov (United States)

    Chevelkov, Veniamin; Giller, Karin; Becker, Stefan; Lange, Adam

    2017-10-01

    In this report we present site-specific measurements of amide hydrogen-deuterium exchange rates in a protein in the solid state phase by MAS NMR. Employing perdeuteration, proton detection and a high external magnetic field we could adopt the highly efficient Relax-EXSY protocol previously developed for liquid state NMR. According to this method, we measured the contribution of hydrogen exchange on apparent 15N longitudinal relaxation rates in samples with differing D2O buffer content. Differences in the apparent T1 times allowed us to derive exchange rates for multiple residues in the type III secretion system needle protein.

  8. A High-Resolution Magic Angle Spinning NMR Study of the Enantiodiscrimination of 3,4-Methylenedioxymethamphetamine (MDMA by an Immobilized Polysaccharide-Based Chiral Phase.

    Directory of Open Access Journals (Sweden)

    Juliana C Barreiro

    Full Text Available This paper reports the investigation of the chiral interaction between 3,4-methylenedioxy-methamphetamine (MDMA enantiomers and an immobilized polysaccharide-based chiral phase. For that, suspended-state high-resolution magic angle spinning nuclear magnetic resonance spectroscopy (1H HR-MAS NMR was used. 1H HR-MAS longitudinal relaxation time and Saturation Transfer Difference (STD NMR titration experiments were carried out yielding information at the molecular level of the transient diastereoisomeric complexes of MDMA enantiomers and the chiral stationary phase. The interaction of the enantiomers takes place through the aromatic moiety of MDMA and the aromatic group of the chiral selector by π-π stacking for both enantiomers; however, a stronger interaction was observed for the (R-enantiomer, which is the second one to elute at the chromatographic conditions.

  9. 1H High Resolution Magic-Angle Coil Spinning (HR-MACS µNMR Metabolic Profiling of whole Saccharomyces cervisiae cells: A Demonstrative Study

    Directory of Open Access Journals (Sweden)

    Alan eWong

    2014-06-01

    Full Text Available The low sensitivity of Nuclear Magnetic Resonance (NMR is its prime shortcoming compared to other analytical methods for metabolomic studies. It relies on large sample volume (30–50 µl for HR-MAS for rich metabolic profiling, hindering high-throughput screening especially when the sample requires a labor-intensive preparation or is a sacred specimen. This is indeed the case for some living organisms. This study evaluates a 1H HR-MAS approach for metabolic profiling of small volume (250 nl whole bacterial cells, Saccharomyces cervisiae, using an emerging micro-NMR technology: high-resolution magic-angle coil spinning (HR-MACS. As a demonstrative study for whole cells, we perform two independent metabolomics studies identifying the significant metabolites associated with osmotic stress and aging.

  10. Who bears the burden of international taxation? Evidence from cross-border M&As

    NARCIS (Netherlands)

    Huizinga, H.P.; Voget, J.; Wagner, W.B.

    2012-01-01

    Cross-border M&As can trigger additional taxation of the target's income in the form of non-resident dividend withholding taxes and acquirer-country corporate income taxation. This paper finds that this additional international taxation is fully capitalized into lower takeover premiums. In contrast,

  11. Acceptance Test Report for the Modular Automation System (MAS) Manufactured by Honeywell Inc

    International Nuclear Information System (INIS)

    ANDERSON, D.L.

    2000-01-01

    This document details the performance of the acceptance test of the Honeywell MAS Control System for equipment to be installed in gloveboxes HA-20MB and HA-211 at a later date. Equipment that was anticipated included 6 stabilization furnaces, only three and their associated equipment were installed

  12. SecMAS: Security Enhanced Monitoring and Analysis Systems for Wireless Sensor Networks

    Directory of Open Access Journals (Sweden)

    Ding Chao

    2016-01-01

    Full Text Available The monitoring, control, and security guarantee for the communication in the wireless sensor networks (WSNs are currently treated as three independent issues and addressed separately through specialized tools. However, most cases of WSNs applications requires the network administrator change the network configuration in a very short time to response to the change of observed phenomenon with security guarantee. To meet this requirement, we propose a security enhanced monitoring and control platform named SecMAS for WSNs, which provides the real-time visualization about network states and online reconfiguration of the network properties and behaviours in a resource-efficient way. Besides, basic cryptographic primitives and part of the anomaly detection functionalities are implemented in SecMAS to enabling the secure communication in WSNs. Furthermore, we conduct experiments to evaluate the performance of SecMAS in terms of the latency, throughput, communication overhead, and the security capacity. The experimental results demonstrate that the SecMAS system achieves stable, efficient and secure data collection with lightweight quick-response network control.

  13. Characterization and significance of ACE2 and Mas receptor in human colon adenocarcinoma.

    Science.gov (United States)

    Bernardi, Stella; Zennaro, Cristina; Palmisano, Silvia; Velkoska, Elena; Sabato, Nicoletta; Toffoli, Barbara; Giacomel, Greta; Buri, Luigi; Zanconati, Fabrizio; Bellini, Giuseppe; Burrell, Louise M; De Manzini, Nicolò; Fabris, Bruno

    2012-03-01

    A new arm of the renin-angiotensin system (RAS) has been recently characterized; this includes angiotensin converting enzyme (ACE)2 and angiotensin (Ang)1-7, a heptapeptide acting through the Mas receptor (MasR). Recent studies show that Ang1-7 has an antiproliferative action on lung adenocarcinoma cells. The aim of this study was to characterize RAS expression in human colon adenocarcinoma and to investigate whether Ang1-7 exerts an antiproliferative effect on human colon adenocarcinoma cells. Gene, protein expression and enzymatic activity of the main components of the RAS were determined on non-neoplastic colon mucosa as well as on the tumor mass and the mucosa taken 5 cm distant from it, both collected from patients with colon adenocarcinoma. Two different human colon cancer cell lines were treated with AngII and Ang1-7. The novel finding of this study was that MasR was significantly upregulated in colon adenocarcinoma compared with non-neoplastic colon mucosa, which showed little or no expression of it. ACE gene expression and enzymatic activity were also increased in the tumors. However, AngII and Ang1-7 did not have any pro-/antiproliferative effects in the cell lines studied. The data suggest that upregulation of the MasR could be used as a diagnostic marker of colon adenocarcinoma.

  14. 77 FR 43084 - Multiple Award Schedule (MAS) Program Continuous Open Season-Operational Change

    Science.gov (United States)

    2012-07-23

    ... (GSA), Federal Acquisition Service (FAS) intends to institute a Demand Based Model (DBM) designed to... will restore and maintain the MAS program's value to Federal agencies as a streamlined acquisition... adding innovative solutions, improving pricing and simplifying the buying experience. DATES: This change...

  15. An Analysis of the Rise and Fall of the AA-MAS Policy

    Science.gov (United States)

    Lazarus, Sheryl S.; Thurlow, Martha L.; Ysseldyke, James E.; Edwards, Lynn M.

    2015-01-01

    In 2005, to address concerns about students who might fall in the "gap" between the regular assessment and the alternate assessment based on alternate achievement standards (AA-AAS), the U.S. Department of Education announced that states could develop alternate assessments based on modified achievement standards (AA-MAS). This article…

  16. Considerations for Consortia as States Transition Away from AA-MAS. NCEO Brief. Number 7

    Science.gov (United States)

    National Center on Educational Outcomes, 2014

    2014-01-01

    States with an alternate assessment based on modified achievement standards (AA-MAS) that received a flexibility waiver from some of the requirements of No Child Left Behind are required to phase out their use of this assessment. And, on August 23, 2013, the U.S. Department of Education published a proposed rollback of regulation that allowed the…

  17. Successfully Transitioning from the AA-MAS to the General Assessment. NCEO Policy Directions. Number 22

    Science.gov (United States)

    Lazarus, Sheryl; Thurlow, Martha; Christensen, Laurene; Shyyan, Vitaliy

    2014-01-01

    Federal policy initiatives such as the flexibility waivers for accountability are requiring that states transition away from the use of an alternate assessment based on modified achievement standards (AA-MAS). It is expected that those students who had participated in that assessment will instead participate in the state's general assessment (or a…

  18. Marker-assisted-selection (MAS): A fast track to increase genetic ...

    African Journals Online (AJOL)

    Mapping and tagging of agriculturally important genes have been greatly facilitated by an array of molecular markers in crop plants. Marker-assisted selection (MAS) is gaining considerable importance as it would improve the efficiency of plant breeding through precise transfer of genomic regions of interest (foreground ...

  19. Two-Stage MAS Technique for Analysis of DRA Elements and Arrays on Finite Ground Planes

    DEFF Research Database (Denmark)

    Larsen, Niels Vesterdal; Breinbjerg, Olav

    2007-01-01

    A two-stage Method of Auxiliary Sources (MAS) technique is proposed for analysis of dielectric resonator antenna (DRA) elements and arrays on finite ground planes (FGPs). The problem is solved by first analysing the DRA on an infinite ground plane (IGP) and then using this solution to model the FGP...

  20. HUBUNGAN ANTARA PERTUMBUHAN DENGAN KEBERADAAN GEN TAHAN PENYAKIT MAJOR HISTOCOMPATIBILITY COMPLEX (MHC PADA IKAN MAS (Cyprinus carpio

    Directory of Open Access Journals (Sweden)

    Erma Primanita Hayuningtyas

    2016-04-01

    Full Text Available Wabah penyakit koi herpes virus (KHV di Indonesia yang terjadi sejak tahun 2002 merupakan salah satu faktor yang memicu kemerosotan produksi ikan mas budidaya. Pembentukan strain unggul ikan mas tahan KHV dapat menjadi solusi bagi permasalahan tersebut. Pemilihan genotip ikan mas tahan KHV dengan marka molekuler gen major histocompatibility complex class II (MHC-II, khususnya pada alel Cyca DAB 1*05 akan membantu dalam kegiatan seleksi. Penelitian ini bertujuan untuk mengetahui keberadaan gen MHC-II pada populasi dasar G0 ikan mas strain Rajadanu dan hubungannya dengan pertumbuhan (bobot. Metode deteksi keberadaan gen MHC-II pada dua kelompok ikan dengan ukuran berbeda dilakukan dengan teknik PCR. Hubungan antara pertumbuhan ikan mas dengan persentase kemunculan gen MHC-II dianalisis dengan menggunakan program SPSS (Statistical Package for the Social Sciences, sehingga diperoleh korelasi di antara keduanya. Hasil penelitian menunjukkan bahwa hubungan antara pertumbuhan dengan persentase keberadaan gen MHC-II berkorelasi negatif dengan nilai R = -0,742. Hal ini mengindikasikan bahwa semakin cepat pertumbuhan populasi ikan mas maka semakin sedikit persentase individu yang mempunyai gen MHC-II pada setiap populasi ikan mas. Sehingga populasi ikan mas yang pertumbuhannya lambat memiliki tingkat persentase positif MHC-II lebih tinggi (85,71%-100% dibandingkan populasi ikan mas yang pertumbuhannya cepat (42,86%-85,71%.