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Sample records for variable angle nmr

  1. Variable angle correlation spectroscopy

    International Nuclear Information System (INIS)

    Lee, Y.K.; Lawrence Berkeley Lab., CA

    1994-05-01

    In this dissertation, a novel nuclear magnetic resonance (NMR) technique, variable angle correlation spectroscopy (VACSY) is described and demonstrated with 13 C nuclei in rapidly rotating samples. These experiments focus on one of the basic problems in solid state NMR: how to extract the wealth of information contained in the anisotropic component of the NMR signal while still maintaining spectral resolution. Analysis of the anisotropic spectral patterns from poly-crystalline systems reveal information concerning molecular structure and dynamics, yet in all but the simplest of systems, the overlap of spectral patterns from chemically distinct sites renders the spectral analysis difficult if not impossible. One solution to this problem is to perform multi-dimensional experiments where the high-resolution, isotropic spectrum in one dimension is correlated with the anisotropic spectral patterns in the other dimensions. The VACSY technique incorporates the angle between the spinner axis and the static magnetic field as an experimental parameter that may be incremented during the course of the experiment to help correlate the isotropic and anisotropic components of the spectrum. The two-dimensional version of the VACSY experiments is used to extract the chemical shift anisotropy tensor values from multi-site organic molecules, study molecular dynamics in the intermediate time regime, and to examine the ordering properties of partially oriented samples. The VACSY technique is then extended to three-dimensional experiments to study slow molecular reorientations in a multi-site polymer system

  2. 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.

  3. Variable angle asymmetric cut monochromator

    International Nuclear Information System (INIS)

    Smither, R.K.; Fernandez, P.B.

    1993-09-01

    A variable incident angle, asymmetric cut, double crystal monochromator was tested for use on beamlines at the Advanced Photon Source (APS). For both undulator and wiggler beams the monochromator can expand area of footprint of beam on surface of the crystals to 50 times the area of incident beam; this will reduce the slope errors by a factor of 2500. The asymmetric cut allows one to increase the acceptance angle for incident radiation and obtain a better match to the opening angle of the incident beam. This can increase intensity of the diffracted beam by a factor of 2 to 5 and can make the beam more monochromatic, as well. The monochromator consists of two matched, asymmetric cut (18 degrees), silicon crystals mounted so that they can be rotated about three independent axes. Rotation around the first axis controls the Bragg angle. The second rotation axis is perpendicular to the diffraction planes and controls the increase of the area of the footprint of the beam on the crystal surface. Rotation around the third axis controls the angle between the surface of the crystal and the wider, horizontal axis for the beam and can make the footprint a rectangle with a minimum. length for this area. The asymmetric cut is 18 degrees for the matched pair of crystals, which allows one to expand the footprint area by a factor of 50 for Bragg angles up to 19.15 degrees (6 keV for Si[111] planes). This monochromator, with proper cooling, will be useful for analyzing the high intensity x-ray beams produced by both undulators and wigglers at the APS

  4. Practical evaluation of action-angle variables

    International Nuclear Information System (INIS)

    Boozer, A.H.

    1984-02-01

    A practical method is described for establishing action-angle variables for a Hamiltonian system. That is, a given nearly integrable Hamiltonian is divided into an exactly integrable system plus a perturbation in action-angle form. The transformation of variables, which is carried out using a few short trajectory integrations, permits a rapid determination of trajectory properties throughout a phase space volume

  5. 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

  6. Nuclear Magnetic Resonance Spectroscopy Applications: Proton NMR In Biological Objects Subjected To Magic Angle Spinning

    International Nuclear Information System (INIS)

    Wind, Robert A.; Hu, Jian Zhi

    2005-01-01

    Proton NMR in Biological Objects Submitted to Magic Angle Spinning, In Encyclopedia of Analytical Science, Second Edition (Paul J. Worsfold, Alan Townshend and Colin F. Poole, eds.), Elsevier, Oxford 6:333-342. Published January 1, 2005. Proposal Number 10896

  7. A variable angle slant-hole collimator

    International Nuclear Information System (INIS)

    Moore, R.H.; Alpert, N.M.; Strauss, H.W.

    1983-01-01

    A variable-angle slant-hole (VASH) collimator was constructed to show the feasibility of using multiple sliding plates to achieve a range of collimator channel inclinations. One hundred and sixty tungsten plates, 0.125 mm thick and 14 cm square, were photoetched to produce 3025 1.5-mm2 holes in each plate, separated by 0.8-mm septa. Along with the collimator holes, registration holes and positioning grooves were also etched. The plates were placed in a holder and stacked to form a collimator 2.0 cm high. The holder permitted the plates to be sheared to achieve viewing angles from 0 to 40 degrees from the vertical. Resolution and sensitivity were determined both across and along the shear directions. Resolution of a thin /sup 99m/Tc source, 1.24 mm diam and 7 cm long, located 5 cm from the collimator face in air, was 1.1 cm FWHM at 0 degree shear and remained unchanged with increasing slant. The resolution was similar both across and along the shear plane. Sensitivity was determined with a point source placed 7 cm from the collimator face. At 0 degree slant the sensitivity was 169 cps/MBq (6.24 csp/mu Ci). A general all purpose (GAP) collimator had a FWHM of 1 cm for the line source in air at 5 cm, and a sensitivity of 205 cps/MBq (7.58 cps/mu Ci) for the point source at 7 cm. The data suggest that a variable-angle slant-hole collimator can be constructed of laminated plates

  8. NMR and rotational angles in solution conformation of polypeptides

    Science.gov (United States)

    Bystrov, V. F.

    1985-01-01

    Professor San-Ichiro Mizushima and Professor Yonezo Morino's classical contributions provided unique means and firm basis for understanding of conformational states and internal rotation in polypeptide molecules. Now the NMR spectroscopy is the best choice to study molecular conformation, mechanism of action and structure-functional relationships of peptide and proteins in solution under conditions approaching those of their physiological environments. Crucial details of spatial structure and interactions of these molecules in solution are revealed by using proton-proton and carbon-proton vicinal coupling constants, proton nuclear Overhauser effect and spectral perturbation techniques. The results of NMR conformational analysis are presented for valinomycin "bracelet", gramicidin A double helices, honey-bee neurotoxin apamin, scorpion insectotoxins and snake neurotoxins of long and short types.

  9. 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.

  10. Apparatus and method for variable angle slant hole collimator

    Science.gov (United States)

    Lee, Seung Joon; Kross, Brian J.; McKisson, John E.

    2017-07-18

    A variable angle slant hole (VASH) collimator for providing collimation of high energy photons such as gamma rays during radiological imaging of humans. The VASH collimator includes a stack of multiple collimator leaves and a means of quickly aligning each leaf to provide various projection angles. Rather than rotate the detector around the subject, the VASH collimator enables the detector to remain stationary while the projection angle of the collimator is varied for tomographic acquisition. High collimator efficiency is achieved by maintaining the leaves in accurate alignment through the various projection angles. Individual leaves include unique angled cuts to maintain a precise target collimation angle. Matching wedge blocks driven by two actuators with twin-lead screws accurately position each leaf in the stack resulting in the precise target collimation angle. A computer interface with the actuators enables precise control of the projection angle of the collimator.

  11. Hydrogen and deuterium NMR of solids by magic-angle spinning

    International Nuclear Information System (INIS)

    Eckman, R.R.

    1982-10-01

    The nuclear magnetic resonance of solids has long been characterized by very large specral broadening which arises from internuclear dipole-dipole coupling or the nuclear electric quadrupole interaction. These couplings can obscure the smaller chemical shift interaction and make that information unavailable. Two important and difficult cases are that of hydrogen and deuterium. The development of cross polarization, heteronuclear radiofrequency decoupling, and coherent averaging of nuclear spin interactions has provided measurement of chemical shift tensors in solids. Recently, double quantum NMR and double quantum decoupling have led to measurement of deuterium and proton chemical shift tensors, respectively. A general problem of these experiments is the overlapping of the tensor powder pattern spectra of magnetically distinct sites which cannot be resolved. In this work, high resolution NMR of hydrogen and deuterium in solids is demonstrated. For both nuclei, the resonances are narrowed to obtain liquid-like isotropic spectra by high frequency rotation of the sample about an axis inclined at the magic angle, β/sub m/ = Arccos (3/sup -1/2/), with respect to the direction of the external magnetic field. For deuterium, the powder spectra were narrowed by over three orders of magnitude by magic angle rotation with precise control of β. A second approach was the observation of deuterium double quantum transitions under magic angle rotation. For hydrogen, magic angle rotation alone could be applied to obtain the isotropic spectrum when H/sub D/ was small. This often occurs naturally when the nuclei are semi-dilute or involved in internal motion. In the general case of large H/sub D/, isotropic spectra were obtained by dilution of 1 H with 2 H combined with magic angle rotation. The resolution obtained represents the practical limit for proton NMR of solids

  12. 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

  13. Uncertainty in T1 mapping using the variable flip angle method with two flip angles

    International Nuclear Information System (INIS)

    Schabel, Matthias C; Morrell, Glen R

    2009-01-01

    Propagation of errors, in conjunction with the theoretical signal equation for spoiled gradient echo pulse sequences, is used to derive a theoretical expression for uncertainty in quantitative variable flip angle T 1 mapping using two flip angles. This expression is then minimized to derive a rigorous expression for optimal flip angles that elucidates a commonly used empirical result. The theoretical expressions for uncertainty and optimal flip angles are combined to derive a lower bound on the achievable uncertainty for a given set of pulse sequence parameters and signal-to-noise ratio (SNR). These results provide a means of quantitatively determining the effect of changing acquisition parameters on T 1 uncertainty. (note)

  14. Protein backbone and sidechain torsion angles predicted from NMR chemical shifts using artificial neural networks

    Energy Technology Data Exchange (ETDEWEB)

    Shen Yang; Bax, Ad, E-mail: bax@nih.gov [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)

    2013-07-15

    A new program, TALOS-N, is introduced for predicting protein backbone torsion angles from NMR chemical shifts. The program relies far more extensively on the use of trained artificial neural networks than its predecessor, TALOS+. Validation on an independent set of proteins indicates that backbone torsion angles can be predicted for a larger, {>=}90 % fraction of the residues, with an error rate smaller than ca 3.5 %, using an acceptance criterion that is nearly two-fold tighter than that used previously, and a root mean square difference between predicted and crystallographically observed ({phi}, {psi}) torsion angles of ca 12 Masculine-Ordinal-Indicator . TALOS-N also reports sidechain {chi}{sup 1} rotameric states for about 50 % of the residues, and a consistency with reference structures of 89 %. The program includes a neural network trained to identify secondary structure from residue sequence and chemical shifts.

  15. 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)

  16. Variable-flip-angle spin-echo imaging (VFSE)

    International Nuclear Information System (INIS)

    Kasai, Toshifumi; Sugimura, Kazuro; Kawamitsu, Hideaki; Yasui, Kiyoshi; Ishida, Tetsuya; Tsukamoto, Tetsuji.

    1990-01-01

    T 2 weighted imaging provides images with high object contrast for pathologic conditions in which the water content of tissues is increased. The authors predicted theoretical analysis of the effects of changing flip angle, and analyzed the effects in MR imaging of both phantoms and humans. Variable flip angle spin echo MR imaging (VFSE) with a 1,000/80 (repetition time msec/echo time msec) can obtain T 2 weighted image when flip angle is smaller than 80 degrees. VFSE with 40 to 60 degrees flip angle have higher contrast than other flip angle images. Signal to noise ratio (S/N) of VFSE are 55% at a 30 degree, 76% at a 45 degree, 92% at a 60 degree respectively as compared with conventional spin echo image (2000/80, flip angle 90 degree). VFSE is applicable to obtain T 2 weighted image reduced imaging time. (author)

  17. TALOS+: a hybrid method for predicting protein backbone torsion angles from NMR chemical shifts

    Energy Technology Data Exchange (ETDEWEB)

    Shen Yang; Delaglio, Frank [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Cornilescu, Gabriel [National Magnetic Resonance Facility (United States); Bax, Ad [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)], E-mail: bax@nih.gov

    2009-08-15

    NMR chemical shifts in proteins depend strongly on local structure. The program TALOS establishes an empirical relation between {sup 13}C, {sup 15}N and {sup 1}H chemical shifts and backbone torsion angles {phi} and {psi} (Cornilescu et al. J Biomol NMR 13 289-302, 1999). Extension of the original 20-protein database to 200 proteins increased the fraction of residues for which backbone angles could be predicted from 65 to 74%, while reducing the error rate from 3 to 2.5%. Addition of a two-layer neural network filter to the database fragment selection process forms the basis for a new program, TALOS+, which further enhances the prediction rate to 88.5%, without increasing the error rate. Excluding the 2.5% of residues for which TALOS+ makes predictions that strongly differ from those observed in the crystalline state, the accuracy of predicted {phi} and {psi} angles, equals {+-}13{sup o}. Large discrepancies between predictions and crystal structures are primarily limited to loop regions, and for the few cases where multiple X-ray structures are available such residues are often found in different states in the different structures. The TALOS+ output includes predictions for individual residues with missing chemical shifts, and the neural network component of the program also predicts secondary structure with good accuracy.

  18. 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.

  19. Magic Angle Spinning NMR Structure Determination of Proteins from Pseudocontact Shifts

    KAUST Repository

    Li, Jianping; Pilla, Kala Bharath; Li, Qingfeng; Zhang, Zhengfeng; Su, Xuncheng; Huber, Thomas; Yang, Jun

    2013-01-01

    Magic angle spinning solid-state NMR is a unique technique to study atomic-resolution structure of biomacromolecules which resist crystallization or are too large to study by solution NMR techniques. However, difficulties in obtaining sufficient number of long-range distance restraints using dipolar coupling based spectra hamper the process of structure determination of proteins in solid-state NMR. In this study it is shown that high-resolution structure of proteins in solid phase can be determined without the use of traditional dipolar-dipolar coupling based distance restraints by combining the measurements of pseudocontact shifts (PCSs) with Rosetta calculations. The PCSs were generated by chelating exogenous paramagnetic metal ions to a tag 4-mercaptomethyl-dipicolinic acid, which is covalently attached to different residue sites in a 56-residue immunoglobulin-binding domain of protein G (GB1). The long-range structural restraints with metal-nucleus distance of up to ∼20 Å are quantitatively extracted from experimentally observed PCSs, and these are in good agreement with the distances back-calculated using an X-ray structure model. Moreover, we demonstrate that using several paramagnetic ions with varied paramagnetic susceptibilities as well as the introduction of paramagnetic labels at different sites can dramatically increase the number of long-range restraints and cover different regions of the protein. The structure generated from solid-state NMR PCSs restraints combined with Rosetta calculations has 0.7 Å root-mean-square deviation relative to X-ray structure. © 2013 American Chemical Society.

  20. Magic Angle Spinning NMR Structure Determination of Proteins from Pseudocontact Shifts

    KAUST Repository

    Li, Jianping

    2013-06-05

    Magic angle spinning solid-state NMR is a unique technique to study atomic-resolution structure of biomacromolecules which resist crystallization or are too large to study by solution NMR techniques. However, difficulties in obtaining sufficient number of long-range distance restraints using dipolar coupling based spectra hamper the process of structure determination of proteins in solid-state NMR. In this study it is shown that high-resolution structure of proteins in solid phase can be determined without the use of traditional dipolar-dipolar coupling based distance restraints by combining the measurements of pseudocontact shifts (PCSs) with Rosetta calculations. The PCSs were generated by chelating exogenous paramagnetic metal ions to a tag 4-mercaptomethyl-dipicolinic acid, which is covalently attached to different residue sites in a 56-residue immunoglobulin-binding domain of protein G (GB1). The long-range structural restraints with metal-nucleus distance of up to ∼20 Å are quantitatively extracted from experimentally observed PCSs, and these are in good agreement with the distances back-calculated using an X-ray structure model. Moreover, we demonstrate that using several paramagnetic ions with varied paramagnetic susceptibilities as well as the introduction of paramagnetic labels at different sites can dramatically increase the number of long-range restraints and cover different regions of the protein. The structure generated from solid-state NMR PCSs restraints combined with Rosetta calculations has 0.7 Å root-mean-square deviation relative to X-ray structure. © 2013 American Chemical Society.

  1. Pitch Angle Control for Variable Speed Wind Turbines

    DEFF Research Database (Denmark)

    Chen, Zhe; Zhang, Jianzhong; Cheng, M

    2008-01-01

    Pitch angle control is the most common means for adjusting the aerodynamic torque of the wind turbine when wind speed is above rated speed and various controlling variables may be chosen, such as wind speed, generator speed and generator power. As conventional pitch control usually use PI...... controller, the mathematical model of the system should be known well. A fuzzy logic pitch angle controller is developed in this paper, in which it does not need well known about the system and the mean wind speed is used to compensate the non-linear sensitivity. The fuzzy logic control strategy may have...... the potential when the system contains strong non-linearity, such as wind turbulence is strong, or the control objectives include fatigue loads. The design of the fuzzy logic controller and the comparisons with conversional pitch angle control strategies with various controlling variables are carried out...

  2. 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

  3. DRAMAtic transforms in magic angle spinning recoupling NMR: The Bessel function pathway.

    Science.gov (United States)

    Goodman, Russell; Hancock, Jason; Siemens, Mark; Jarrell, Harold; Siminovitch, David

    2005-07-01

    In magic angle spinning (MAS) NMR recoupling experiments, the extraction of multiple couplings or a coupling distribution from the observed dephasing signals remains a challenging problem. At least for REDOR experiments, the REDOR transform solves this problem, enabling the simultaneous measurement of multiple dipolar couplings. Focusing on the quadrupolar dephasing observed in QUADRAMA experiments as a representative example, we demonstrate that the same analytical form used for the mathematical description of REDOR dephasing also describes the dephasing observed in a wide variety of MAS NMR recoupling experiments. This fact immediately extends REDOR transform techniques to a much broader suite of recoupling experiments than had previously been realized, including those of DRAMA, MELODRAMA and QUADRAMA. As an illustration, we use the DRAMAtic transform to provide the first inversion of a QUADRAMA dephasing signal to extract the quadrupole coupling distribution. Using a complete elliptic integral of the first kind, we further develop a novel expression for the Pake-spun powder patterns of the corresponding recoupled lineshapes. Our methods and results reinforce the central role that Bessel functions can play in simplifying the integrals that define both the dephasing signals in the time domain, and their Fourier transforms in the frequency domain.

  4. 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.

  5. 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.

  6. Magic angle spinning NMR below 6 K with a computational fluid dynamics analysis of fluid flow and temperature gradients

    Science.gov (United States)

    Sesti, Erika L.; Alaniva, Nicholas; Rand, Peter W.; Choi, Eric J.; Albert, Brice J.; Saliba, Edward P.; Scott, Faith J.; Barnes, Alexander B.

    2018-01-01

    We report magic angle spinning (MAS) up to 8.5 kHz with a sample temperature below 6 K using liquid helium as a variable temperature fluid. Cross polarization 13C NMR spectra exhibit exquisite sensitivity with a single transient. Remarkably, 1H saturation recovery experiments show a 1H T1 of 21 s with MAS below 6 K in the presence of trityl radicals in a glassy matrix. Leveraging the thermal spin polarization available at 4.2 K versus 298 K should result in 71 times higher signal intensity. Taking the 1H longitudinal relaxation into account, signal averaging times are therefore predicted to be expedited by a factor of >500. Computer assisted design (CAD) and finite element analysis were employed in both the design and diagnostic stages of this cryogenic MAS technology development. Computational fluid dynamics (CFD) models describing temperature gradients and fluid flow are presented. The CFD models bearing and drive gas maintained at 100 K, while a colder helium variable temperature fluid stream cools the center of a zirconia rotor. Results from the CFD were used to optimize the helium exhaust path and determine the sample temperature. This novel cryogenic experimental platform will be integrated with pulsed dynamic nuclear polarization and electron decoupling to interrogate biomolecular structure within intact human cells.

  7. 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

  8. Action–angle variables, ladder operators and coherent states

    International Nuclear Information System (INIS)

    Campoamor-Stursberg, R.; Gadella, M.; Kuru, Ş.; Negro, J.

    2012-01-01

    This Letter is devoted to the building of coherent states from arguments based on classical action–angle variables. First, we show how these classical variables are associated to an algebraic structure in terms of Poisson brackets. In the quantum context these considerations are implemented by ladder type operators and a structure known as spectrum generating algebra. All this allows to generate coherent states and thereby the correspondence of classical–quantum properties by means of the aforementioned underlying structure. This approach is illustrated with the example of the one-dimensional Pöschl–Teller potential system. -- Highlights: ► We study the building of coherent states from classical action–angle variables arguments. ► The classical variables are associated to an algebraic structure in terms of Poisson brackets. ► In the quantum context these considerations are implemented by ladder type operators. ► All this allows to formulate coherent states and the correspondence of classical–quantum properties.

  9. Asymmetric-cut variable-incident-angle monochromator.

    Science.gov (United States)

    Smither, R K; Graber, T J; Fernandez, P B; Mills, D M

    2012-03-01

    A novel asymmetric-cut variable-incident-angle monochromator was constructed and tested in 1997 at the Advanced Photon Source of Argonne National Laboratory. The monochromator was originally designed as a high heat load monochromator capable of handling 5-10 kW beams from a wiggler source. This was accomplished by spreading the x-ray beam out on the surface an asymmetric-cut crystal and by using liquid metal cooling of the first crystal. The monochromator turned out to be a highly versatile monochromator that could perform many different types of experiments. The monochromator consisted of two 18° asymmetrically cut Si crystals that could be rotated about 3 independent axes. The first stage (Φ) rotates the crystal around an axis perpendicular to the diffraction plane. This rotation changes the angle of the incident beam with the surface of the crystal without changing the Bragg angle. The second rotation (Ψ) is perpendicular to the first and is used to control the shape of the beam footprint on the crystal. The third rotation (Θ) controls the Bragg angle. Besides the high heat load application, the use of asymmetrically cut crystals allows one to increase or decrease the acceptance angle for crystal diffraction of a monochromatic x-ray beam and allows one to increase or decrease the wavelength bandwidth of the diffraction of a continuum source like a bending-magnet beam or a normal x-ray-tube source. When the monochromator is used in the doubly expanding mode, it is possible to expand the vertical size of the double-diffracted beam by a factor of 10-15. When this was combined with a bending magnet source, it was possible to generate an 8 keV area beam, 16 mm wide by 26 mm high with a uniform intensity and parallel to 1.2 arc sec that could be applied in imaging experiments.

  10. Variability and Similarity of Gait as Evaluated by Joint Angles

    DEFF Research Database (Denmark)

    Yang, Sylvia X M; Larsen, Peter Kastmand; Alkjær, Tine

    2014-01-01

    . Six sets from 12 men were collected. For each man, a variability range VR (mean ± 1SD) of a specific joint angle at a specific time point (a gait cycle was 100 time points) was calculated. In turn, each individual was compared with the 11 others, and whenever 1 of these 11 had a value within...... this individual’s VR, it counted as positive. By adding the positives throughout the gait cycle, we created simple bar graphs; tall bars indicated a small discriminatory power, short bars indicated a larger one. The highest discriminatory power was at time points 60–80 in the gait cycle. We show how our data can...

  11. 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.

  12. Magic-angle spinning NMR of a class I filamentous bacteriophage virus.

    Science.gov (United States)

    Abramov, Gili; Morag, Omry; Goldbourt, Amir

    2011-08-11

    The fd bacteriophage is a filamentous virus that is widely used for bio- and nanotechnology applications ranging from phage display to battery materials. The possibility of obtaining a detailed description of its structural properties regardless of its state is therefore essential not only for understanding its physical arrangement and its bacterial infection process but also for many other applications. Here we present a study of the fd phage by magic-angle spinning solid-state NMR. While current structures rely on a Y21M mutant, experiments performed on a strain bearing a wild-type capsid report on high symmetry of the phage and lack of explicit subunit polymorphism. Chemical shift analysis confirmed that the coat protein mostly consists of a rigid right-handed curved α-helix (residues 6-47 of 50), preceded by a flexible loop-structured N-terminus. We were able to qualitatively assign the resonances belonging to the DNA, including the deoxyribose sugars and the thymine bases. These chemical shifts are consistent with base stacking and a C2'-endo/C3'-exo sugar pucker. © 2011 American Chemical Society

  13. NMR longitudinal relaxation enhancement in metal halides by heteronuclear polarization exchange during magic-angle spinning

    Energy Technology Data Exchange (ETDEWEB)

    Shmyreva, Anna A. [Center for Magnetic Resonance, St. Petersburg State University, St. Petersburg 198504 (Russian Federation); Safdari, Majid; Furó, István [Department of Chemistry, KTH Royal Institute of Technology, SE-10044 Stockholm (Sweden); Dvinskikh, Sergey V., E-mail: sergeid@kth.se [Department of Chemistry, KTH Royal Institute of Technology, SE-10044 Stockholm (Sweden); Laboratory of Biomolecular NMR, St. Petersburg State University, St. Petersburg 199034 (Russian Federation)

    2016-06-14

    Orders of magnitude decrease of {sup 207}Pb and {sup 199}Hg NMR longitudinal relaxation times T{sub 1} upon magic-angle-spinning (MAS) are observed and systematically investigated in solid lead and mercury halides MeX{sub 2} (Me = Pb, Hg and X = Cl, Br, I). In lead(II) halides, the most dramatic decrease of T{sub 1} relative to that in a static sample is in PbI{sub 2}, while it is smaller but still significant in PbBr{sub 2}, and not detectable in PbCl{sub 2}. The effect is magnetic-field dependent but independent of the spinning speed in the range 200–15 000 Hz. The observed relaxation enhancement is explained by laboratory-frame heteronuclear polarization exchange due to crossing between energy levels of spin-1/2 metal nuclei and adjacent quadrupolar-spin halogen nuclei. The enhancement effect is also present in lead-containing organometal halide perovskites. Our results demonstrate that in affected samples, it is the relaxation data recorded under non-spinning conditions that characterize the local properties at the metal sites. A practical advantage of fast relaxation at slow MAS is that spectral shapes with orientational chemical shift anisotropy information well retained can be acquired within a shorter experimental time.

  14. Variable-temperature NMR and conformational analysis of Oenothein B

    International Nuclear Information System (INIS)

    Santos, Suzana C.; Carvalho, Ariadne G.; Fortes, Gilmara A.C.; Ferri, Pedro H.; Oliveira, Anselmo E. de

    2014-01-01

    Oenothein B is a dimeric hydrolyzable tannin with a wide range of biological activities, such as antitumour, anti-inflammatory and antiviral. Its nuclear magnetic resonance (NMR) at room temperature show duplications and broadening of signals. Experiments of 1D and 2D NMR at lower temperatures were useful for the complete NMR assignments of all hydrogens and carbons. The 3D structure of the most stable conformer was determined for the first time by nuclear Overhauser effect spectroscopy (NOESY) experiment (-20 deg C) and density functional theory (DFT)(B3LYP/6-31G)/ polarizable continuum model (PCM) quantum chemical calculations. The favoured conformation showed a highly compacted geometry and a lack of symmetry, in which the two valoneoyl groups showed distinct conformational parameters and stabilities. (author)

  15. Variable-temperature NMR and conformational analysis of Oenothein B

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Suzana C.; Carvalho, Ariadne G.; Fortes, Gilmara A.C.; Ferri, Pedro H.; Oliveira, Anselmo E. de, [Universidade Federal de Goias (UFGO), Goiania, GO (Brazil). Instituto de Quimica

    2014-02-15

    Oenothein B is a dimeric hydrolyzable tannin with a wide range of biological activities, such as antitumour, anti-inflammatory and antiviral. Its nuclear magnetic resonance (NMR) at room temperature show duplications and broadening of signals. Experiments of 1D and 2D NMR at lower temperatures were useful for the complete NMR assignments of all hydrogens and carbons. The 3D structure of the most stable conformer was determined for the first time by nuclear Overhauser effect spectroscopy (NOESY) experiment (-20 deg C) and density functional theory (DFT)(B3LYP/6-31G)/ polarizable continuum model (PCM) quantum chemical calculations. The favoured conformation showed a highly compacted geometry and a lack of symmetry, in which the two valoneoyl groups showed distinct conformational parameters and stabilities. (author)

  16. Characterization of lithium coordination sites with magic-angle spinning NMR

    Science.gov (United States)

    Haimovich, A.; Goldbourt, A.

    2015-05-01

    Lithium, in the form of lithium carbonate, is one of the most common drugs for bipolar disorder. Lithium is also considered to have an effect on many other cellular processes hence it possesses additional therapeutic as well as side effects. In order to quantitatively characterize the binding mode of lithium, it is required to identify the interacting species and measure their distances from the metal center. Here we use magic-angle spinning (MAS) solid-state NMR to study the binding site of lithium in complex with glycine and water (LiGlyW). Such a compound is a good enzyme mimetic since lithium is four-coordinated to one water molecule and three carboxylic groups. Distance measurements to carbons are performed using a 2D transferred echo double resonance (TEDOR) MAS solid-state NMR experiment, and water binding is probed by heteronuclear high-resolution proton-lithium and proton-carbon correlation (wPMLG-HETCOR) experiments. Both HETCOR experiments separate the main complex from impurities and non-specifically bound lithium species, demonstrating the sensitivity of the method to probe the species in the binding site. Optimizations of the TEDOR pulse scheme in the case of a quadrupolar nucleus with a small quadrupole coupling constant show that it is most efficient when pulses are positioned on the spin-1/2 (carbon-13) nucleus. Since the intensity of the TEDOR signal is not normalized, careful data analysis that considers both intensity and dipolar oscillations has to be performed. Nevertheless we show that accurate distances can be extracted for both carbons of the bound glycine and that these distances are consistent with the X-ray data and with lithium in a tetrahedral environment. The lithium environment in the complex is very similar to the binding site in inositol monophosphatase, an enzyme associated with bipolar disorder and the putative target for lithium therapy. A 2D TEDOR experiment applied to the bacterial SuhB gene product of this enzyme was designed

  17. Indirectly detected chemical shift correlation NMR spectroscopy in solids under fast magic angle spinning

    Energy Technology Data Exchange (ETDEWEB)

    Mao, Kanmi [Iowa State Univ., Ames, IA (United States)

    2011-01-01

    The development of fast magic angle spinning (MAS) opened up an opportunity for the indirect detection of insensitive low-γ nuclei (e.g., 13C and 15N) via the sensitive high-{gamma} nuclei (e.g., 1H and 19F) in solid-state NMR, with advanced sensitivity and resolution. In this thesis, new methodology utilizing fast MAS is presented, including through-bond indirectly detected heteronuclear correlation (HETCOR) spectroscopy, which is assisted by multiple RF pulse sequences for 1H-1H homonuclear decoupling. Also presented is a simple new strategy for optimization of 1H-1H homonuclear decoupling. As applications, various classes of materials, such as catalytic nanoscale materials, biomolecules, and organic complexes, are studied by combining indirect detection and other one-dimensional (1D) and two-dimensional (2D) NMR techniques. Indirectly detected through-bond HETCOR spectroscopy utilizing refocused INEPT (INEPTR) mixing was developed under fast MAS (Chapter 2). The time performance of this approach in 1H detected 2D 1H{l_brace}13C{r_brace} spectra was significantly improved, by a factor of almost 10, compared to the traditional 13C detected experiments, as demonstrated by measuring naturally abundant organic-inorganic mesoporous hybrid materials. The through-bond scheme was demonstrated as a new analytical tool, which provides complementary structural information in solid-state systems in addition to through-space correlation. To further benefit the sensitivity of the INEPT transfer in rigid solids, the combined rotation and multiple-pulse spectroscopy (CRAMPS) was implemented for homonuclear 1H decoupling under fast MAS (Chapter 3). Several decoupling schemes (PMLG5m$\\bar{x}$, PMLG5mm$\\bar{x}$x and SAM3) were analyzed to maximize the performance of through-bond transfer based

  18. Si-O-Si bond-angle distribution in vitreous silica from first-principles 29Si NMR analysis

    International Nuclear Information System (INIS)

    Mauri, Francesco; Pasquarello, Alfredo; Pfrommer, Bernd G.; Yoon, Young-Gui; Louie, Steven G.

    2000-01-01

    The correlation between 29 Si chemical shifts and Si-O-Si bond angles in SiO 2 is determined within density-functional theory for the full range of angles present in vitreous silica. This relation closely reproduces measured shifts of crystalline polymorphs. The knowledge of the correlation allows us to reliably extract from the experimental NMR spectrum the mean (151 degree sign ) and the standard deviation (11 degree sign ) of the Si-O-Si angular distribution of vitreous silica. In particular, we show that the Mozzi-Warren Si-O-Si angular distribution is not consistent with the NMR data. This analysis illustrates the potential of our approach for structural determinations of silicate glasses. (c) 2000 The American Physical Society

  19. Morphology of fast-tumbling bicelles: a small angle neutron scattering and NMR study.

    Science.gov (United States)

    Luchette, P A; Vetman, T N; Prosser, R S; Hancock, R E; Nieh, M P; Glinka, C J; Krueger, S; Katsaras, J

    2001-08-06

    Bilayered micelles, or bicelles, which consist of a mixture of long- and short-chain phospholipids, are a popular model membrane system. Depending on composition, concentration, and temperature, bicelle mixtures may adopt an isotropic phase or form an aligned phase in magnetic fields. Well-resolved (1)H NMR spectra are observed in the isotropic or so-called fast-tumbling bicelle phase, over the range of temperatures investigated (10-40 degrees C), for molar ratios of long-chain lipid to short-chain lipid between 0.20 and 1.0. Small angle neutron scattering data of this phase are consistent with the model in which bicelles were proposed to be disk-shaped. The experimentally determined dimensions are roughly consistent with the predictions of R.R. Vold and R.S. Prosser (J. Magn. Reson. B 113 (1996)). Differential paramagnetic shifts of head group resonances of dimyristoylphosphatidylcholine (DMPC) and dihexanoylphosphatidylcholine (DHPC), induced by the addition of Eu(3+), are also consistent with the bicelle model in which DHPC is believed to be primarily sequestered to bicelle rims. Selective irradiation of the DHPC aliphatic methyl resonances results in no detectable magnetization transfer to the corresponding DMPC methyl resonances (and vice versa) in bicelles, which also suggests that DHPC and DMPC are largely sequestered in the bicelle. Finally, (1)H spectra of the antibacterial peptide indolicidin (ILPWKWPWWPWRR-NH(2)) are compared, in a DPC micellar phase and the above fast-tumbling bicellar phases for a variety of compositions. The spectra exhibit adequate resolution and improved dispersion of amide and aromatic resonances in certain bicelle mixtures.

  20. Biplanar variable angle x-ray examining apparatus

    International Nuclear Information System (INIS)

    Grady, J.K.

    1986-01-01

    This invention relates to radiological equipment, particularly to apparatus for supporting and maneuvering a plurality of radiological examination sets to permit simultaneous or sequential exposure through different planes of an organ. The apparatus comprises: a first radiological examining set including a radiation source, receptor, and support for holding the source and receptor along an axis; and a second examining set with the source and receptor aligned to intersect the first axis at a common isocenter. The first support means is rotatable independently of the second support means about a rotational axis intersecting the common isocenter. The support means for one radiological examining set comprises two arms respectively carrying the radiation source and the radiation receptor of the one set and means reciprocally supporting the respective arms for movement independently of each other parallel to the rotational axis, whereby a series of substantially simultaneous radiological examinations can be made on both radiation axes through the subject at variable angles between the axes

  1. A solvable Hamiltonian system: Integrability and action-angle variables

    International Nuclear Information System (INIS)

    Karimipour, V.

    1997-01-01

    We prove that the dynamical system characterized by the Hamiltonian H=λN summation j N p j +μ summation j,k N (p j p k ) 1/2 {cos[ν(q j -q k )]} proposed and studied by Calogero [J. Math. Phys. 36, 9 (1994)] and Calogero and van Diejen [Phys. Lett. A 205, 143 (1995)] is equivalent to a system of noninteracting harmonic oscillators both classically and quantum mechanically. We find the explicit form of the conserved currents that are in involution. We also find the action-angle variables and solve the initial value problem in a very simple form.copyright 1997 American Institute of Physics

  2. Permanent magnet assembly producing a strong tilted homogeneous magnetic field: towards magic angle field spinning NMR and MRI.

    Science.gov (United States)

    Sakellariou, Dimitris; Hugon, Cédric; Guiga, Angelo; Aubert, Guy; Cazaux, Sandrine; Hardy, Philippe

    2010-12-01

    We introduce a cylindrical permanent magnet design that generates a homogeneous and strong magnetic field having an arbitrary inclination with respect to the axis of the cylinder. The analytical theory of 3 D magnetostatics has been applied to this problem, and a hybrid magnet structure has been designed. This structure contains two magnets producing a longitudinal and transverse component for the magnetic field, whose amplitudes and homogeneities can be fully controlled by design. A simple prototype has been constructed using inexpensive small cube magnets, and its magnetic field has been mapped using Hall and NMR probe sensors. This magnet can, in principle, be used for magic angle field spinning NMR and MRI experiments allowing for metabolic chemical shift profiling in small living animals. Copyright © 2010 John Wiley & Sons, Ltd.

  3. 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.

  4. 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

  5. High Resolution Magic Angle Spinning Nuclear Magnetic Resonance (HRMAS NMR) for Studies of Reactive Fabrics

    Science.gov (United States)

    2015-11-01

    spectroscopy (NMR) Self- decontaminating fabric Reactive fabric...reactions of reagents including chemical weapons on materials like concrete, soil , and sand, as well as reactive polymers.3,4,5,6,7 There are...sample. The rotor and cap can be cleaned by rinsing with solvent or decontamination solution and reused. 12.0 DATA ANALYSIS AND CALCULATIONS 12.1

  6. Structural changes in C–S–H gel during dissolution: Small-angle neutron scattering and Si-NMR characterization

    Energy Technology Data Exchange (ETDEWEB)

    Trapote-Barreira, Ana, E-mail: anatrapotebarreira@gmail.com [Institute of Environmental Assessment and Water Research (IDAEA), Barcelona 08034, Catalonia (Spain); Porcar, Lionel [National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899 (United States); Large Scale Structure Group, Institut Laue Langevin, Grenoble (France); Cama, Jordi; Soler, Josep M. [Institute of Environmental Assessment and Water Research (IDAEA), Barcelona 08034, Catalonia (Spain); Allen, Andrew J. [National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899 (United States)

    2015-06-15

    Flow-through experiments were conducted to study the calcium–silicate–hydrate (C–S–H) gel dissolution kinetics. During C–S–H gel dissolution the initial aqueous Ca/Si ratio decreases to reach the stoichiometric value of the Ca/Si ratio of a tobermorite-like phase (Ca/Si = 0.83). As the Ca/Si ratio decreases, the solid C–S–H dissolution rate increases from (4.5 × 10{sup −} {sup 14} to 6.7 × 10{sup −} {sup 12}) mol m{sup −} {sup 2} s{sup −} {sup 1}. The changes in the microstructure of the dissolving C–S–H gel were characterized by small-angle neutron scattering (SANS) and {sup 29}Si magic-angle-spinning nuclear magnetic resonance ({sup 29}Si-MAS NMR). The SANS data were fitted using a fractal model. The SANS specific surface area tends to increase with time and the obtained fit parameters reflect the changes in the nanostructure of the dissolving solid C–S–H within the gel. The {sup 29}Si MAS NMR analyses show that with dissolution the solid C–S–H structure tends to a more ordered tobermorite structure, in agreement with the Ca/Si ratio evolution.

  7. Resonance Assignments and Secondary Structure Analysis of Dynein Light Chain 8 by Magic-angle Spinning NMR Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Shangjin; Butterworth, Andrew H.; Paramasivam, Sivakumar; Yan, Si; Lightcap, Christine M.; Williams, John C.; Polenova, Tatyana E.

    2011-08-04

    Dynein light chain LC8 is the smallest subunit of the dynein motor complex and has been shown to play important roles in both dynein-dependent and dynein-independent physiological functions via its interaction with a number of its binding partners. It has also been linked to pathogenesis including roles in viral infections and tumorigenesis. Structural information for LC8-target proteins is critical to understanding the underlying function of LC8 in these complexes. However, some LC8-target interactions are not amenable to structural characterization by conventional structural biology techniques owing to their large size, low solubility, and crystallization difficulties. Here, we report magic-angle spinning (MAS) NMR studies of the homodimeric apo-LC8 protein as a first effort in addressing more complex, multi-partner, LC8-based protein assemblies. We have established site-specific backbone and side-chain resonance assignments for the majority of the residues of LC8, and show TALOS+-predicted torsion angles ø and ψ in close agreement with most residues in the published LC8 crystal structure. Data obtained through these studies will provide the first step toward using MAS NMR to examine the LC8 structure, which will eventually be used to investigate protein–protein interactions in larger systems that cannot be determined by conventional structural studies.

  8. Vacuum variable-angle far-infrared ellipsometer

    Science.gov (United States)

    Friš, Pavel; Dubroka, Adam

    2017-11-01

    We present the design and performance of a vacuum far-infrared (∼50-680 cm-1) ellipsometer with a rotating analyser. The system is based on a Fourier transform spectrometer, an in-house built ellipsometer chamber and a closed-cycle bolometer. The ellipsometer chamber is equipped with a computer controlled θ-2θ goniometer for automated measurements at various angles of incidence. We compare our measurements on SrTiO3 crystal with the results acquired above 300 cm-1 with a commercially available ellipsometer system. After the calibration of the angle of incidence and after taking into account the finite reflectivity of mirrors in the detector part we obtain a very good agreement between the data from the two instruments. The system can be supplemented with a closed-cycle He cryostat for measurements between 5 and 400 K.

  9. Pitch Angle Control for Variable Speed Wind Turbines

    Directory of Open Access Journals (Sweden)

    Mouna Ben Smida

    2015-08-01

    Full Text Available Abstract.Pitch control is a practical technique for power regulation above the rated wind speed it is considered as the most efficient and popular power control method. As conventional pitch control usually use PI controller, the mathematical model of the system should be known well.This paper deals with the operation and the control of the direct driven permanent magnet synchronous generator (PMSG.Different conventional strategies of pitch angle control are described and validated through simulation results under Matlab\\Simulink.

  10. Magic-Angle-Spinning NMR Magnet Development: Field Analysis and Prototypes

    Science.gov (United States)

    Voccio, John; Hahn, Seungyong; Park, Dong Keun; Ling, Jiayin; Kim, Youngjae; Bascuñán, Juan; Iwasa, Yukikazu

    2013-01-01

    We are currently working on a program to complete a 1.5 T/75 mm RT bore magic-angle-spinning nuclear magnetic resonance magnet. The magic-angle-spinning magnet comprises a z-axis 0.866-T solenoid and an x-axis 1.225-T dipole, each to be wound with NbTi wire and operated at 4.2 K in persistent mode. A combination of the fields creates a 1.5-T field pointed at 54.74 degrees (magic angle) from the rotation (z) axis. In the first year of this 3-year program, we have completed magnetic analysis and design of both coils. Also, using a winding machine of our own design and fabrication, we have wound several prototype dipole coils with NbTi wire. As part of this development, we have repeatedly made successful persistent NbTi-NbTi joints with this multifilamentary NbTi wire. PMID:24058275

  11. Measurements of relative chemical shift tensor orientations in solid-state NMR: new slow magic angle spinning dipolar recoupling experiments.

    Science.gov (United States)

    Jurd, Andrew P S; Titman, Jeremy J

    2009-08-28

    Solid-state NMR experiments can be used to determine conformational parameters, such as interatomic distances and torsion angles. The latter can be obtained from measurements of the relative orientation of two chemical shift tensors, if the orientation of these with respect to the surrounding bonds is known. In this paper, a new rotor-synchronized magic angle spinning (MAS) dipolar correlation experiment is described which can be used in this way. Because the experiment requires slow MAS rates, a novel recoupling sequence, designed using symmetry principles, is incorporated into the mixing period. This recoupling sequence is based in turn on a new composite cyclic pulse referred to as COAST (for combined offset and anisotropy stabilization). The new COAST-C7(2)(1) sequence is shown to give good theoretical and experimental recoupling efficiency, even when the CSA far exceeds the MAS rate. In this regime, previous recoupling sequences, such as POST-C7(2)(1), exhibit poor recoupling performance. The effectiveness of the new method has been explored by a study of the dipeptide L-phenylalanyl-L-phenylalanine.

  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. Action-angle variable for the Gel'fand-Dikii flows

    International Nuclear Information System (INIS)

    Beals, R.; Sattinger, D.H.

    1992-01-01

    Using the scattering transform for nth order linear scalar operators, the Poisson bracket found by Gel'fans and Dikii, which generalizes the Gardner Poisson bracket for the KdV hierarchy, is computed on the scattering side. Action-angle variables are then constructed. Using this, complete integrability is demonstrated in the strong sense. Real action-angle variables are constructed in the self-adjoint case. (orig.)

  14. Application of High-Resolution Magic-Angle Spinning NMR Spectroscopy to Define the Cell Uptake of MRI Contrast Agents

    Science.gov (United States)

    Calabi, Luisella; Alfieri, Goffredo; Biondi, Luca; De Miranda, Mario; Paleari, Lino; Ghelli, Stefano

    2002-06-01

    A new method, based on proton high-resolution magic-angle spinning ( 1H HR-MAS) NMR spectroscopy, has been employed to study the cell uptake of magnetic resonance imaging contrast agents (MRI-CAs). The method was tested on human red blood cells (HRBC) and white blood cells (HWBC) by using three gadolinium complexes, widely used in diagnostics, Gd-BOPTA, Gd-DTPA, and Gd-DOTA, and the analogous complexes obtained by replacing Gd(III) with Dy(III), Nd(III), and Tb(III) (i.e., complexes isostructural to the ones of gadolinium but acting as shift agents). The method is based on the evaluation of the magnetic effects, line broadening, or induced lanthanide shift (LIS) caused by these complexes on NMR signals of intra- and extracellular water. Since magnetic effects are directly linked to permeability, this method is direct. In all the tests, these magnetic effects were detected for the extracellular water signal only, providing a direct proof that these complexes are not able to cross the cell membrane. Line broadening effects (i.e., the use of gadolinium complexes) only allow qualitative evaluations. On the contrary, LIS effects can be measured with high precision and they can be related to the concentration of the paramagnetic species in the cellular compartments. This is possible because the HR-MAS technique provides the complete elimination of bulk magnetic susceptibility (BMS) shift and the differentiation of extra- and intracellular water signals. Thus with this method, the rapid quantification of the MRI-CA amount inside and outside the cells is actually feasible.

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

    KAUST Repository

    Parthasarathy, Sudhakar

    2013-09-17

    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 in this area by presenting (13)C and (1)H solid-state NMR (SSNMR) studies on paramagnetic systems and biomolecules under fast MAS from our laboratories. First, we describe how very fast MAS (VFMAS) at the spinning speed of at least 20 kHz allows us to overcome major difficulties in (1)H and (13)C high-resolution SSNMR of paramagnetic systems. As a result, we can enhance both sensitivity and resolution by up to a few orders of magnitude. Using fast recycling (∼ms/scan) with short (1)H T1 values, we can perform (1)H SSNMR microanalysis of paramagnetic systems on the microgram scale with greatly improved sensitivity over that observed for diamagnetic systems. Second, we discuss how VFMAS at a spinning speed greater than ∼40 kHz can enhance the sensitivity and resolution of (13)C biomolecular SSNMR measurements. Low-power (1)H decoupling schemes under VFMAS offer excellent spectral resolution for (13)C SSNMR by nominal (1)H RF irradiation at ∼10 kHz. By combining the VFMAS approach with enhanced (1)H T1 relaxation by paramagnetic doping, we can achieve extremely fast recycling in modern biomolecular SSNMR experiments. Experiments with (13)C-labeled ubiquitin doped with 10 mM Cu-EDTA demonstrate how effectively this new approach, called paramagnetic assisted condensed data collection (PACC), enhances the sensitivity. Lastly, we examine (13)C SSNMR measurements for biomolecules under faster MAS at a higher field. Our preliminary (13)C SSNMR data of Aβ amyloid fibrils and GB1 microcrystals acquired at (1)H NMR frequencies of 750-800 MHz suggest that the combined use of the PACC approach and ultrahigh fields could allow for routine multidimensional SSNMR analyses of proteins at the 50-200 nmol level. Also, we briefly discuss the

  16. The determinants of bond angle variability in protein/peptide backbones: A comprehensive statistical/quantum mechanics analysis.

    Science.gov (United States)

    Improta, Roberto; Vitagliano, Luigi; Esposito, Luciana

    2015-11-01

    The elucidation of the mutual influence between peptide bond geometry and local conformation has important implications for protein structure refinement, validation, and prediction. To gain insights into the structural determinants and the energetic contributions associated with protein/peptide backbone plasticity, we here report an extensive analysis of the variability of the peptide bond angles by combining statistical analyses of protein structures and quantum mechanics calculations on small model peptide systems. Our analyses demonstrate that all the backbone bond angles strongly depend on the peptide conformation and unveil the existence of regular trends as function of ψ and/or φ. The excellent agreement of the quantum mechanics calculations with the statistical surveys of protein structures validates the computational scheme here employed and demonstrates that the valence geometry of protein/peptide backbone is primarily dictated by local interactions. Notably, for the first time we show that the position of the H(α) hydrogen atom, which is an important parameter in NMR structural studies, is also dependent on the local conformation. Most of the trends observed may be satisfactorily explained by invoking steric repulsive interactions; in some specific cases the valence bond variability is also influenced by hydrogen-bond like interactions. Moreover, we can provide a reliable estimate of the energies involved in the interplay between geometry and conformations. © 2015 Wiley Periodicals, Inc.

  17. Selectively dispersed isotope labeling for protein structure determination by magic angle spinning NMR

    Energy Technology Data Exchange (ETDEWEB)

    Eddy, Matthew T. [Massachusetts Institute of Technology, Department of Chemistry (United States); Belenky, Marina [Brandeis University, Department of Chemistry (United States); Sivertsen, Astrid C. [Massachusetts Institute of Technology, Francis Bitter Magnet Laboratory (United States); Griffin, Robert G. [Massachusetts Institute of Technology, Department of Chemistry (United States); Herzfeld, Judith, E-mail: herzfeld@brandeis.edu [Brandeis University, Department of Chemistry (United States)

    2013-10-15

    The power of nuclear magnetic resonance spectroscopy derives from its site-specific access to chemical, structural and dynamic information. However, the corresponding multiplicity of interactions can be difficult to tease apart. Complimentary approaches involve spectral editing on the one hand and selective isotope substitution on the other. Here we present a new 'redox' approach to the latter: acetate is chosen as the sole carbon source for the extreme oxidation numbers of its two carbons. Consistent with conventional anabolic pathways for the amino acids, [1-{sup 13}C] acetate does not label {alpha} carbons, labels other aliphatic carbons and the aromatic carbons very selectively, and labels the carboxyl carbons heavily. The benefits of this labeling scheme are exemplified by magic angle spinning spectra of microcrystalline immunoglobulin binding protein G (GB1): the elimination of most J-couplings and one- and two-bond dipolar couplings provides narrow signals and long-range, intra- and inter-residue, recoupling essential for distance constraints. Inverse redox labeling, from [2-{sup 13}C] acetate, is also expected to be useful: although it retains one-bond couplings in the sidechains, the removal of CA-CO coupling in the backbone should improve the resolution of NCACX spectra.

  18. An oilspill trajectory analysis model with a variable wind deflection angle

    Science.gov (United States)

    Samuels, W.B.; Huang, N.E.; Amstutz, D.E.

    1982-01-01

    The oilspill trajectory movement algorithm consists of a vector sum of the surface drift component due to wind and the surface current component. In the U.S. Geological Survey oilspill trajectory analysis model, the surface drift component is assumed to be 3.5% of the wind speed and is rotated 20 degrees clockwise to account for Coriolis effects in the Northern Hemisphere. Field and laboratory data suggest, however, that the deflection angle of the surface drift current can be highly variable. An empirical formula, based on field observations and theoretical arguments relating wind speed to deflection angle, was used to calculate a new deflection angle at each time step in the model. Comparisons of oilspill contact probabilities to coastal areas calculated for constant and variable deflection angles showed that the model is insensitive to this changing angle at low wind speeds. At high wind speeds, some statistically significant differences in contact probabilities did appear. ?? 1982.

  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. Assessment of metabolic phenotypic variability in children’s urine using 1H NMR spectroscopy

    Science.gov (United States)

    Maitre, Léa; Lau, Chung-Ho E.; Vizcaino, Esther; Robinson, Oliver; Casas, Maribel; Siskos, Alexandros P.; Want, Elizabeth J.; Athersuch, Toby; Slama, Remy; Vrijheid, Martine; Keun, Hector C.; Coen, Muireann

    2017-04-01

    The application of metabolic phenotyping in clinical and epidemiological studies is limited by a poor understanding of inter-individual, intra-individual and temporal variability in metabolic phenotypes. Using 1H NMR spectroscopy we characterised short-term variability in urinary metabolites measured from 20 children aged 8-9 years old. Daily spot morning, night-time and pooled (50:50 morning and night-time) urine samples across six days (18 samples per child) were analysed, and 44 metabolites quantified. Intraclass correlation coefficients (ICC) and mixed effect models were applied to assess the reproducibility and biological variance of metabolic phenotypes. Excellent analytical reproducibility and precision was demonstrated for the 1H NMR spectroscopic platform (median CV 7.2%). Pooled samples captured the best inter-individual variability with an ICC of 0.40 (median). Trimethylamine, N-acetyl neuraminic acid, 3-hydroxyisobutyrate, 3-hydroxybutyrate/3-aminoisobutyrate, tyrosine, valine and 3-hydroxyisovalerate exhibited the highest stability with over 50% of variance specific to the child. The pooled sample was shown to capture the most inter-individual variance in the metabolic phenotype, which is of importance for molecular epidemiology study design. A substantial proportion of the variation in the urinary metabolome of children is specific to the individual, underlining the potential of such data to inform clinical and exposome studies conducted early in life.

  1. 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

  2. Action-angle variables for the harmonic oscillator : ambiguity spin x duplication spin

    International Nuclear Information System (INIS)

    Oliveira, C.R. de; Malta, C.P.

    1983-08-01

    The difficulties of obtaining for the harmonic oscillator a well defined unitary transformation to action-angle variables were overcome by M. Moshinsky and T.H. Seligman through the introduction of a spinlike variable (ambiguity spin) from a classical point of view. The difficulty of defining a unitary phase operator for the harmonic oscillator was overcome by Roger G. Newton also through the introduction of a spinlike variable (named duplication spin by us) but within a quantum framework. The relation between the ambiguity spin and the duplication spin by introducing these two types of spins in the canonical transformation to action-angle variables is investigated. Doing this it is possible to obtain both well defined unitary transformation and phase operator. (Author) [pt

  3. Light refraction in sapphire plates with a variable angle of crystal optical axis to the surface

    International Nuclear Information System (INIS)

    Vetrov, V. N.; Ignatenkov, B. A.

    2013-01-01

    The modification of sapphire by inhomogeneous plastic deformation makes it possible to obtain plates with a variable angle of inclination of the crystal optical axis to the plate surface. The refraction of light in this plate at perpendicular and oblique incidence of a parallel beam of rays is considered. The algorithm of calculating the refractive index of extraordinary ray and the birefringence is proposed.

  4. Spatial resolution properties in 3D fast spin-echo using variable refocusing flip angles

    International Nuclear Information System (INIS)

    Ozaki, Masanori; Mizukami, Shinya; Hata, Hirofumi; Sato, Mayumi; Komi, Syotaro; Miyati, Tosiaki; Nozaki, Atsushi

    2011-01-01

    A new 3-dimensional fast spin-echo (3D FSE) method that uses a variable refocusing flip angle technique has recently been applied to imaging. The imaging pulse sequence can inhibit T 2 decay by varying the refocusing flip angle. Use of a long echo train length allows acquisition of 3D T 2 -weighted images with less blurring in a short scan time. The smaller refocusing flip angle in the new 3D FSE method than in the conventional method can reduce the specific absorption rate. However, T 2 decay differs between the new and conventional 3D FSE methods, so the resolution properties of the 2 methods may differ. We investigated the resolution properties of the new 3D FSE method using a variable refocusing flip angle technique. Varying the refocusing flip angle resulted in different resolution properties for the new 3D FSE method compared to the conventional method, a difference particularly noticeable when the imaging parameters were set for obtaining proton density weighted images. (author)

  5. UV-Vis reflection spectroscopy under variable angle incidence at the air-liquid interface.

    Science.gov (United States)

    Roldán-Carmona, Cristina; Rubia-Payá, Carlos; Pérez-Morales, Marta; Martín-Romero, María T; Giner-Casares, Juan J; Camacho, Luis

    2014-03-07

    The UV-Vis reflection spectroscopy (UV-Vis-RS) in situ at the air-liquid interface provides information about tilt and aggregation of chromophores in Langmuir monolayers. This information is particularly important given in most cases the chromophore is located at the polar region of the Langmuir monolayer. This region of the Langmuir monolayers has been hardly accessible by other experimental techniques. In spite of its enormous potential, the application of UV-Vis-RS has been limited mainly to reflection measurements under light normal incidence or at lower incidence angles than the Brewster angle. Remarkably, this technique is quite sensitive to the tilt of the chromophores at values of incidence angles close to or larger than the Brewster angle. Therefore, a novel method to obtain the order parameter of the chromophores at the air-liquid interface by using s- and p-polarized radiation at different incidence angles is proposed. This method allowed for the first time the experimental observation of the two components with different polarization properties of a single UV-Vis band at the air-liquid interface. The method of UV-Vis spectroscopy under variable angle incidence is presented as a new tool for obtaining rich detailed information on Langmuir monolayers.

  6. Variable-angle total internal reflection fluorescence microscopy of intact cells of Arabidopsis thaliana

    Directory of Open Access Journals (Sweden)

    Kim Myung K

    2011-09-01

    Full Text Available Abstract Background Total internal reflection fluorescence microscopy (TIRFM is a powerful tool for observing fluorescently labeled molecules on the plasma membrane surface of animal cells. However, the utility of TIRFM in plant cell studies has been limited by the fact that plants have cell walls, thick peripheral layers surrounding the plasma membrane. Recently, a new technique known as variable-angle epifluorescence microscopy (VAEM was developed to circumvent this problem. However, the lack of a detailed analysis of the optical principles underlying VAEM has limited its applications in plant-cell biology. Results Here, we present theoretical and experimental evidence supporting the use of variable-angle TIRFM in observations of intact plant cells. We show that when total internal reflection occurs at the cell wall/cytosol interface with an appropriate angle of incidence, an evanescent wave field of constant depth is produced inside the cytosol. Results of experimental TIRFM observations of the dynamic behaviors of phototropin 1 (a membrane receptor protein and clathrin light chain (a vesicle coat protein support our theoretical analysis. Conclusions These findings demonstrate that variable-angle TIRFM is appropriate for quantitative live imaging of cells in intact tissues of Arabidopsis thaliana.

  7. Kinematics of a vertical axis wind turbine with a variable pitch angle

    Science.gov (United States)

    Jakubowski, Mateusz; Starosta, Roman; Fritzkowski, Pawel

    2018-01-01

    A computational model for the kinematics of a vertical axis wind turbine (VAWT) is presented. A H-type rotor turbine with a controlled pitch angle is considered. The aim of this solution is to improve the VAWT productivity. The discussed method is related to a narrow computational branch based on the Blade Element Momentum theory (BEM theory). The paper can be regarded as a theoretical basis and an introduction to further studies with the application of BEM. The obtained torque values show the main advantage of using the variable pitch angle.

  8. Variable angle spectroscopic ellipsometric characterization of HfO2 thin film

    Science.gov (United States)

    Kumar, M.; Kumari, N.; Karar, V.; Sharma, A. L.

    2018-02-01

    Hafnium Oxide film was deposited on BK7 glass substrate using reactive oxygenated E-Beam deposition technique. The film was deposited using in-situ quartz crystal thickness monitoring to control the film thickness and rate of evaporation. The thin film was grown with a rate of deposition of 0.3 nm/s. The coated substrate was optically characterized using spectrophotometer to determine its transmission spectra. The optical constants as well as film thickness of the hafnia film were extracted by variable angle spectroscopic ellipsometry with Cauchy fitting at incidence angles of 65˚, 70˚ and 75˚.

  9. Effectiveness of Variable-Gain Kalman Filter Based on Angle Error Calculated from Acceleration Signals in Lower Limb Angle Measurement with Inertial Sensors

    Science.gov (United States)

    Watanabe, Takashi

    2013-01-01

    The wearable sensor system developed by our group, which measured lower limb angles using Kalman-filtering-based method, was suggested to be useful in evaluation of gait function for rehabilitation support. However, it was expected to reduce variations of measurement errors. In this paper, a variable-Kalman-gain method based on angle error that was calculated from acceleration signals was proposed to improve measurement accuracy. The proposed method was tested comparing to fixed-gain Kalman filter and a variable-Kalman-gain method that was based on acceleration magnitude used in previous studies. First, in angle measurement in treadmill walking, the proposed method measured lower limb angles with the highest measurement accuracy and improved significantly foot inclination angle measurement, while it improved slightly shank and thigh inclination angles. The variable-gain method based on acceleration magnitude was not effective for our Kalman filter system. Then, in angle measurement of a rigid body model, it was shown that the proposed method had measurement accuracy similar to or higher than results seen in other studies that used markers of camera-based motion measurement system fixing on a rigid plate together with a sensor or on the sensor directly. The proposed method was found to be effective in angle measurement with inertial sensors. PMID:24282442

  10. 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.

  11. 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.

  12. Variable flip angle excitation for reduced acquisition time magnetic resonance imaging

    International Nuclear Information System (INIS)

    Mills, T.C.; Ortendahl, D.A.; Hylton, N.M.; Carlson, J.W.; Crooks, L.E.; Kaufman, L.

    1987-01-01

    This paper describes an MRI technique which can be used to acquire images at short TR values while maintaining the sensitivity to disease found in longer TR images. For spin echo imaging there are three acquisition parameters that can be set in the imaging protocol; TR, the repetition interval; TE, the time of echo and Θ, the excitation flip angle. Standard imaging techniques set Θ to 90 degrees regardless of the TR value. With Θ fixed, imaging systems have been optimized by varying the value for TE and TR with the results in general indicating the need for long TR values. However, if the flip angle is included as a variable acquisition parameter the optimal operating point can be changed. The solution to the Bloch equation shows a functional relationship between the flip angle and the ratio TR/T1. This functionality was first observed by Ernst and Anderson as a method to increase the signal generated in fourier transform magnetic resonance spectroscopy. When TR/T1<1 the optimum flip angle for producing maximum magnetization in the transverse plane is less then 90 degrees. Therefore, by reducing both TR and flip angle it is possible to maintain signal intensity while reducing the time of data acquisition

  13. Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

    International Nuclear Information System (INIS)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam; Gabel, Frank; Sattler, Michael

    2013-01-01

    Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

  14. Combining NMR and small angle X-ray and neutron scattering in the structural analysis of a ternary protein-RNA complex

    Energy Technology Data Exchange (ETDEWEB)

    Hennig, Janosch; Wang, Iren; Sonntag, Miriam [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany); Gabel, Frank [Extremophiles and Large Molecular Assemblies Group (ELMA), Institut de Biologie Structurale (IBS) CEA-CNRS-UJF (France); Sattler, Michael, E-mail: sattler@helmholtz-muenchen.de [Institute of Structural Biology, Helmholtz Zentrum Muenchen (Germany)

    2013-05-15

    Many processes in the regulation of gene expression and signaling involve the formation of protein complexes involving multi-domain proteins. Individual domains that mediate protein-protein and protein-nucleic acid interactions are typically connected by flexible linkers, which contribute to conformational dynamics and enable the formation of complexes with distinct binding partners. Solution techniques are therefore required for structural analysis and to characterize potential conformational dynamics. Nuclear magnetic resonance spectroscopy (NMR) provides such information but often only sparse data are obtained with increasing molecular weight of the complexes. It is therefore beneficial to combine NMR data with additional structural restraints from complementary solution techniques. Small angle X-ray/neutron scattering (SAXS/SANS) data can be efficiently combined with NMR-derived information, either for validation or by providing additional restraints for structural analysis. Here, we show that the combination of SAXS and SANS data can help to refine structural models obtained from data-driven docking using HADDOCK based on sparse NMR data. The approach is demonstrated with the ternary protein-protein-RNA complex involving two RNA recognition motif (RRM) domains of Sex-lethal, the N-terminal cold shock domain of Upstream-to-N-Ras, and msl-2 mRNA. Based on chemical shift perturbations we have mapped protein-protein and protein-RNA interfaces and complemented this NMR-derived information with SAXS data, as well as SANS measurements on subunit-selectively deuterated samples of the ternary complex. Our results show that, while the use of SAXS data is beneficial, the additional combination with contrast variation in SANS data resolves remaining ambiguities and improves the docking based on chemical shift perturbations of the ternary protein-RNA complex.

  15. Semiclassical use of action-angle variables in the presence of tunnelling

    International Nuclear Information System (INIS)

    Carvalho, R.E. de; Almeida, A.M.O. de

    1988-01-01

    Semiclassical approximations of quantum mechanics are known to be invariant with respect to classical cannonical transformations even though these are not in general isomorphic to unitary transformations in quantum mechanics. It is verified computationally that the energy eigenlevels of a resonant system computed in a harmonic oscillator basis are in good agreement with the semiclassical values obtained with the use of action-angle variables. (A.C.A.S.) [pt

  16. 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

  17. Chemical Shifts of the Carbohydrate Binding Domain of Galectin-3 from Magic Angle Spinning NMR and Hybrid Quantum Mechanics/Molecular Mechanics Calculations.

    Science.gov (United States)

    Kraus, Jodi; Gupta, Rupal; Yehl, Jenna; Lu, Manman; Case, David A; Gronenborn, Angela M; Akke, Mikael; Polenova, Tatyana

    2018-03-22

    Magic angle spinning NMR spectroscopy is uniquely suited to probe the structure and dynamics of insoluble proteins and protein assemblies at atomic resolution, with NMR chemical shifts containing rich information about biomolecular structure. Access to this information, however, is problematic, since accurate quantum mechanical calculation of chemical shifts in proteins remains challenging, particularly for 15 N H . Here we report on isotropic chemical shift predictions for the carbohydrate recognition domain of microcrystalline galectin-3, obtained from using hybrid quantum mechanics/molecular mechanics (QM/MM) calculations, implemented using an automated fragmentation approach, and using very high resolution (0.86 Å lactose-bound and 1.25 Å apo form) X-ray crystal structures. The resolution of the X-ray crystal structure used as an input into the AF-NMR program did not affect the accuracy of the chemical shift calculations to any significant extent. Excellent agreement between experimental and computed shifts is obtained for 13 C α , while larger scatter is observed for 15 N H chemical shifts, which are influenced to a greater extent by electrostatic interactions, hydrogen bonding, and solvation.

  18. 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.

  19. 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.

  20. Refractive Index Imaging of Cells with Variable-Angle Near-Total Internal Reflection (TIR) Microscopy.

    Science.gov (United States)

    Bohannon, Kevin P; Holz, Ronald W; Axelrod, Daniel

    2017-10-01

    The refractive index in the interior of single cells affects the evanescent field depth in quantitative studies using total internal reflection (TIR) fluorescence, but often that index is not well known. We here present method to measure and spatially map the absolute index of refraction in a microscopic sample, by imaging a collimated light beam reflected from the substrate/buffer/cell interference at variable angles of incidence. Above the TIR critical angle (which is a strong function of refractive index), the reflection is 100%, but in the immediate sub-critical angle zone, the reflection intensity is a very strong ascending function of incidence angle. By analyzing the angular position of that edge at each location in the field of view, the local refractive index can be estimated. In addition, by analyzing the steepness of the edge, the distance-to-substrate can be determined. We apply the technique to liquid calibration samples, silica beads, cultured Chinese hamster ovary cells, and primary culture chromaffin cells. The optical technique suffers from decremented lateral resolution, scattering, and interference artifacts. However, it still provides reasonable results for both refractive index (~1.38) and for distance-to-substrate (~150 nm) for the cells, as well as a lateral resolution to about 1 µm.

  1. Air core notch-coil magnet with variable geometry for fast-field-cycling NMR.

    Science.gov (United States)

    Kruber, S; Farrher, G D; Anoardo, E

    2015-10-01

    In this manuscript we present details on the optimization, construction and performance of a wide-bore (71 mm) α-helical-cut notch-coil magnet with variable geometry for fast-field-cycling NMR. In addition to the usual requirements for this kind of magnets (high field-to-power ratio, good magnetic field homogeneity, low inductance and resistance values) a tunable homogeneity and a more uniform heat dissipation along the magnet body are considered. The presented magnet consists of only one machined metallic cylinder combined with two external movable pieces. The optimal configuration is calculated through an evaluation of the magnetic flux density within the entire volume of interest. The magnet has a field-to-current constant of 0.728 mT/A, allowing to switch from zero to 0.125 T in less than 3 ms without energy storage assistance. For a cylindrical sample volume of 35 cm(3) the effective magnet homogeneity is lower than 130 ppm. Copyright © 2015 Elsevier Inc. All rights reserved.

  2. Action-angle variables for the massless relativistic string in 1+1 dimensions

    International Nuclear Information System (INIS)

    Soederberg, B.; Andersson, B.; Gustafson, G.

    1985-01-01

    In this paper the Poisson bracket algebra for the open massless relativistic string in the one-space- and one-time-dimensional case is considered. In order to characterize the orbit of the system the directrix function, i.e., the orbit of one of the endpoints of the string, is used. It turns out that the Poisson bracket algebra is of a very simple form in terms of the parameters of the directrix function. We use these results to construct action-angle variables for the general motion of the string. The variables are different for different Lorentz frames, with a continuous dependence. The action-angle variables of the center-of-mass frame and of the light-cone frames are of particular interest with respect to the simplicity of the Poincare generators and the physical interpretation. For the light-cone frame variables the equivalence to a set of indistinguishable oscillators is shown, for which an excitation corresponds to an instantaneous momentum transfer to an endpoint of the string

  3. Inter-observer variability between radiologists reporting on cerebellopontine angle tumours on magnetic resonance imaging.

    Science.gov (United States)

    Teh, S R; Ranguis, S; Fagan, P

    2017-01-01

    Studies demonstrate the significance of intra- and inter-observer variability when measuring cerebellopontine angle tumours on magnetic resonance imaging, with measured differences as high as 2 mm. To determine intra- and inter-observer measurement variability of cerebellopontine angle tumours in a specialised institution. The magnetic resonance imaging maximal diameter of 12 randomly selected cerebellopontine angle tumours were independently measured by 4 neuroradiologists at a tertiary referral centre using a standard definition for maximal tumour diameter. Average deviation and intraclass correlation were subsequently calculated. Inter-observer difference averaged 0.33 ± 0.04 mm (range, 0.0-0.8 mm). Intra-observer measurements were more consistent than inter-observer measurements, with differences averaging 0.17 mm (95 per cent confidence interval = 0.27-0.06, p = 0.002). Inter-observer reliability was 0.99 (95 per cent confidence interval = 0.97-0.99), suggesting high reliability between the readings. The use of a standard definition for maximal tumour volume provided high reliability amongst radiologists' readings. To avoid oversizing tumours, it is recommended that conservative monitoring be conducted by the same institution with thin slice magnetic resonance imaging scans.

  4. Solar Cycle Variability Induced by Tilt Angle Scatter in a Babcock-Leighton Solar Dynamo Model

    Science.gov (United States)

    Karak, Bidya Binay; Miesch, Mark

    2017-09-01

    We present results from a three-dimensional Babcock-Leighton (BL) dynamo model that is sustained by the emergence and dispersal of bipolar magnetic regions (BMRs). On average, each BMR has a systematic tilt given by Joy’s law. Randomness and nonlinearity in the BMR emergence of our model produce variable magnetic cycles. However, when we allow for a random scatter in the tilt angle to mimic the observed departures from Joy’s law, we find more variability in the magnetic cycles. We find that the observed standard deviation in Joy’s law of {σ }δ =15^\\circ produces a variability comparable to the observed solar cycle variability of ˜32%, as quantified by the sunspot number maxima between 1755 and 2008. We also find that tilt angle scatter can promote grand minima and grand maxima. The time spent in grand minima for {σ }δ =15^\\circ is somewhat less than that inferred for the Sun from cosmogenic isotopes (about 9% compared to 17%). However, when we double the tilt scatter to {σ }δ =30^\\circ , the simulation statistics are comparable to the Sun (˜18% of the time in grand minima and ˜10% in grand maxima). Though the BL mechanism is the only source of poloidal field, we find that our simulations always maintain magnetic cycles even at large fluctuations in the tilt angle. We also demonstrate that tilt quenching is a viable and efficient mechanism for dynamo saturation; a suppression of the tilt by only 1°-2° is sufficient to limit the dynamo growth. Thus, any potential observational signatures of tilt quenching in the Sun may be subtle.

  5. 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.

  6. 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.

  7. Single cell adhesion strength assessed with variable-angle total internal reflection fluorescence microscopy

    Directory of Open Access Journals (Sweden)

    Marcelina Cardoso Dos Santos

    2017-06-01

    Full Text Available We propose a new strategy to evaluate adhesion strength at the single cell level. This approach involves variable-angle total internal reflection fluorescence microscopy to monitor in real time the topography of cell membranes, i.e. a map of the membrane/substrate separation distance. According to the Boltzmann distribution, both potential energy profile and dissociation energy related to the interactions between the cell membrane and the substrate were determined from the membrane topography. We have highlighted on glass substrates coated with poly-L-lysine and fibronectin, that the dissociation energy is a reliable parameter to quantify the adhesion strength of MDA-MB-231 motile cells.

  8. 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

  9. Pairwise NMR experiments for the determination of protein backbone dihedral angle Φ based on cross-correlated spin relaxation

    International Nuclear Information System (INIS)

    Takahashi, Hideo; Shimada, Ichio

    2007-01-01

    Novel cross-correlated spin relaxation (CCR) experiments are described, which measure pairwise CCR rates for obtaining peptide dihedral angles Φ. The experiments utilize intra-HNCA type coherence transfer to refocus 2-bond J NCα coupling evolution and generate the N (i)-C α (i) or C'(i-1)-C α (i) multiple quantum coherences which are required for measuring the desired CCR rates. The contribution from other coherences is also discussed and an appropriate setting of the evolution delays is presented. These CCR experiments were applied to 15 N- and 13 C-labeled human ubiquitin. The relevant CCR rates showed a high degree of correlation with the Φ angles observed in the X-ray structure. By utilizing these CCR experiments in combination with those previously established for obtaining dihedral angle Ψ, we can determine high resolution structures of peptides that bind weakly to large target molecules

  10. MERA: a webserver for evaluating backbone torsion angle distributions in dynamic and disordered proteins from NMR data

    Energy Technology Data Exchange (ETDEWEB)

    Mantsyzov, Alexey B. [M.V. Lomonosov Moscow State University, Faculty of Fundamental Medicine (Russian Federation); Shen, Yang; Lee, Jung Ho [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States); Hummer, Gerhard [Max Planck Institute of Biophysics (Germany); Bax, Ad, E-mail: bax@nih.gov [National Institutes of Health, Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases (United States)

    2015-09-15

    MERA (Maximum Entropy Ramachandran map Analysis from NMR data) is a new webserver that generates residue-by-residue Ramachandran map distributions for disordered proteins or disordered regions in proteins on the basis of experimental NMR parameters. As input data, the program currently utilizes up to 12 different parameters. These include three different types of short-range NOEs, three types of backbone chemical shifts ({sup 15}N, {sup 13}C{sup α}, and {sup 13}C′), six types of J couplings ({sup 3}J{sub HNHα}, {sup 3}J{sub C′C′}, {sup 3}J{sub C′Hα}, {sup 1}J{sub HαCα}, {sup 2}J{sub CαN} and {sup 1}J{sub CαN}), as well as the {sup 15}N-relaxation derived J(0) spectral density. The Ramachandran map distributions are reported in terms of populations of their 15° × 15° voxels, and an adjustable maximum entropy weight factor is available to ensure that the obtained distributions will not deviate more from a newly derived coil library distribution than required to account for the experimental data. MERA output includes the agreement between each input parameter and its distribution-derived value. As an application, we demonstrate performance of the program for several residues in the intrinsically disordered protein α-synuclein, as well as for several static and dynamic residues in the folded protein GB3.

  11. Magic-angle-spinning NMR spectroscopy. January 1978-May 1988 (Citations from the INSPEC: Information Services for the Physics and Engineering Communities data base). Report for January 1978-May 1988

    International Nuclear Information System (INIS)

    1988-05-01

    This bibliography contains citations concerning the principles and applications of magic-angle spinning (MAS) nuclear magnetic resonance (NMR) in high-resolution spectra analysis of solids. Magic-angle spinning NMR is a very powerful spectrographic technique for the study of structures, dynamics, and reactivity of solids, and polcrystalline and amorphous solids. Studies of various materials are presented, including zeolites, organic compounds and polymers, liquid crystals, silicate and borate glasses, and alumina and oxide films. Applications in conductive polymers, biological systems, and organic matrixes of composite materials are presented. (Contains 89 citations fully indexed and including a title list.)

  12. Cross polarization with phase and amplitude modulation of radio frequency fields in NMR-experiments with sample rotation at magic angle

    International Nuclear Information System (INIS)

    Dvinskij, S.V.; Chizhik, V.I.

    2006-01-01

    One analyzes cross polarization of nuclei within a rotating system of coordinates as applied to the NMR-experiments with a specimen rotation under the magic angle. One worded a concept of simultaneous phase and amplitude modulation according to which the Hamiltonian form of the restored dipole interaction persisted if inversion of difference of radiofrequency field amplitudes occurred simultaneously with phase inversion. One presents a theoretical substantiation in terms of the average Hamiltonian theory. The concept is demonstrated both experimentally and by means of numerical analysis for a number of special cases. Phase periodic inversion in cross polarized experiments is shown to result into practically important advantage of suppression of interactions of chemical shift and influence of effects of coarse adjustment of radiofrequency field parameters [ru

  13. Determination of the torsion angles of alanine and glycine residues of model compounds of spider silk (AGG){sub 10} using solid-state NMR methods

    Energy Technology Data Exchange (ETDEWEB)

    Ashida, Jun; Ohgo, Kosuke; Komatsu, Kohei; Kubota, Ayumi; Asakura, Tetsuo [Tokyo University of Agriculture and Technology, Department of Biotechnology (Japan)], E-mail: asakura@cc.tuat.ac.jp

    2003-02-15

    Spiders synthesize several kinds of silk fibers. In the primary structure of spider silk, one of the major ampullate (dragline, frame) silks, spidroin 1, and flagelliform silk (core fibers of adhesive spiral), there are common repeated X-Gly-Gly (X = Ala, Leu, Pro, Tyr, Glu, and Arg) sequences, which are considered to be related to the elastic character of these fibers. In this paper, two dimensional spin diffusion solid-state NMR under off magic angle spinning (OMAS), {sup 13}C chemical shift contour plots, and Rotational Echo DOuble Resonance (REDOR) were applied to determine the torsion angles of one Ala and two kinds of Gly residues in the Ala-Gly-Gly sequence of {sup 13}C=O isotope-labeled (Ala-Gly-Gly){sub 10}. The torsion angles were determined to be ({phi}, {psi}) = (-90 deg., 150 deg.) within an experimental error of {+-}10 deg. for each residue. This conformation is characterized as 3{sub 1} helix which is in agreement with the structure proposed from the X-ray powder diffraction pattern of poly(Ala-Gly-Gly). The 3{sub 1} helix of (Ala-Gly-Gly){sub 10} does not change by formic acid treatment although (Ala-Gly){sub 15} easily changes from the silk I conformation (the structure of Bombyx mori silk fibroin before spinning in the solid state) to silk II conformation (the structure of the silk fiber after spinning) by such treatment. Thus, the 3{sub 1} helix conformation of (Ala-Gly-Gly){sub 10} is considered very stable. Furthermore, the torsion angles of the 16th Leu residue of (Leu-Gly-Gly){sub 10} were also determined as ({phi}, {psi}) = (-90 deg., 150 deg.) and this peptide is also considered to take 3{sub 1} helix conformation.

  14. A KAM theorem without action-angle variables for elliptic lower dimensional tori

    International Nuclear Information System (INIS)

    Luque, Alejandro; Villanueva, Jordi

    2011-01-01

    We study elliptic lower dimensional invariant tori of Hamiltonian systems via parametrizations. The method is based on solving iteratively the functional equations that stand for invariance and reducibility. In contrast with classical methods, we do not assume that the system is close to an integrable one nor that it is written in action-angle variables. We only require an approximation of an invariant torus with a fixed vector of basic frequencies and a basis along the torus that approximately reduces the normal variational equations to constant coefficients. We want to highlight that this approach presents many advantages compared with methods which are built in terms of canonical transformations, e.g., it produces simpler and more constructive proofs that lead to more efficient numerical algorithms for the computation of these objects. Such numerical algorithms are suitable to be adapted in order to perform computer assisted proofs

  15. Practical way to avoid spurious geometrical contributions in Brillouin light scattering experiments at variable scattering angles.

    Science.gov (United States)

    Battistoni, Andrea; Bencivenga, Filippo; Fioretto, Daniele; Masciovecchio, Claudio

    2014-10-15

    In this Letter, we present a simple method to avoid the well-known spurious contributions in the Brillouin light scattering (BLS) spectrum arising from the finite aperture of collection optics. The method relies on the use of special spatial filters able to select the scattered light with arbitrary precision around a given value of the momentum transfer (Q). We demonstrate the effectiveness of such filters by analyzing the BLS spectra of a reference sample as a function of scattering angle. This practical and inexpensive method could be an extremely useful tool to fully exploit the potentiality of Brillouin acoustic spectroscopy, as it will easily allow for effective Q-variable experiments with unparalleled luminosity and resolution.

  16. Adhesion of living cells revealed by variable-angle total internal reflection fluorescence microscopy (Conference Presentation)

    Science.gov (United States)

    Cardoso Dos Santos, Marcelina; Vézy, Cyrille; Jaffiol, Rodolphe

    2016-02-01

    Total Internal Reflection Fluorescence Microscopy (TIRFM) is a widespread technique to study cellular process occurring near the contact region with the glass substrate. In this field, determination of the accurate distance from the surface to the plasma membrane constitutes a crucial issue to investigate the physical basis of cellular adhesion process. However, quantitative interpretation of TIRF pictures regarding the distance z between a labeled membrane and the substrate is not trivial. Indeed, the contrast of TIRF images depends on several parameters more and less well known (local concentration of dyes, absorption cross section, angular emission pattern…). The strategy to get around this problem is to exploit a series of TIRF pictures recorded at different incident angles in evanescent regime. This technique called variable-angle TIRF microscopy (vaTIRFM), allowing to map the membrane-substrate separation distance with a nanometric resolution (10-20 nm). vaTIRFM was developed by Burmeister, Truskey and Reichert in the early 1990s with a prism-based TIRF setup [Journal of Microscopy 173, 39-51 (1994)]. We propose a more convenient prismless setup, which uses only a rotatable mirror to adjust precisely the laser beam on the back focal plane of the oil immersion objective (no azimuthal scanning is needed). The series of TIRF images permit us to calculate accurately membrane-surface distances in each pixel. We demonstrate that vaTIRFM are useful to quantify the adhesion of living cells for specific and unspecific membrane-surface interactions, achieved on various functionalized substrates with polymers (BSA, poly-L-lysin) or extracellular matrix proteins (collagen and fibronectin).

  17. Atomic-resolution structure of the CAP-Gly domain of dynactin on polymeric microtubules determined by magic angle spinning NMR spectroscopy.

    Science.gov (United States)

    Yan, Si; Guo, Changmiao; Hou, Guangjin; Zhang, Huilan; Lu, Xingyu; Williams, John Charles; Polenova, Tatyana

    2015-11-24

    Microtubules and their associated proteins perform a broad array of essential physiological functions, including mitosis, polarization and differentiation, cell migration, and vesicle and organelle transport. As such, they have been extensively studied at multiple levels of resolution (e.g., from structural biology to cell biology). Despite these efforts, there remain significant gaps in our knowledge concerning how microtubule-binding proteins bind to microtubules, how dynamics connect different conformational states, and how these interactions and dynamics affect cellular processes. Structures of microtubule-associated proteins assembled on polymeric microtubules are not known at atomic resolution. Here, we report a structure of the cytoskeleton-associated protein glycine-rich (CAP-Gly) domain of dynactin motor on polymeric microtubules, solved by magic angle spinning NMR spectroscopy. We present the intermolecular interface of CAP-Gly with microtubules, derived by recording direct dipolar contacts between CAP-Gly and tubulin using double rotational echo double resonance (dREDOR)-filtered experiments. Our results indicate that the structure adopted by CAP-Gly varies, particularly around its loop regions, permitting its interaction with multiple binding partners and with the microtubules. To our knowledge, this study reports the first atomic-resolution structure of a microtubule-associated protein on polymeric microtubules. Our approach lays the foundation for atomic-resolution structural analysis of other microtubule-associated motors.

  18. Action-angle variables and a KAM theorem for b-Poisson manifolds

    OpenAIRE

    Kiesenhofer, Anna; Miranda Galcerán, Eva; Scott, Geoffrey

    2015-01-01

    In this article we prove an action-angle theorem for b-integrable systems on b-Poisson manifolds improving the action-angle theorem contained in [14] for general Poisson manifolds in this setting. As an application, we prove a KAM-type theorem for b-Poisson manifolds. (C) 2015 Elsevier Masson SAS. All rights reserved.

  19. Dielectric energy versus plasma energy, and Hamiltonian action-angle variables for the Vlasov equation

    International Nuclear Information System (INIS)

    Morrison, P.J.

    1992-04-01

    Expressions for the energy content of one-dimensional electrostatic perturbations about homogeneous equilibria are revisited. The well-known dielectric energy, var-epsilon D , is compared with the exact plasma free energy expression, δ 2 F, that is conserved by the Vlasov-Poisson system. The former is an expression in terms of the perturbed electric field amplitude, while the latter is determined by a generating function, which describes perturbations of the distribution function that respect the important constraint of dynamical accessibility of the system. Thus the comparison requires solving the Vlasov equation for such a perturbations of the distribution function in terms of the electric field. This is done for neutral modes of oscillation that occur for equilibria with stationary inflection points, and it is seen that for these special modes δ 2 F = var-epsilon D . In the case of unstable and corresponding damped modes it is seen that δ 2 F ≠ var-epsilon D ; in fact δ 2 F ≡ 0. This failure of the dielectric energy expression persists even for arbitrarily small growth and damping rates since var-epsilon D is nonzero in this limit, whereas δ 2 F remains zero. The connection between the new exact energy expression and the at-best approximate var-epsilon D is described. The new expression motivates natural definitions of Hamiltonian action variables and signature. A general linear integral transform is introduced that maps the linear version of the noncanonical Hamiltonian structure, which describes the Vlasov equation, to action-angle (diagonal) form

  20. Synthesis, Characterization, and Variable-Temperature NMR Studies of Silver(I) Complexes for Selective Nitrene Transfer.

    Science.gov (United States)

    Huang, Minxue; Corbin, Joshua R; Dolan, Nicholas S; Fry, Charles G; Vinokur, Anastasiya I; Guzei, Ilia A; Schomaker, Jennifer M

    2017-06-05

    An array of silver complexes supported by nitrogen-donor ligands catalyze the transformation of C═C and C-H bonds to valuable C-N bonds via nitrene transfer. The ability to achieve high chemoselectivity and site selectivity in an amination event requires an understanding of both the solid- and solution-state behavior of these catalysts. X-ray structural characterizations were helpful in determining ligand features that promote the formation of monomeric versus dimeric complexes. Variable-temperature 1 H and DOSY NMR experiments were especially useful for understanding how the ligand identity influences the nuclearity, coordination number, and fluxional behavior of silver(I) complexes in solution. These insights are valuable for developing improved ligand designs.

  1. I. The synthesis and characterization of annulated uranocenes. II. The variable temperature 1H NMR of uranocenes

    International Nuclear Information System (INIS)

    Luke, W.D.

    1980-01-01

    A general synthetic route to alkyl annulated cyclooctatetraene dianions and the corresponding annulated uranocenes has been developed. Dideprotonation of bicyclooctatrienes, resulting from reaction of cyclooctatetraene dianion with l,n-dialkylbromides or methanesulfonates, affords alkyl annulated cyclooctatetraene dianions in moderate yields. Dicyclopenteno-, bisdimethylcyclopenteno- and dicyclohexenouranocene were prepared from the corresponding cyclooctatetraene dianions and UCl 4 . The structures of dicyclobuteno- and dicyclopentenouranocene were elucidated by single crystal X-ray diffraction, and the effects of annulation on the uranocene skeleton are discussed. Attempted synthesis of benzocyclooctatetraene and a benzannulated uranocene is reported. The variable temperature 1 H NMR spectrum of uranocene has been reinvestigated from -100 to 100 0 C. The isotropic shift was found to be linear in T -1 with an extrapolated intercept of 0 at T -1 = 0. Variable temperature 1 H NMR spectra, from -80 to 70 0 C, of 17 substituted uranocenes are reported. The energy barrier to ring rotation in 1,1', 4,4'-tetra-t-butyl-uranocene was determined to be 8.24 +- 0.5 kcal/mole while the barrier in the corresponding 1,1', 3,3'-tetra-t-butylferrocene was determined to be 13.1 kcal/mole. Alkyl substitution is shown to have little effect on the electronic and magnetic properties of the uranocene skeleton, and thus alkyl substituted uranocenes are treated as having effective axial symmetry in analysis of the observed isotropic shifts. Using diannulated uranocenes as model systems an analysis of the contact and pseudocontact components of the observed isotropic shifts in uranocene and alkyl substituted uranocenes is presented

  2. Variability of photovoltaic panels efficiency depending on the value of the angle of their inclination relative to the horizon

    Directory of Open Access Journals (Sweden)

    Majdak Marek

    2017-01-01

    Full Text Available The objective of this paper was to determine the relationship between the efficiency of photovoltaic panels and the value of the angle of their inclination relative to the horizon. For the purpose of experimental research have been done tests on the photovoltaic modules made of monocrystalline, polycrystalline and amorphous silicon. The experiment consisted of measurement of the voltage and current generated by photovoltaic panels at a known value of solar radiation and a specified resistance value determined by using resistor with variable value of resistance and known value of the angle of their inclination relative to the horizon.

  3. Exploring structural variability in X-ray crystallographic models using protein local optimization by torsion-angle sampling

    International Nuclear Information System (INIS)

    Knight, Jennifer L.; Zhou, Zhiyong; Gallicchio, Emilio; Himmel, Daniel M.; Friesner, Richard A.; Arnold, Eddy; Levy, Ronald M.

    2008-01-01

    Torsion-angle sampling, as implemented in the Protein Local Optimization Program (PLOP), is used to generate multiple structurally variable single-conformer models which are in good agreement with X-ray data. An ensemble-refinement approach to differentiate between positional uncertainty and conformational heterogeneity is proposed. Modeling structural variability is critical for understanding protein function and for modeling reliable targets for in silico docking experiments. Because of the time-intensive nature of manual X-ray crystallographic refinement, automated refinement methods that thoroughly explore conformational space are essential for the systematic construction of structurally variable models. Using five proteins spanning resolutions of 1.0–2.8 Å, it is demonstrated how torsion-angle sampling of backbone and side-chain libraries with filtering against both the chemical energy, using a modern effective potential, and the electron density, coupled with minimization of a reciprocal-space X-ray target function, can generate multiple structurally variable models which fit the X-ray data well. Torsion-angle sampling as implemented in the Protein Local Optimization Program (PLOP) has been used in this work. Models with the lowest R free values are obtained when electrostatic and implicit solvation terms are included in the effective potential. HIV-1 protease, calmodulin and SUMO-conjugating enzyme illustrate how variability in the ensemble of structures captures structural variability that is observed across multiple crystal structures and is linked to functional flexibility at hinge regions and binding interfaces. An ensemble-refinement procedure is proposed to differentiate between variability that is a consequence of physical conformational heterogeneity and that which reflects uncertainty in the atomic coordinates

  4. Spectral editing at ultra-fast magic-angle-spinning in solid-state NMR: facilitating protein sequential signal assignment by HIGHLIGHT approach

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Songlin; Matsuda, Isamu; Long, Fei; Ishii, Yoshitaka, E-mail: yishii@uic.edu [University of Illinois at Chicago, Department of Chemistry (United States)

    2016-02-15

    This study demonstrates a novel spectral editing technique for protein solid-state NMR (SSNMR) to simplify the spectrum drastically and to reduce the ambiguity for protein main-chain signal assignments in fast magic-angle-spinning (MAS) conditions at a wide frequency range of 40–80 kHz. The approach termed HIGHLIGHT (Wang et al., in Chem Comm 51:15055–15058, 2015) combines the reverse {sup 13}C, {sup 15}N-isotope labeling strategy and selective signal quenching using the frequency-selective REDOR pulse sequence under fast MAS. The scheme allows one to selectively observe the signals of “highlighted” labeled amino-acid residues that precede or follow unlabeled residues through selectively quenching {sup 13}CO or {sup 15}N signals for a pair of consecutively labeled residues by recoupling {sup 13}CO–{sup 15}N dipolar couplings. Our numerical simulation results showed that the scheme yielded only ∼15 % loss of signals for the highlighted residues while quenching as much as ∼90 % of signals for non-highlighted residues. For lysine-reverse-labeled micro-crystalline GB1 protein, the 2D {sup 15}N/{sup 13}C{sub α} correlation and 2D {sup 13}C{sub α}/{sup 13}CO correlation SSNMR spectra by the HIGHLIGHT approach yielded signals only for six residues following and preceding the unlabeled lysine residues, respectively. The experimental dephasing curves agreed reasonably well with the corresponding simulation results for highlighted and quenched residues at spinning speeds of 40 and 60 kHz. The compatibility of the HIGHLIGHT approach with fast MAS allows for sensitivity enhancement by paramagnetic assisted data collection (PACC) and {sup 1}H detection. We also discuss how the HIGHLIGHT approach facilitates signal assignments using {sup 13}C-detected 3D SSNMR by demonstrating full sequential assignments of lysine-reverse-labeled micro-crystalline GB1 protein (∼300 nmol), for which data collection required only 11 h. The HIGHLIGHT approach offers valuable

  5. Study on variable pitch strategy in H-type wind turbine considering effect of small angle of attack

    DEFF Research Database (Denmark)

    Zhao, Zhenzhou; Qian, Siyuan; Shen, Wenzhong

    2017-01-01

    Variable-pitch (VP) technology is an effective approach to upgrade the aerodynamics of the blade of an H-type vertical-axis wind turbine (VAWT). At present, most of the research efforts are focused on the performance improvement of the azimuth angle owing to the large angle of attack (Ao...... distribution in the swept area of turbine changes from an arched shape of the FP-VAWT into a rectangular shape of the VP-VAWT. At last, an 18.9% growth in power efficiency is achieved. All of the above results confirm that the new VP-technology can effectively improve VAWT performance and also widens...... the highest performance tip speed ratio zone which makes the turbines capable of running with high efficiency in wider zones....

  6. Fast-gradient-echo variable-flip-angle imaging of the cervical spine

    International Nuclear Information System (INIS)

    Van Dyke, C.W.; Ross, J.S.; Masaryk, T.J.; Tkach, J.; Beale, S.; Hueftle, M.G.; Kaufman, B.; Modic, M.T.

    1987-01-01

    Two hundred consecutive patients were studied with 4-mm sagittal and axial T1-weighted images and gradient echo sequences with 6-msec or 13-msec echo time (TE) and 10 0 or 60 0 flip angles to evaluate cervical extradural disease. Images were independently evaluated for contrast behavior and anatomy, then directly compared for conspicuity of lesions. FLASH sequences produced better conspicuity of disease in half the imaging time. T1-weighted spin-echo (SE) sequences were more sensitive to marrow changes and intradural disease. Shorter TEs produced overall image improvement and reduced susceptibility effects. A fast and sensitive cervical examination combines sagittal T1-weighted SE with sagittal and axial FLASH 10 0 sequences with 6-msec TE

  7. Integrability of geodesics and action-angle variables in Sasaki-Einstein space T{sup 1,1}

    Energy Technology Data Exchange (ETDEWEB)

    Visinescu, Mihai [National Institute of Physics and Nuclear Engineering, Department Theoretical Physics, Magurele, Bucharest (Romania)

    2016-09-15

    We briefly describe the construction of Staekel-Killing and Killing-Yano tensors on toric Sasaki-Einstein manifolds without working out intricate generalized Killing equations. The integrals of geodesic motions are expressed in terms of Killing vectors and Killing-Yano tensors of the homogeneous Sasaki-Einstein space T{sup 1,1}. We discuss the integrability of geodesics and construct explicitly the action-angle variables. Two pairs of frequencies of the geodesic motions are resonant giving way to chaotic behavior when the system is perturbed. (orig.)

  8. Controlling T2 blurring in 3D RARE arterial spin labeling acquisition through optimal combination of variable flip angles and k-space filtering.

    Science.gov (United States)

    Zhao, Li; Chang, Ching-Di; Alsop, David C

    2018-02-09

    To improve the SNR efficiency and reduce the T 2 blurring of 3D rapid acquisition with relaxation enhancement stack-of-spiral arterial spin labeling imaging by using variable refocusing flip angles and k-space filtering. An algorithm for determining the optimal combination of variable flip angles and filtering correction is proposed. The flip angles are designed using extended phase graph physical simulations in an analytical and global optimization framework, with an optional constraint on deposited power. Optimal designs for correcting to Hann and Fermi window functions were compared with conventional constant amplitude or variable flip angle only designs on 6 volunteers. With the Fermi window correction, the proposed optimal designs provided 39.8 and 27.3% higher SNR (P variable flip angle designs. Even when power deposition was limited to 50% of the constant amplitude design, the proposed method outperformed the SNR (P variable flip angles can be derived as the output of an optimization problem. The combined design of variable flip angle and k-space filtering provided superior SNR to designs primarily emphasizing either approach singly. © 2018 International Society for Magnetic Resonance in Medicine.

  9. Closed Loop Sawtooth Period Control Using Variable Eccd Injection Angles on Tore Supra

    International Nuclear Information System (INIS)

    Lennholm, M.; Eriksson, L.G.; Turco, F.; Bouquey, F.; Darbos, C.; Dumont, R.; Giruzzi, G.; Jung, M.; Lambert, R.; Magne, R.; Molina, D.; Moreau, P.; Rimini, F.; Segui, J.L.; Song, S.; Traisnel, E.

    2009-01-01

    Closed loop control of the period of fast ion stabilized sawtooth has been demonstrated for the first time on Tore Supra by varying the electron cyclotron current drive (ECCD) injection angles in real time. Fast ions generated by up to 4 MW of central ion cyclotron resonance heating (ICRH) increased the sawtooth period from the ohmic value of 25 ms to 60 to 100 ms. This sawtooth period was reduced to 30 ms by the addition of only 300 kW of ECCD. In ICRH heated shots where the normalized minor radius of the ECCD absorption location was swept from 0.4 to 0.05 in 4 s, the sawtooth period showed an abrupt change from 70 to 30 ms when the ECCD deposition normalized minor radius reached ∼ 0.2. This short period was then maintained until the absorption location moved well inside the sawtooth inversion radius at which point it abruptly returned to 70 ins. A closed loop controller was implemented that allowed the sawtooth period to be switched in real time between short and long sawteeth with a response time of the order of 1 s. (authors)

  10. 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

  11. 1H NMR and small-angle neutron scattering investigation of the structure and solubilization behavior of three-layer nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Kříž, Jaroslav; Pleštil, Josef; Pospíšil, Herman; Kadlec, Petr; Koňák, Čestmír; Almásy, L.; Kuklin, A. I.

    2004-01-01

    Roč. 20, č. 25 (2004), s. 11255-11263 ISSN 0743-7463 R&D Projects: GA ČR GA203/03/0600 Institutional research plan: CEZ:AV0Z4050913 Keywords : nanoparticles * polymer micelles * NMR Subject RIV: CD - Macromolecular Chemistry Impact factor: 3.295, year: 2004

  12. Multiple acquisition of magic angle spinning solid-state NMR experiments using one receiver: Application to microcrystalline and membrane protein preparations

    Science.gov (United States)

    Gopinath, T.; Veglia, Gianluigi

    2015-04-01

    Solid-state NMR spectroscopy of proteins is a notoriously low-throughput technique. Relatively low-sensitivity and poor resolution of protein samples require long acquisition times for multidimensional NMR experiments. To speed up data acquisition, we developed a family of experiments called Polarization Optimized Experiments (POE), in which we utilized the orphan spin operators that are discarded in classical multidimensional NMR experiments, recovering them to allow simultaneous acquisition of multiple 2D and 3D experiments, all while using conventional probes with spectrometers equipped with one receiver. POE allow the concatenation of multiple 2D or 3D pulse sequences into a single experiment, thus potentially combining all of the aforementioned advances, boosting the capability of ssNMR spectrometers at least two-fold without the addition of any hardware. In this perspective, we describe the first generation of POE, such as dual acquisition MAS (or DUMAS) methods, and then illustrate the evolution of these experiments into MEIOSIS, a method that enables the simultaneous acquisition of multiple 2D and 3D spectra. Using these new pulse schemes for the solid-state NMR investigation of biopolymers makes it possible to obtain sequential resonance assignments, as well as distance restraints, in about half the experimental time. While designed for acquisition of heteronuclei, these new experiments can be easily implemented for proton detection and coupled with other recent advancements, such as dynamic nuclear polarization (DNP), to improve signal to noise. Finally, we illustrate the application of these methods to microcrystalline protein preparations as well as single and multi-span membrane proteins reconstituted in lipid membranes.

  13. Constraining variable density of ice shelves using wide-angle radar measurements

    Science.gov (United States)

    Drews, Reinhard; Brown, Joel; Matsuoka, Kenichi; Witrant, Emmanuel; Philippe, Morgane; Hubbard, Bryn; Pattyn, Frank

    2016-04-01

    The thickness of ice shelves, a basic parameter for mass balance estimates, is typically inferred using hydrostatic equilibrium, for which knowledge of the depth-averaged density is essential. The densification from snow to ice depends on a number of local factors (e.g., temperature and surface mass balance) causing spatial and temporal variations in density-depth profiles. However, direct measurements of firn density are sparse, requiring substantial logistical effort. Here, we infer density from radio-wave propagation speed using ground-based wide-angle radar data sets (10 MHz) collected at five sites on Roi Baudouin Ice Shelf (RBIS), Dronning Maud Land, Antarctica. We reconstruct depth to internal reflectors, local ice thickness, and firn-air content using a novel algorithm that includes traveltime inversion and ray tracing with a prescribed shape of the depth-density relationship. For the particular case of an ice-shelf channel, where ice thickness and surface slope change substantially over a few kilometers, the radar data suggest that firn inside the channel is about 5 % denser than outside the channel. Although this density difference is at the detection limit of the radar, it is consistent with a similar density anomaly reconstructed from optical televiewing, which reveals that the firn inside the channel is 4.7 % denser than that outside the channel. Hydrostatic ice thickness calculations used for determining basal melt rates should account for the denser firn in ice-shelf channels. The radar method presented here is robust and can easily be adapted to different radar frequencies and data-acquisition geometries.

  14. High-Resolution Magic-Angle-Spinning NMR and Magnetic Resonance Imaging Spectroscopies Distinguish Metabolome and Structural Properties of Maize Seeds from Plants Treated with Different Fertilizers and Arbuscular mycorrhizal fungi.

    Science.gov (United States)

    Mazzei, Pierluigi; Cozzolino, Vincenza; Piccolo, Alessandro

    2018-03-21

    Both high-resolution magic-angle-spinning (HRMAS) and magnetic resonance imaging (MRI) NMR spectroscopies were applied here to identify the changes of metabolome, morphology, and structural properties induced in seeds (caryopses) of maize plants grown at field level under either mineral or compost fertilization in combination with the inoculation by arbuscular mycorrhizal fungi (AMF). The metabolome of intact caryopses was examined by HRMAS-NMR, while the morphological aspects, endosperm properties and seed water distribution were investigated by MRI. Principal component analysis (PCA) was applied to evaluate 1 H CPMG (Carr-Purcel-Meiboom-Gill) HRMAS spectra as well as several MRI-derived parameters ( T 1 , T 2 , and self-diffusion coefficients) of intact maize caryopses. PCA score-plots from spectral results indicated that both seeds metabolome and structural properties depended on the specific field treatment undergone by maize plants. Our findings show that a combination of multivariate statistical analyses with advanced and nondestructive NMR techniques, such as HRMAS and MRI, enables the evaluation of the effects induced on maize caryopses by different fertilization and management practices at field level. The spectroscopic approach adopted here may become useful for the objective appraisal of the quality of seeds produced under a sustainable agriculture.

  15. Structural Masquerade of Plesiomonas shigelloides Strain CNCTC 78/89 O-Antigen-High-Resolution Magic Angle Spinning NMR Reveals the Modified d-galactan I of Klebsiella pneumoniae.

    Science.gov (United States)

    Ucieklak, Karolina; Koj, Sabina; Pawelczyk, Damian; Niedziela, Tomasz

    2017-11-29

    The high-resolution magic angle spinning nuclear magnetic resonance spectroscopy (HR-MAS NMR) analysis of Plesiomonas shigelloides 78/89 lipopolysaccharide directly on bacteria revealed the characteristic structural features of the O -acetylated polysaccharide in the NMR spectra. The O -antigen profiles were unique, yet the pattern of signals in the, spectra along with their ¹H, 13 C chemical shift values, resembled these of d-galactan I of Klebsiella pneumoniae . The isolated O- specific polysaccharide (O-PS) of P. shigelloides strain CNCTC 78/89 was investigated by ¹H and 13 C NMR spectroscopy, mass spectrometry and chemical methods. The analyses demonstrated that the P. shigelloides 78/89 O- PS is composed of →3)-α-d-Gal p -(1→3)-β-d-Gal f 2OAc-(1→ disaccharide repeating units. The O- acetylation was incomplete and resulted in a microheterogeneity of the O- antigen. This O- acetylation generates additional antigenic determinants within the O- antigen, forms a new chemotype, and contributes to the epitopes recognized by the O- serotype specific antibodies. The serological cross-reactivities further confirmed the inter-specific structural similarity of these O- antigens.

  16. Effect of knee and trunk angle on kinetic variables during the isometric midthigh pull: test-retest reliability.

    Science.gov (United States)

    Comfort, Paul; Jones, Paul A; McMahon, John J; Newton, Robert

    2015-01-01

    The isometric midthigh pull (IMTP) has been used to monitor changes in force, maximum rate of force development (mRFD), and impulse, with performance in this task being associated with performance in athletic tasks. Numerous postures have been adopted in the literature, which may affect the kinetic variables during the task; therefore, the aim of this investigation was to determine whether different knee-joint angles (120°, 130°, 140°, and 150°) and hip-joint angles (125° and 145°), including the subjects preferred posture, affect force, mRFD, and impulse during the IMTP. Intraclass correlation coefficients demonstrated high within-session reliability (r ≥ .870, P kinetic variables determined in all postures, excluding impulse measures during the 130° knee-flexion, 125° hip-flexion posture, which showed a low to moderate reliability (r = .666-.739, P .819, P kinetic variables. There were no significant differences in peak force (P > .05, Cohen d = 0.037, power = .408), mRFD (P > .05, Cohen d = 0.037, power = .409), or impulse at 100 ms (P > .05, Cohen d = 0.056, power = .609), 200 ms (P > .05, Cohen d = 0.057, power = .624), or 300 ms (P > .05, Cohen d = 0.061, power = .656) across postures. Smallest detectable differences demonstrated that changes in performance of >1.3% in peak isometric force, >10.3% in mRFD, >5.3% in impulse at 100 ms, >4.4% in impulse at 200 ms, and >7.1% in impulse at 300 ms should be considered meaningful, irrespective of posture.

  17. A fibre-coupled UHV-compatible variable angle reflection-absorption UV/visible spectrometer

    Science.gov (United States)

    Stubbing, J. W.; Salter, T. L.; Brown, W. A.; Taj, S.; McCoustra, M. R. S.

    2018-05-01

    We present a novel UV/visible reflection-absorption spectrometer for determining the refractive index, n, and thicknesses, d, of ice films. Knowledge of the refractive index of these films is of particular relevance to the astrochemical community, where they can be used to model radiative transfer and spectra of various regions of space. In order to make these models more accurate, values of n need to be recorded under astronomically relevant conditions, that is, under ultra-high vacuum (UHV) and cryogenic cooling. Several design considerations were taken into account to allow UHV compatibility combined with ease of use. The key design feature is a stainless steel rhombus coupled to an external linear drive (z-shift) allowing a variable reflection geometry to be achieved, which is necessary for our analysis. Test data for amorphous benzene ice are presented as a proof of concept, the film thickness, d, was found to vary linearly with surface exposure, and a value for n of 1.43 ± 0.07 was determined.

  18. Variable-angle epifluorescence microscopy characterizes protein dynamics in the vicinity of plasma membrane in plant cells.

    Science.gov (United States)

    Chen, Tong; Ji, Dongchao; Tian, Shiping

    2018-03-14

    The assembly of protein complexes and compositional lipid patterning act together to endow cells with the plasticity required to maintain compositional heterogeneity with respect to individual proteins. Hence, the applications for imaging protein localization and dynamics require high accuracy, particularly at high spatio-temporal level. We provided experimental data for the applications of Variable-Angle Epifluorescence Microscopy (VAEM) in dissecting protein dynamics in plant cells. The VAEM-based co-localization analysis took penetration depth and incident angle into consideration. Besides direct overlap of dual-color fluorescence signals, the co-localization analysis was carried out quantitatively in combination with the methodology for calculating puncta distance and protein proximity index. Besides, simultaneous VAEM tracking of cytoskeletal dynamics provided more insights into coordinated responses of actin filaments and microtubules. Moreover, lateral motility of membrane proteins was analyzed by calculating diffusion coefficients and kymograph analysis, which represented an alternative method for examining protein motility. The present study presented experimental evidence on illustrating the use of VAEM in tracking and dissecting protein dynamics, dissecting endosomal dynamics, cell structure assembly along with membrane microdomain and protein motility in intact plant cells.

  19. Probing Metal Carbonation Reactions of CO2 in a Model System Containing Forsterite and H2O Using Si-29, C-13 Magic Angle Sample Spinning NMR Spectroscopy

    Science.gov (United States)

    Hu, J.; Kwak, J.; Hoyt, D. W.; Sears, J. A.; Rosso, K. M.; Felmy, A. R.

    2009-12-01

    Ex situ solid state NMR have been used for the first time to study fundamental mineral carbonation processes and reaction extent relevant to geologic carbon sequestration using a model silicate mineral forsterite (Mg2SiO4)+scCO2 with and without H2O. Run conditions were 80C and 96 bar. Si-29 NMR clearly shows that in the absence of CO2, the role of H2O is to hydrolyze surface Mg-O-Si bonds to produce Mg2+, and mono- and oligomeric hydroxylated silica species. The surface hydrolysis products contain only Q0 (Si(OH)4) and Q1 (Si(OH)3OSi) species. An equilibrium between Q0, Q1 and Mg2+ with a saturated concentration equivalent to less than 3.2% of the Mg2SiO4 conversion is obtained at a reaction time of up to 7 days. Using scCO2 without H2O, no reaction is observed within 7 days. Using both scCO2 and H2O, the surface reaction products for silica are mainly Q3 (SiOH(OSi)3) species accompanied by a lesser amount of Q2 (Si(OH)2(OSi)2) and Q4 (Si(OSi)4). However, no Q0 and Q1 were detected, indicating the carbonic acid formation/deprotonation and magnesite (MgCO3) precipitation reactions are faster than the forsterite hydrolysis process. Thus it can be concluded that the Mg2SiO4 hydrolysis process is the rate limiting step of the overall mineral carbonation process. Si-29 NMR combined with XRD, TEM, SAED and EDX further reveal that the reaction is a surface reaction with the Mg2SiO4 crystallite in the core and with condensed Q2-Q4 species forming amorphous surface layers. C-13 MAS NMR identified a possible reaction intermediates as (MgCO3)4*Mg(OH)2*5H2O. However, at long reaction times only crystallite magnesite MgCO3 products are observed. This research is part of a broader effort at PNNL to develop experimental tools and fundamental insights into chemical transformations affecting subsurface CO2 reactive transport. Si-29 (left) and C-13 (right) MAS NMR spectra of Mg2SiO4 under various reaction conditions. Si-29 NMR reveals that in scCO2 without H2O, no reaction is

  20. Non-targeted detection of chemical contamination in carbonated soft drinks using NMR spectroscopy, variable selection and chemometrics

    Energy Technology Data Exchange (ETDEWEB)

    Charlton, Adrian J. [Department for Environment, Food and Rural Affairs, Central Science Laboratory, Sand Hutton, York YO41 1LZ (United Kingdom)], E-mail: adrian.charlton@csl.gov.uk; Robb, Paul; Donarski, James A.; Godward, John [Department for Environment, Food and Rural Affairs, Central Science Laboratory, Sand Hutton, York YO41 1LZ (United Kingdom)

    2008-06-23

    An efficient method for detecting malicious and accidental contamination of foods has been developed using a combined {sup 1}H nuclear magnetic resonance (NMR) and chemometrics approach. The method has been demonstrated using a commercially available carbonated soft drink, as being capable of identifying atypical products and to identify contaminant resonances. Soft-independent modelling of class analogy (SIMCA) was used to compare {sup 1}H NMR profiles of genuine products (obtained from the manufacturer) against retail products spiked in the laboratory with impurities. The benefits of using feature selection for extracting contaminant NMR frequencies were also assessed. Using example impurities (paraquat, p-cresol and glyphosate) NMR spectra were analysed using multivariate methods resulting in detection limits of approximately 0.075, 0.2, and 0.06 mM for p-cresol, paraquat and glyphosate, respectively. These detection limits are shown to be approximately 100-fold lower than the minimum lethal dose for paraquat. The methodology presented here is used to assess the composition of complex matrices for the presence of contaminating molecules without a priori knowledge of the nature of potential contaminants. The ability to detect if a sample does not fit into the expected profile without recourse to multiple targeted analyses is a valuable tool for incident detection and forensic applications.

  1. Non-targeted detection of chemical contamination in carbonated soft drinks using NMR spectroscopy, variable selection and chemometrics

    International Nuclear Information System (INIS)

    Charlton, Adrian J.; Robb, Paul; Donarski, James A.; Godward, John

    2008-01-01

    An efficient method for detecting malicious and accidental contamination of foods has been developed using a combined 1 H nuclear magnetic resonance (NMR) and chemometrics approach. The method has been demonstrated using a commercially available carbonated soft drink, as being capable of identifying atypical products and to identify contaminant resonances. Soft-independent modelling of class analogy (SIMCA) was used to compare 1 H NMR profiles of genuine products (obtained from the manufacturer) against retail products spiked in the laboratory with impurities. The benefits of using feature selection for extracting contaminant NMR frequencies were also assessed. Using example impurities (paraquat, p-cresol and glyphosate) NMR spectra were analysed using multivariate methods resulting in detection limits of approximately 0.075, 0.2, and 0.06 mM for p-cresol, paraquat and glyphosate, respectively. These detection limits are shown to be approximately 100-fold lower than the minimum lethal dose for paraquat. The methodology presented here is used to assess the composition of complex matrices for the presence of contaminating molecules without a priori knowledge of the nature of potential contaminants. The ability to detect if a sample does not fit into the expected profile without recourse to multiple targeted analyses is a valuable tool for incident detection and forensic applications

  2. A novel Bayesian approach to quantify clinical variables and to determine their spectroscopic counterparts in 1H NMR metabonomic data

    Directory of Open Access Journals (Sweden)

    Kaski Kimmo

    2007-05-01

    Full Text Available Abstract Background A key challenge in metabonomics is to uncover quantitative associations between multidimensional spectroscopic data and biochemical measures used for disease risk assessment and diagnostics. Here we focus on clinically relevant estimation of lipoprotein lipids by 1H NMR spectroscopy of serum. Results A Bayesian methodology, with a biochemical motivation, is presented for a real 1H NMR metabonomics data set of 75 serum samples. Lipoprotein lipid concentrations were independently obtained for these samples via ultracentrifugation and specific biochemical assays. The Bayesian models were constructed by Markov chain Monte Carlo (MCMC and they showed remarkably good quantitative performance, the predictive R-values being 0.985 for the very low density lipoprotein triglycerides (VLDL-TG, 0.787 for the intermediate, 0.943 for the low, and 0.933 for the high density lipoprotein cholesterol (IDL-C, LDL-C and HDL-C, respectively. The modelling produced a kernel-based reformulation of the data, the parameters of which coincided with the well-known biochemical characteristics of the 1H NMR spectra; particularly for VLDL-TG and HDL-C the Bayesian methodology was able to clearly identify the most characteristic resonances within the heavily overlapping information in the spectra. For IDL-C and LDL-C the resulting model kernels were more complex than those for VLDL-TG and HDL-C, probably reflecting the severe overlap of the IDL and LDL resonances in the 1H NMR spectra. Conclusion The systematic use of Bayesian MCMC analysis is computationally demanding. Nevertheless, the combination of high-quality quantification and the biochemical rationale of the resulting models is expected to be useful in the field of metabonomics.

  3. Buffer-induced swelling and vesicle budding in binary lipid mixtures of dioleoylphosphatidylcholine:dioleoylphosphatidylethanolamine and dioleoylphosphatidylcholine:lysophosphatidylcholine using small-angle X-ray scattering and ³¹P static NMR.

    Science.gov (United States)

    Barriga, Hanna M G; Bazin, Richard; Templer, Richard H; Law, Robert V; Ces, Oscar

    2015-03-17

    A large variety of data exists on lipid phase behavior; however, it is mostly in nonbuffered systems over nonbiological temperature ranges. We present biophysical data on lipid mixtures of dioleoylphosphatidylcholine (DOPC), dioleoylphosphatidylethanolamine (DOPE), and lysophosphatidylcholine (LysoPC) examining their behaviors in excess water and buffer systems over the temperature range 4-34 °C. These mixtures are commonly used to investigate the effects of spontaneous curvature on integral membrane proteins. Using small-angle X-ray scattering (SAXS) and (31)P NMR, we observed lamellar and vesicle phases, with the buffer causing an increase in the layer spacing. Increasing amounts of DOPE in a DOPC bilayer decreased the layer spacing of the mesophase, while the opposite trend was observed for increasing amounts of LysoPC. (31)P static NMR was used to analyze the DOPC:LysoPC samples to investigate the vesicle sizes present, with evidence of vesicle budding observed at LysoPC concentrations above 30 mol %. NMR line shapes were fitted using an adapted program accounting for the distortion of the lipids within the magnetic field. The distortion of the vesicle, because of magnetic susceptibility, varied with LysoPC content, and a discontinuity was found in both the water and buffer samples. Generally, the distortion increased with LysoPC content; however, at a ratio of DOPC:LysoPC 60:40, the sample showed a level of distortion of the vesicle similar to that of pure DOPC. This implies an increased flexibility in the membrane at this point. Commonly, the assumption is that for increasing LysoPC concentration there is a reduction in membrane tension, implying that estimations of membrane tension based on spontaneous curvature assumptions may not be accurate.

  4. High-resolution magic angle spinning 1H-NMR spectroscopy studies on the renal biochemistry in the bank vole (Clethrionomys glareolus) and the effects of arsenic (As3+) toxicity.

    Science.gov (United States)

    Griffin, J L; Walker, L; Shore, R F; Nicholson, J K

    2001-06-01

    1. High-resolution magic angle spinning (MAS) 1H-NMR spectroscopy was used to study renal metabolism and the toxicity of As3+, a common environmental contaminant, in the bank vole (Clethrionomys glareolus), a wild species of rodent. 2. Following a 14-day exposure to an environmentally relevant dose of As2O3 (28 mg kg(-1) feed), voles displayed tissue damage at autopsy. MAS 1H spectra indicated abnormal lipid profiles in these samples. 3. Tissue necrosis was also evident from measurements of the apparent diffusion coefficient of water in the intact tissue using MAS 1H diffusion-weighted spectroscopy, its first application to toxicology. 4. Comparison of renal tissue from the wood mouse (Apodemus sylvaticus) exposed to identical exposure levels of As3+ suggested that the bank vole is particularly vulnerable to As3+ toxicity.

  5. Midterm Follow-up of Treating Volar Marginal Rim Fractures with Variable Angle Lcp Volar Rim Distal Radius Plates.

    Science.gov (United States)

    Goorens, Chul Ki; Geeurickx, Stijn; Wernaers, Pascal; Staelens, Barbara; Scheerlinck, Thierry; Goubau, Jean

    2017-06-01

    Specific treatment of the volar marginal rim fragment of distal radius fractures avoids occurance of volar radiocarpal dislocation. Although several fixation systems are available to capture this fragment, adequately maintaining internal fixation is difficult. We present our experience of the first 10 cases using the 2.4 mm variable angle LCP volar rim distal radius plate (Depuy Synthes®, West Chester, US), a low-profile volar rim-contouring plate designed for distal plate positioning and stable buttressing of the volar marginal fragment. Follow-up patient satisfaction, range of motion, grips strength, functional scoring with the QuickDASH and residual pain with a numeric rating scale were assessed. Radiological evaluation consisted in evaluating fracture consolidation, ulnar variance, volar angulation and maintenance of the volar rim fixation. The female to male ratio was 5:5 and the mean age was 52.2 (range, 17-80) years. The mean follow-up period was 11 (range, 5-19) months postoperatively. Patient satisfaction was high. The mean total flexion/extension range was 144° (range, 100-180°) compared to the contralateral uninjured side 160° (range, 95-180°). The mean total pronation/supination range was 153° (range, 140-180°) compared to the contralateral uninjured side 170° (range, 155-180°). Mean grip strength was 14 kg (range, 9-22), compared to the contralateral uninjured side 20 kg (range, 12-25 kg). Mean pre-injury level activity QuickDASH was 23 (range, 0-34.1), while post-recovery QuickDASH was 25 (range 0-43.2). Residual pain was 1.5 on the visual numerical pain rating scale. Radiological evaluation revealed in all cases fracture consolidation, satisfactory reconstruction of ulnar variance, volar angulation and volar rim. We encountered no flexor tendon complications, although plate removal was systematically performed after fracture consolidation. The 2.4 mm variable angle LCP volar rim distal radius plates is a valid treatment option for treating

  6. Comparison of Newly Diagnosed Ocular Hypertension and Open-Angle Glaucoma: Ocular Variables, Risk Factors, and Disease Severity

    Directory of Open Access Journals (Sweden)

    Yvonne M. Buys

    2012-01-01

    Full Text Available Purpose. To describe the distribution of ocular variables, risk factors, and disease severity in newly diagnosed ocular hypertension (OH or open-angle glaucoma (OAG. Methods. Eligible subjects underwent a complete history and examination. Adjusted odds ratios (ORs and 95% confidence intervals (CIs obtained from multiple logistic regression models were used to compare OAG to OH and advanced to early/moderate OAG. Results. 405 subjects were enrolled: 292 (72.1% with OAG and 113 (27.9% with OH. 51.7% had early, 27.1% moderate, and 20.9% advanced OAG. The OR for OAG versus OH was 8.19 (P<0.0001 for disc notch, 5.36 (P<0.0001 for abnormal visual field, 1.45 (P=0.001 for worsening mean deviation, 1.91 (P<0.0001 for increased cupping, 1.03 for increased age (P=0.030, and 0.36 (P=0.010 for smoking. Conclusions. Increased age was a risk for OAG, and smoking decreased the risk of OAG compared to OH. Almost half of the OAG subjects had moderate/advanced disease at diagnosis.

  7. Application of 1H and 23Na magic angle spinning NMR spectroscopy to define the HRBC up-taking of MRI contrast agents

    Science.gov (United States)

    Calabi, Luisella; Paleari, Lino; Biondi, Luca; Linati, Laura; De Miranda, Mario; Ghelli, Stefano

    2003-09-01

    The up-take of Gd(III) complexes of BOPTA, DTPA, DOTA, EDTP, HPDO3A, and DOTP in HRBC has been evaluated by measuring the lanthanide induced shift (LIS) produced by the corresponding dysprosium complexes (DC) on the MAS-NMR resonances of water protons and free sodium ions. These complexes are important in their use as MRI contrast agents (MRI-CA) in diagnostics. 1H and 23Na MAS-NMR spectra of HRBC suspension, collected at 9.395 T, show only one signal due to extra- and intra-cellular water (or sodium). In MAS spectra, the presence of DC in a cellular compartment produces the LIS of only the nuclei (water proton or sodium) in that cellular compartment and this LIS can be related to the DC concentrations (by the experimental curves of LIS vs. DC concentrations) collected in the physiological solution. To obtain correct results about LIS, the use of MAS technique is mandatory, because it guarantees the only the nuclei staying in the same cellular compartment where the LC is present show the LIS. In all the cases considered, the addition of the DC to HRBC (100% hematocrit) produced a shift of only the extra-cellular water (or sodium) signal and the gradient of concentration ( GC) between extra- and intra-cellular compartments resulted greater than 100:1, when calculated by means of sodium signals. These high values of GC are direct proofs that none of the tested dysprosium complexes crosses the HRBC membrane. Since the DC are iso-structural to the gadolinium complexes the corresponding gadolinium ones (MRI-CA) do not cross the HRBC membrane and, consequently, they are not up-taken in HRBC. The GC values calculated by means of water proton signals resulted much lower than those obtained by sodium signals. This proves that the choice of the isotope is a crucial step in order to use this method in the best way. In fact, GC value depends on the lowest detectable LIS which, in turn, depends on the nature of the LC (lanthanide complex) and the observed isotopes.

  8. Mesoporous Silica Nanoparticles Loaded with Surfactant: Low Temperature Magic Angle Spinning 13C and 29Si NMR Enhanced by Dynamic Nuclear Polarization

    Energy Technology Data Exchange (ETDEWEB)

    Lafon, Olivier [Universite de Lille Nord de France; Thankamony, Aany S. Lilly [Universite de Lille Nord de France; Kokayashi, Takeshi [Ames Laboratory; Carnevale, Diego [Ecole Polytechnique Federale de Lausanne; Vitzthum, Veronika [Ecole Polytechnique Federale de Lausanne; Slowing, Igor I. [Ames Laboratory; Kandel, Kapil [Ames Laboratory; Vezin, Herve [Universite de Lille Nord de France; Amoureux, Jean-Paul [Universite de Lille Nord de France; Bodenhausen, Geoffrey [Ecole Polytechnique Federale de Lausanne; Pruski, Marek [Ames Laboratory

    2012-12-21

    We show that dynamic nuclear polarization (DNP) can be used to enhance NMR signals of 13C and 29Si nuclei located in mesoporous organic/inorganic hybrid materials, at several hundreds of nanometers from stable radicals (TOTAPOL) trapped in the surrounding frozen disordered water. The approach is demonstrated using mesoporous silica nanoparticles (MSN), functionalized with 3-(N-phenylureido)propyl (PUP) groups, filled with the surfactant cetyltrimethylammonium bromide (CTAB). The DNP-enhanced proton magnetization is transported into the mesopores via 1H–1H spin diffusion and transferred to rare spins by cross-polarization, yielding signal enhancements εon/off of around 8. When the CTAB molecules are extracted, so that the radicals can enter the mesopores, the enhancements increase to εon/off ≈ 30 for both nuclei. A quantitative analysis of the signal enhancements in MSN with and without surfactant is based on a one-dimensional proton spin diffusion model. The effect of solvent deuteration is also investigated.

  9. Rapid assessment of pulmonary gas transport with hyperpolarized 129Xe MRI using a 3D radial double golden-means acquisition with variable flip angles.

    Science.gov (United States)

    Ruppert, Kai; Amzajerdian, Faraz; Hamedani, Hooman; Xin, Yi; Loza, Luis; Achekzai, Tahmina; Duncan, Ian F; Profka, Harrilla; Siddiqui, Sarmad; Pourfathi, Mehrdad; Cereda, Maurizio F; Kadlecek, Stephen; Rizi, Rahim R

    2018-04-22

    To demonstrate the feasibility of using a 3D radial double golden-means acquisition with variable flip angles to monitor pulmonary gas transport in a single breath hold with hyperpolarized xenon-129 MRI. Hyperpolarized xenon-129 MRI scans with interleaved gas-phase and dissolved-phase excitations were performed using a 3D radial double golden-means acquisition in mechanically ventilated rabbits. The flip angle was either held fixed at 15 ° or 5 °, or it was varied linearly in ascending or descending order between 5 ° and 15 ° over a sampling interval of 1000 spokes. Dissolved-phase and gas-phase images were reconstructed at high resolution (32 × 32 × 32 matrix size) using all 1000 spokes, or at low resolution (22 × 22 × 22 matrix size) using 400 spokes at a time in a sliding-window fashion. Based on these sliding-window images, relative change maps were obtained using the highest mean flip angle as the reference, and aggregated pixel-based changes were tracked. Although the signal intensities in the dissolve-phase maps were mostly constant in the fixed flip-angle acquisitions, they varied significantly as a function of average flip angle in the variable flip-angle acquisitions. The latter trend reflects the underlying changes in observed dissolve-phase magnetization distribution due to pulmonary gas uptake and transport. 3D radial double golden-means acquisitions with variable flip angles provide a robust means for rapidly assessing lung function during a single breath hold, thereby constituting a particularly valuable tool for imaging uncooperative or pediatric patient populations. © 2018 International Society for Magnetic Resonance in Medicine.

  10. Accurate measurement of heteronuclear dipolar couplings by phase-alternating R-symmetry (PARS) sequences in magic angle spinning NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Guangjin, E-mail: hou@udel.edu, E-mail: tpolenov@udel.edu; Lu, Xingyu, E-mail: luxingyu@udel.edu, E-mail: lexvega@comcast.net; Vega, Alexander J., E-mail: luxingyu@udel.edu, E-mail: lexvega@comcast.net; Polenova, Tatyana, E-mail: hou@udel.edu, E-mail: tpolenov@udel.edu [Department of Chemistry and Biochemistry, University of Delaware, Newark, Delaware 19716, USA and Pittsburgh Center for HIV Protein Interactions, University of Pittsburgh School of Medicine, 1051 Biomedical Science Tower 3, 3501 Fifth Ave., Pittsburgh, Pennsylvania 15261 (United States)

    2014-09-14

    We report a Phase-Alternating R-Symmetry (PARS) dipolar recoupling scheme for accurate measurement of heteronuclear {sup 1}H-X (X = {sup 13}C, {sup 15}N, {sup 31}P, etc.) dipolar couplings in MAS NMR experiments. It is an improvement of conventional C- and R-symmetry type DIPSHIFT experiments where, in addition to the dipolar interaction, the {sup 1}H CSA interaction persists and thereby introduces considerable errors in the dipolar measurements. In PARS, phase-shifted RN symmetry pulse blocks applied on the {sup 1}H spins combined with π pulses applied on the X spins at the end of each RN block efficiently suppress the effect from {sup 1}H chemical shift anisotropy, while keeping the {sup 1}H-X dipolar couplings intact. Another advantage over conventional DIPSHIFT experiments, which require the signal to be detected in the form of a reduced-intensity Hahn echo, is that the series of π pulses refocuses the X chemical shift and avoids the necessity of echo formation. PARS permits determination of accurate dipolar couplings in a single experiment; it is suitable for a wide range of MAS conditions including both slow and fast MAS frequencies; and it assures dipolar truncation from the remote protons. The performance of PARS is tested on two model systems, [{sup 15}N]-N-acetyl-valine and [U-{sup 13}C,{sup 15}N]-N-formyl-Met-Leu-Phe tripeptide. The application of PARS for site-resolved measurement of accurate {sup 1}H-{sup 15}N dipolar couplings in the context of 3D experiments is presented on U-{sup 13}C,{sup 15}N-enriched dynein light chain protein LC8.

  11. Q(n) species distribution in K2O.2SiO2 glass by 29Si magic angle flipping NMR.

    Science.gov (United States)

    Davis, Michael C; Kaseman, Derrick C; Parvani, Sahar M; Sanders, Kevin J; Grandinetti, Philip J; Massiot, Dominique; Florian, Pierre

    2010-05-06

    Two-dimensional magic angle flipping (MAF) was employed to measure the Q((n)) distribution in a (29)Si-enriched potassium disilicate glass (K(2)O.2SiO(2)). Relative concentrations of [Q((4))] = 7.2 +/- 0.3%, [Q((3))] = 82.9 +/- 0.1%, and [Q((2))] = 9.8 +/- 0.6% were obtained. Using the thermodynamic model for Q((n)) species disproportionation, these relative concentrations yield an equilibrium constant k(3) = 0.0103 +/- 0.0008, indicating, as expected, that the Q((n)) species distribution is close to binary in the potassium disilicate glass. A Gaussian distribution of isotropic chemical shifts was observed for each Q((n)) species with mean values of -82.74 +/- 0.03, -91.32 +/- 0.01, and -101.67 +/- 0.02 ppm and standard deviations of 3.27 +/- 0.03, 4.19 +/- 0.01, and 5.09 +/- 0.03 ppm for Q((2)), Q((3)), and Q((4)), respectively. Additionally, nuclear shielding anisotropy values of zeta =-85.0 +/- 1.3 ppm, eta = 0.48 +/- 0.02 for Q((2)) and zeta = -74.9 +/- 0.2 ppm, eta = 0.03 +/- 0.01 for Q((3)) were observed in the potassium disilicate glass.

  12. Variable flip angle 3D ultrashort echo time (UTE) T1 mapping of mouse lung: A repeatability assessment.

    Science.gov (United States)

    Alamidi, Daniel F; Smailagic, Amir; Bidar, Abdel W; Parker, Nicole S; Olsson, Marita; Hockings, Paul D; Lagerstrand, Kerstin M; Olsson, Lars E

    2018-03-08

    Lung T 1 is a potential translational biomarker of lung disease. The precision and repeatability of variable flip angle (VFA) T 1 mapping using modern 3D ultrashort echo time (UTE) imaging of the whole lung needs to be established before it can be used to assess response to disease and therapy. To evaluate the feasibility of regional lung T 1 quantification with VFA 3D-UTE and to investigate long- and short-term T 1 repeatability in the lungs of naive mice. Prospective preclinical animal study. Eight naive mice and phantoms. 3D free-breathing radial UTE (8 μs) at 4.7T. VFA 3D-UTE T 1 calculations were validated against T 1 values measured with inversion recovery (IR) in phantoms. Lung T 1 and proton density (S 0 ) measurements of whole lung and muscle were repeated five times over 1 month in free-breathing naive mice. Two consecutive T 1 measurements were performed during one of the imaging sessions. Agreement in T 1 between VFA 3D-UTE and IR in phantoms was assessed using Bland-Altman and Pearson 's correlation analysis. The T 1 repeatability in mice was evaluated using coefficient of variation (CV), repeated-measures analysis of variance (ANOVA), and paired t-test. Good T 1 agreement between the VFA 3D-UTE and IR methods was found in phantoms. T 1 in lung and muscle showed a 5% and 3% CV (1255 ± 63 msec and 1432 ± 42 msec, respectively, mean ± SD) with no changes in T 1 or S 0 over a month. Consecutive measurements resulted in an increase of 2% in both lung T 1 and S 0 . VFA 3D-UTE shows promise as a reliable T 1 mapping method that enables full lung coverage, high signal-to-noise ratio (∼25), and spatial resolution (300 μm) in freely breathing animals. The precision of the VFA 3D-UTE method will enable better design and powering of studies. 1 Technical Efficacy: Stage 2 J. Magn. Reson. Imaging 2018. © 2018 International Society for Magnetic Resonance in Medicine.

  13. Structural properties of carbon nanotubes derived from 13C NMR

    KAUST Repository

    Abou-Hamad, E.; Babaa, M.-R.; Bouhrara, M.; Kim, Y.; Saih, Y.; Dennler, S.; Mauri, F.; Basset, Jean-Marie; Goze-Bac, C.; Wå gberg, T.

    2011-01-01

    We present a detailed experimental and theoretical study on how structural properties of carbon nanotubes can be derived from 13C NMR investigations. Magic angle spinning solid state NMR experiments have been performed on single- and multiwalled

  14. Study of solid chemical evolution in torrefaction of different biomasses through solid-state "1"3C cross-polarization/magic angle spinning NMR (nuclear magnetic resonance) and TGA (thermogravimetric analysis)

    International Nuclear Information System (INIS)

    Rodriguez Alonso, Elvira; Dupont, Capucine; Heux, Laurent; Da Silva Perez, Denilson; Commandre, Jean-Michel; Gourdon, Christophe

    2016-01-01

    The objective of this work is to compare mass loss and chemical evolution of the solid phase, versus time, during dynamic torrefaction of different types of biomass. For this purpose, two experiments, ThermoGravimetric Analysis and solid-state "1"3C Cross-Polarization/Magic Angle Spinning Nuclear Magnetic Resonance, were run on four representative biomasses. Overall mass loss and chemical evolution of the solid phase were followed, respectively, as a function of temperature and time. Thanks to this coupled information, it was shown that the knowledge of both solid mass loss and chemical evolution is necessary to characterize torrefaction severity. Moreover, biomasses containing higher proportions of xylan lost mass faster than those containing lower proportions. Lignin showed a protecting role towards cellulose, which would lead to a faster degradation of non-woody biomasses in comparison with woody biomasses. Three parameters would have an influence on solid chemical evolution during torrefaction: xylan content in hemicellulose, lignin content in biomass, and cellulose crystallinity. - Highlights: • Torrefaction of four biomasses was studied with TGA and solid-state NMR. • Both solid mass loss and chemical evolution characterize torrefaction severity. • Biomasses containing a higher proportion of xylan lose mass faster. • Lignin shows a stronger protecting role in degradation of woody biomasses. • Xylan, lignin and crystalline cellulose values influence solid chemical evolution.

  15. Variable field-to-normal angles in the shock foreshock boundary observed by ISEE 1 and 2

    International Nuclear Information System (INIS)

    Greenstadt, E.W.; Mellot, M.M.

    1985-01-01

    Saturated ULF waves in the foreshock, with amplitudes comparable to the magnitude of the average field, are convected by the solar wind to the quasi-parallel shock where the average field-normal angle is less than, or about, 45 0 . Several examples from ISEE 1 and 2 magnetometer data show waves that defined local, instantaneous field-normal angles very different periodically from the average. Local geometric conditions at the nominally quasi-parallel shock varied from nearly parallel to nearly perpendicular, at the periods of typical upstream waves. Clear magnetic shock transitions occurred under temporarily quasi-perpendicular geometry

  16. High accuracy subwavelength distance measurements: A variable-angle standing-wave total-internal-reflection optical microscope

    International Nuclear Information System (INIS)

    Haynie, A.; Min, T.-J.; Luan, L.; Mu, W.; Ketterson, J. B.

    2009-01-01

    We describe an extension of the total-internal-reflection microscopy technique that permits direct in-plane distance measurements with high accuracy (<10 nm) over a wide range of separations. This high position accuracy arises from the creation of a standing evanescent wave and the ability to sweep the nodal positions (intensity minima of the standing wave) in a controlled manner via both the incident angle and the relative phase of the incoming laser beams. Some control over the vertical resolution is available through the ability to scan the incoming angle and with it the evanescent penetration depth.

  17. Adaptive sliding mode back-stepping pitch angle control of a variable-displacement pump controlled pitch system for wind turbines.

    Science.gov (United States)

    Yin, Xiu-xing; Lin, Yong-gang; Li, Wei; Liu, Hong-wei; Gu, Ya-jing

    2015-09-01

    A variable-displacement pump controlled pitch system is proposed to mitigate generator power and flap-wise load fluctuations for wind turbines. The pitch system mainly consists of a variable-displacement hydraulic pump, a fixed-displacement hydraulic motor and a gear set. The hydraulic motor can be accurately regulated by controlling the pump displacement and fluid flows to change the pitch angle through the gear set. The detailed mathematical representation and dynamic characteristics of the proposed pitch system are thoroughly analyzed. An adaptive sliding mode pump displacement controller and a back-stepping stroke piston controller are designed for the proposed pitch system such that the resulting pitch angle tracks its desired value regardless of external disturbances and uncertainties. The effectiveness and control efficiency of the proposed pitch system and controllers have been verified by using realistic dataset of a 750 kW research wind turbine. Copyright © 2015 ISA. Published by Elsevier Ltd. All rights reserved.

  18. Action-angle variables for spherical mechanics related to near horizon extremal Myers–Perry black hole

    International Nuclear Information System (INIS)

    Galajinsky, Anton; Nersessian, Armen; Saghatelian, Armen

    2013-01-01

    The action-angle formulation for the spherical part of the conformal mechanics describing a massive relativistic particle moving near the horizon of an extremal rotating black hole in arbitrary dimension is presented for the special case that all rotation parameters are equal

  19. Morphology control of tungsten nanorods grown by glancing angle RF magnetron sputtering under variable argon pressure and flow rate

    International Nuclear Information System (INIS)

    Khedir, Khedir R.; Kannarpady, Ganesh K.; Ishihara, Hidetaka; Woo, Justin; Ryerson, Charles; Biris, Alexandru S.

    2010-01-01

    Morphologically novel tungsten nanorods (WNRs) with the co-existence of two crystalline phases, α-W (thermodynamically stable) and β-W, were fabricated by glancing angle RF magnetron sputtering technique under various Ar pressures and flow rates. For these nanorods, a significant variation in their morphology and surface roughness was observed. These structures could be useful in a wide range of applications such as field emission, robust superhydrophobic coatings, energy, and medicine.

  20. Variability of photovoltaic panels efficiency depending on the value of the angle of their inclination relative to the horizon

    OpenAIRE

    Majdak Marek

    2017-01-01

    The objective of this paper was to determine the relationship between the efficiency of photovoltaic panels and the value of the angle of their inclination relative to the horizon. For the purpose of experimental research have been done tests on the photovoltaic modules made of monocrystalline, polycrystalline and amorphous silicon. The experiment consisted of measurement of the voltage and current generated by photovoltaic panels at a known value of solar radiation and a specified resistance...

  1. Nano-Mole Scale Side-Chain Signal Assignment by 1H-Detected Protein Solid-State NMR by Ultra-Fast Magic-Angle Spinning and Stereo-Array Isotope Labeling

    KAUST Repository

    Wang, Songlin

    2015-04-09

    We present a general approach in 1H-detected 13C solid-state NMR (SSNMR) for side-chain signal assignments of 10-50 nmol quantities of proteins using a combination of a high magnetic field, ultra-fast magic-angle spinning (MAS) at ~80 kHz, and stereo-array-isotope-labeled (SAIL) proteins [Kainosho M. et al., Nature 440, 52–57, 2006]. First, we demonstrate that 1H indirect detection improves the sensitivity and resolution of 13C SSNMR of SAIL proteins for side-chain assignments in the ultra-fast MAS condition. 1H-detected SSNMR was performed for micro-crystalline ubiquitin (~55 nmol or ~0.5mg) that was SAIL-labeled at seven isoleucine (Ile) residues. Sensitivity was dramatically improved by 1H-detected 2D 1H/13C SSNMR by factors of 5.4-9.7 and 2.1-5.0, respectively, over 13C-detected 2D 1H/13C SSNMR and 1D 13C CPMAS, demonstrating that 2D 1H-detected SSNMR offers not only additional resolution but also sensitivity advantage over 1D 13C detection for the first time. High 1H resolution for the SAIL-labeled side-chain residues offered reasonable resolution even in the 2D data. A 1H-detected 3D 13C/13C/1H experiment on SAIL-ubiquitin provided nearly complete 1H and 13C assignments for seven Ile residues only within ~2.5 h. The results demonstrate the feasibility of side-chain signal assignment in this approach for as little as 10 nmol of a protein sample within ~3 days. The approach is likely applicable to a variety of proteins of biological interest without any requirements of highly efficient protein expression systems.

  2. Nano-Mole Scale Side-Chain Signal Assignment by 1H-Detected Protein Solid-State NMR by Ultra-Fast Magic-Angle Spinning and Stereo-Array Isotope Labeling

    KAUST Repository

    Wang, Songlin; Parthasarathy, Sudhakar; Nishiyama, Yusuke; Endo, Yuki; Nemoto, Takahiro; Yamauchi, Kazuo; Asakura, Tetsuo; Takeda, Mitsuhiro; Terauchi, Tsutomu; Kainosho, Masatsune; Ishii, Yoshitaka

    2015-01-01

    We present a general approach in 1H-detected 13C solid-state NMR (SSNMR) for side-chain signal assignments of 10-50 nmol quantities of proteins using a combination of a high magnetic field, ultra-fast magic-angle spinning (MAS) at ~80 kHz, and stereo-array-isotope-labeled (SAIL) proteins [Kainosho M. et al., Nature 440, 52–57, 2006]. First, we demonstrate that 1H indirect detection improves the sensitivity and resolution of 13C SSNMR of SAIL proteins for side-chain assignments in the ultra-fast MAS condition. 1H-detected SSNMR was performed for micro-crystalline ubiquitin (~55 nmol or ~0.5mg) that was SAIL-labeled at seven isoleucine (Ile) residues. Sensitivity was dramatically improved by 1H-detected 2D 1H/13C SSNMR by factors of 5.4-9.7 and 2.1-5.0, respectively, over 13C-detected 2D 1H/13C SSNMR and 1D 13C CPMAS, demonstrating that 2D 1H-detected SSNMR offers not only additional resolution but also sensitivity advantage over 1D 13C detection for the first time. High 1H resolution for the SAIL-labeled side-chain residues offered reasonable resolution even in the 2D data. A 1H-detected 3D 13C/13C/1H experiment on SAIL-ubiquitin provided nearly complete 1H and 13C assignments for seven Ile residues only within ~2.5 h. The results demonstrate the feasibility of side-chain signal assignment in this approach for as little as 10 nmol of a protein sample within ~3 days. The approach is likely applicable to a variety of proteins of biological interest without any requirements of highly efficient protein expression systems.

  3. 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...

  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. Improved imaging of cochlear nerve hypoplasia using a 3-Tesla variable flip-angle turbo spin-echo sequence and a 7-cm surface coil.

    Science.gov (United States)

    Giesemann, Anja M; Raab, Peter; Lyutenski, Stefan; Dettmer, Sabine; Bültmann, Eva; Frömke, Cornelia; Lenarz, Thomas; Lanfermann, Heinrich; Goetz, Friedrich

    2014-03-01

    Magnetic resonance imaging of the temporal bone has an important role in decision making with regard to cochlea implantation, especially in children with cochlear nerve deficiency. The purpose of this study was to evaluate the usefulness of the combination of an advanced high-resolution T2-weighted sequence with a surface coil in a 3-Tesla magnetic resonance imaging scanner in cases of suspected cochlear nerve aplasia. Prospective study. Seven patients with cochlear nerve hypoplasia or aplasia were prospectively examined using a high-resolution three-dimensional variable flip-angle turbo spin-echo sequence using a surface coil, and the images were compared with the same sequence in standard resolution using a standard head coil. Three neuroradiologists evaluated the magnetic resonance images independently, rating the visibility of the nerves in diagnosing hypoplasia or aplasia. Eight ears in seven patients with hypoplasia or aplasia of the cochlear nerve were examined. The average age was 2.7 years (range, 9 months-5 years). Seven ears had accompanying malformations. The inter-rater reliability in diagnosing hypoplasia or aplasia was greater using the high-resolution three-dimensional variable flip-angle turbo spin-echo sequence (fixed-marginal kappa: 0.64) than with the same sequence in lower resolution (fixed-marginal kappa: 0.06). Examining cases of suspected cochlear nerve aplasia using the high-resolution three-dimensional variable flip-angle turbo spin-echo sequence in combination with a surface coil shows significant improvement over standard methods. © 2013 The American Laryngological, Rhinological and Otological Society, Inc.

  6. Normal mode analysis based on an elastic network model for biomolecules in the Protein Data Bank, which uses dihedral angles as independent variables.

    Science.gov (United States)

    Wako, Hiroshi; Endo, Shigeru

    2013-06-01

    We have developed a computer program, named PDBETA, that performs normal mode analysis (NMA) based on an elastic network model that uses dihedral angles as independent variables. Taking advantage of the relatively small number of degrees of freedom required to describe a molecular structure in dihedral angle space and a simple potential-energy function independent of atom types, we aimed to develop a program applicable to a full-atom system of any molecule in the Protein Data Bank (PDB). The algorithm for NMA used in PDBETA is the same as the computer program FEDER/2, developed previously. Therefore, the main challenge in developing PDBETA was to find a method that can automatically convert PDB data into molecular structure information in dihedral angle space. Here, we illustrate the performance of PDBETA with a protein-DNA complex, a protein-tRNA complex, and some non-protein small molecules, and show that the atomic fluctuations calculated by PDBETA reproduce the temperature factor data of these molecules in the PDB. A comparison was also made with elastic-network-model based NMA in a Cartesian-coordinate system. Copyright © 2013 Elsevier Ltd. All rights reserved.

  7. Studies on Inx(As2Se31-x thin films using variable angle spectroscopic ellipsometry (VASE

    Directory of Open Access Journals (Sweden)

    Amin G. A. M.

    2015-09-01

    Full Text Available The results of multi-angle ellipsometrical measurements of thermally evaporated Inx(As2Se31-x (x = 0, 0.01,0.05 films are presented. Optical parameters n and Es of thin Inx(As2Se31-x films show that indium atoms were incorporated into the host matrix of As2Se3 forming distinct features depending on the indium concentration. Refractive index, n, was found to decrease with the addition of In to the binary As2Se3. The real and imaginary parts of the dielectric function, ε' and ε" were also calculated from the obtained data and correlated with In concentration. It was found that e' decreases with the increase of In content while ε" increases with the increase of In content. Absorption edge is shifted towards lower photon energy with the increase of In content. As a result, the optical energy gap decreases with increasing In content. This has been correlated with the chemical character of the additive as well as with the structural and bonding aspects of the amorphous composition. Nonlinear optical constants (χ(3 and n2 were determined from linear optical parameters using semi-empirical relations in the long wavelength limit.

  8. 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.

  9. The effect of pressure, isotopic (H/D) substitution, and other variables on miscibility in polymer-solvent systems. The nature of the demixing process; dynamic light scattering and small angle neutron scattering studies. Final report

    International Nuclear Information System (INIS)

    Van Hook, W.A.

    2000-01-01

    A research program examining the effects of pressure, isotope substitution and other variables on miscibility in polymer solvent systems is described. The techniques employed included phase equilibrium measurements and dynamic light scattering and small angle neutron scattering

  10. Methods of NMR structure refinement: molecular dynamics simulations improve the agreement with measured NMR data of a C-terminal peptide of GCN4-p1

    International Nuclear Information System (INIS)

    Dolenc, Jozica; Missimer, John H.; Steinmetz, Michel O.; Gunsteren, Wilfred F. van

    2010-01-01

    The C-terminal trigger sequence is essential in the coiled-coil formation of GCN4-p1; its conformational properties are thus of importance for understanding this process at the atomic level. A solution NMR model structure of a peptide, GCN4p16-31, encompassing the GCN4-p1 trigger sequence was proposed a few years ago. Derived using a standard single-structure refinement protocol based on 172 nuclear Overhauser effect (NOE) distance restraints, 14 hydrogen-bond and 11 φ torsional-angle restraints, the resulting set of 20 NMR model structures exhibits regular α-helical structure. However, the set slightly violates some measured NOE bounds and does not reproduce all 15 measured 3 J(H N -H Cα )-coupling constants, indicating that different conformers of GCN4p16-31 might be present in solution. With the aim to resolve structures compatible with all NOE upper distance bounds and 3 J-coupling constants, we executed several structure refinement protocols employing unrestrained and restrained molecular dynamics (MD) simulations with two force fields. We find that only configurational ensembles obtained by applying simultaneously time-averaged NOE distance and 3 J-coupling constant restraining with either force field reproduce all the experimental data. Additionally, analyses of the simulated ensembles show that the conformational variability of GCN4p16-31 in solution admitted by the available set of 187 measured NMR data is larger than represented by the set of the NMR model structures. The conformations of GCN4p16-31 in solution differ in the orientation not only of the side-chains but also of the backbone. The inconsistencies between the NMR model structures and the measured NMR data are due to the neglect of averaging effects and the inclusion of hydrogen-bond and torsional-angle restraints that have little basis in the primary, i.e. measured NMR data.

  11. Methods of NMR structure refinement: molecular dynamics simulations improve the agreement with measured NMR data of a C-terminal peptide of GCN4-p1.

    Science.gov (United States)

    Dolenc, Jozica; Missimer, John H; Steinmetz, Michel O; van Gunsteren, Wilfred F

    2010-07-01

    The C-terminal trigger sequence is essential in the coiled-coil formation of GCN4-p1; its conformational properties are thus of importance for understanding this process at the atomic level. A solution NMR model structure of a peptide, GCN4p16-31, encompassing the GCN4-p1 trigger sequence was proposed a few years ago. Derived using a standard single-structure refinement protocol based on 172 nuclear Overhauser effect (NOE) distance restraints, 14 hydrogen-bond and 11 phi torsional-angle restraints, the resulting set of 20 NMR model structures exhibits regular alpha-helical structure. However, the set slightly violates some measured NOE bounds and does not reproduce all 15 measured (3)J(H(N)-H(Calpha))-coupling constants, indicating that different conformers of GCN4p16-31 might be present in solution. With the aim to resolve structures compatible with all NOE upper distance bounds and (3)J-coupling constants, we executed several structure refinement protocols employing unrestrained and restrained molecular dynamics (MD) simulations with two force fields. We find that only configurational ensembles obtained by applying simultaneously time-averaged NOE distance and (3)J-coupling constant restraining with either force field reproduce all the experimental data. Additionally, analyses of the simulated ensembles show that the conformational variability of GCN4p16-31 in solution admitted by the available set of 187 measured NMR data is larger than represented by the set of the NMR model structures. The conformations of GCN4p16-31 in solution differ in the orientation not only of the side-chains but also of the backbone. The inconsistencies between the NMR model structures and the measured NMR data are due to the neglect of averaging effects and the inclusion of hydrogen-bond and torsional-angle restraints that have little basis in the primary, i.e. measured NMR data.

  12. Faster pediatric 3-T abdominal magnetic resonance imaging: comparison between conventional and variable refocusing flip-angle single-shot fast spin-echo sequences

    Energy Technology Data Exchange (ETDEWEB)

    Ruangwattanapaisarn, Nichanan [Mahidol University, Department of Diagnostic and Therapeutic Radiology, Ramathibodi Hospital, Bangkok (Thailand); Stanford University, LPCH Department of Radiology, Stanford, CA (United States); Loening, Andreas M.; Saranathan, Manojkumar; Vasanawala, Shreyas S. [Stanford University, LPCH Department of Radiology, Stanford, CA (United States); Litwiller, Daniel V. [GE Healthcare, Rochester, MN (United States)

    2015-06-15

    Single-shot fast spin echo (SSFSE) is particularly appealing in pediatric patients because of its motion robustness. However radiofrequency energy deposition at 3 tesla forces long pauses between slices, leading to longer scans, longer breath-holds and more between-slice motion. We sought to learn whether modulation of the SSFSE refocusing flip-angle train could reduce radiofrequency energy deposition without degrading image quality, thereby reducing inter-slice pauses and overall scan times. We modulated the refocusing flip-angle train for SSFSE to minimize energy deposition while minimizing blurring and motion-related signal loss. In a cohort of 50 consecutive patients (25 boys, mean age 5.5 years, range 1 month to 17 years) referred for abdominal MRI we obtained standard SSFSE and variable refocusing flip-angle (vrfSSFSE) images and recorded sequence scan times. Two readers independently scored the images in blinded, randomized order for noise, tissue contrast, sharpness, artifacts and left lobe hepatic signal uniformity on a four-point scale. The null hypothesis of no difference between SSFSE and vrfSSFSE image-quality was assessed with a Mann-Whitney U test, and the null hypothesis of no scan time difference was assessed with the paired t-test. SSFSE and vrfSSFSE mean acquisition times were 54.3 and 26.2 s, respectively (P-value <0.0001). For each reader, SSFSE and vrfSSFSE noise, tissue contrast, sharpness and artifacts were not significantly different (P-values 0.18-0.86). However, SSFSE had better left lobe hepatic signal uniformity (P < 0.01, both readers). vrfSSFSE is twice as fast as SSFSE, with equivalent image quality with the exception of left hepatic lobe signal heterogeneity. (orig.)

  13. Intracranial cerebrospinal fluid spaces imaging using a pulse-triggered three-dimensional turbo spin echo MR sequence with variable flip-angle distribution

    Energy Technology Data Exchange (ETDEWEB)

    Hodel, Jerome [Unite Analyse et Restauration du Mouvement, UMR-CNRS, 8005 LBM ParisTech Ensam, Paris (France); University Paris Est Creteil (UPEC), Creteil (France); Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Henri Mondor, Department of Neuroradiology, Creteil (France); Hopital Henri Mondor, Creteil (France); Silvera, Jonathan [University Paris Est Creteil (UPEC), Creteil (France); Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Henri Mondor, Department of Neuroradiology, Creteil (France); Bekaert, Olivier; Decq, Philippe [Unite Analyse et Restauration du Mouvement, UMR-CNRS, 8005 LBM ParisTech Ensam, Paris (France); University Paris Est Creteil (UPEC), Creteil (France); Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Henri Mondor, Department of Neurosurgery, Creteil (France); Rahmouni, Alain [University Paris Est Creteil (UPEC), Creteil (France); Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Henri Mondor, Department of Radiology, Creteil (France); Bastuji-Garin, Sylvie [University Paris Est Creteil (UPEC), Creteil (France); Assistance Publique-Hopitaux de Paris, Paris (France); Hopital Henri Mondor, Department of Public Health, Creteil (France); Vignaud, Alexandre [Siemens Healthcare, Saint Denis (France); Petit, Eric; Durning, Bruno [Laboratoire Images Signaux et Systemes Intelligents, UPEC, Creteil (France)

    2011-02-15

    To assess the three-dimensional turbo spin echo with variable flip-angle distribution magnetic resonance sequence (SPACE: Sampling Perfection with Application optimised Contrast using different flip-angle Evolution) for the imaging of intracranial cerebrospinal fluid (CSF) spaces. We prospectively investigated 18 healthy volunteers and 25 patients, 20 with communicating hydrocephalus (CH), five with non-communicating hydrocephalus (NCH), using the SPACE sequence at 1.5T. Volume rendering views of both intracranial and ventricular CSF were obtained for all patients and volunteers. The subarachnoid CSF distribution was qualitatively evaluated on volume rendering views using a four-point scale. The CSF volumes within total, ventricular and subarachnoid spaces were calculated as well as the ratio between ventricular and subarachnoid CSF volumes. Three different patterns of subarachnoid CSF distribution were observed. In healthy volunteers we found narrowed CSF spaces within the occipital aera. A diffuse narrowing of the subarachnoid CSF spaces was observed in patients with NCH whereas patients with CH exhibited narrowed CSF spaces within the high midline convexity. The ratios between ventricular and subarachnoid CSF volumes were significantly different among the volunteers, patients with CH and patients with NCH. The assessment of CSF spaces volume and distribution may help to characterise hydrocephalus. (orig.)

  14. Intracranial cerebrospinal fluid spaces imaging using a pulse-triggered three-dimensional turbo spin echo MR sequence with variable flip-angle distribution

    International Nuclear Information System (INIS)

    Hodel, Jerome; Silvera, Jonathan; Bekaert, Olivier; Decq, Philippe; Rahmouni, Alain; Bastuji-Garin, Sylvie; Vignaud, Alexandre; Petit, Eric; Durning, Bruno

    2011-01-01

    To assess the three-dimensional turbo spin echo with variable flip-angle distribution magnetic resonance sequence (SPACE: Sampling Perfection with Application optimised Contrast using different flip-angle Evolution) for the imaging of intracranial cerebrospinal fluid (CSF) spaces. We prospectively investigated 18 healthy volunteers and 25 patients, 20 with communicating hydrocephalus (CH), five with non-communicating hydrocephalus (NCH), using the SPACE sequence at 1.5T. Volume rendering views of both intracranial and ventricular CSF were obtained for all patients and volunteers. The subarachnoid CSF distribution was qualitatively evaluated on volume rendering views using a four-point scale. The CSF volumes within total, ventricular and subarachnoid spaces were calculated as well as the ratio between ventricular and subarachnoid CSF volumes. Three different patterns of subarachnoid CSF distribution were observed. In healthy volunteers we found narrowed CSF spaces within the occipital aera. A diffuse narrowing of the subarachnoid CSF spaces was observed in patients with NCH whereas patients with CH exhibited narrowed CSF spaces within the high midline convexity. The ratios between ventricular and subarachnoid CSF volumes were significantly different among the volunteers, patients with CH and patients with NCH. The assessment of CSF spaces volume and distribution may help to characterise hydrocephalus. (orig.)

  15. 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)

  16. Correlating the P-31 NMR Chemical Shielding Tensor and the (2)J(P,C) Spin-Spin Coupling Constants with Torsion Angles zeta and alpha in the Backbone of Nucleic Acids

    Czech Academy of Sciences Publication Activity Database

    Benda, Ladislav; Sochorová Vokáčová, Zuzana; Straka, Michal; Sychrovský, Vladimír

    2012-01-01

    Roč. 116, č. 12 (2012), s. 3823-3833 ISSN 1520-6106 R&D Projects: GA ČR GAP205/10/0228; GA ČR GPP208/10/P398; GA ČR GA203/09/2037 Institutional research plan: CEZ:AV0Z40550506 Keywords : nucleic acids * phosphorus NMR * NMR calculations * cross-correlated relaxation * spin–spin coupling constants Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.607, year: 2012

  17. Non-contrast-enhanced 4D MR angiography with STAR spin labeling and variable flip angle sampling: a feasibility study for the assessment of Dural Arteriovenous Fistula

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Jinhee; Kim, Bom-yi; Choi, Hyun Seok; Jung, So-Lyung; Ahn, Kook-Jin; Kim, Bum-soo [The Catholic University of Korea, Department of Radiology, Seoul St. Mary' s Hospital, College of Medicine, Seoul (Korea, Republic of); Schmitt, Peter [Siemens AG, Healthcare Sector, Erlangen (Germany); Kim, Inseong; Paek, Munyoung [Siemens AG, Healthcare, Seoul (Korea, Republic of)

    2014-04-15

    This study aimed to evaluate the feasibility of non-contrast-enhanced 4D magnetic resonance angiography (NCE 4D MRA) with signal targeting with alternative radiofrequency (STAR) spin labeling and variable flip angle (VFA) sampling in the assessment of dural arteriovenous fistula (DAVF) in the transverse sinus. Nine patients underwent NCE 4D MRA for the evaluation of DAVF in the transverse sinus at 3 T. One patient was examined twice, once before and once after the interventional treatment. All patients also underwent digital subtraction angiography (DSA) and/or contrast-enhanced magnetic resonance angiography (CEMRA). For the acquisition of NCE 4D MRA, a STAR spin tagging method was used, and a VFA sampling was applied in the data readout module instead of a constant flip angle. Two readers evaluated the NCE 4D MRA data for the diagnosis of DAVF and its type with consensus. The results were compared with those from DSA and/or CEMRA. All patients underwent NCE 4D MRA without any difficulty. Among seven patients with patent DAVFs, all cases showed an early visualization of the transverse sinus on NCE 4D MRA. Except for one case, the type of DAVF of NCE 4D MRA was agreed with that of reference standard study. Cortical venous reflux (CVR) was demonstrated in two cases out of three patients with CVR. NCE 4D MRA with STAR tagging and VFA sampling is technically and clinically feasible and represents a promising technique for assessment of DAVF in the transverse sinus. Further technical developments should aim at improvements of spatial and temporal coverage. (orig.)

  18. Non-contrast-enhanced 4D MR angiography with STAR spin labeling and variable flip angle sampling: a feasibility study for the assessment of Dural Arteriovenous Fistula

    International Nuclear Information System (INIS)

    Jang, Jinhee; Kim, Bom-yi; Choi, Hyun Seok; Jung, So-Lyung; Ahn, Kook-Jin; Kim, Bum-soo; Schmitt, Peter; Kim, Inseong; Paek, Munyoung

    2014-01-01

    This study aimed to evaluate the feasibility of non-contrast-enhanced 4D magnetic resonance angiography (NCE 4D MRA) with signal targeting with alternative radiofrequency (STAR) spin labeling and variable flip angle (VFA) sampling in the assessment of dural arteriovenous fistula (DAVF) in the transverse sinus. Nine patients underwent NCE 4D MRA for the evaluation of DAVF in the transverse sinus at 3 T. One patient was examined twice, once before and once after the interventional treatment. All patients also underwent digital subtraction angiography (DSA) and/or contrast-enhanced magnetic resonance angiography (CEMRA). For the acquisition of NCE 4D MRA, a STAR spin tagging method was used, and a VFA sampling was applied in the data readout module instead of a constant flip angle. Two readers evaluated the NCE 4D MRA data for the diagnosis of DAVF and its type with consensus. The results were compared with those from DSA and/or CEMRA. All patients underwent NCE 4D MRA without any difficulty. Among seven patients with patent DAVFs, all cases showed an early visualization of the transverse sinus on NCE 4D MRA. Except for one case, the type of DAVF of NCE 4D MRA was agreed with that of reference standard study. Cortical venous reflux (CVR) was demonstrated in two cases out of three patients with CVR. NCE 4D MRA with STAR tagging and VFA sampling is technically and clinically feasible and represents a promising technique for assessment of DAVF in the transverse sinus. Further technical developments should aim at improvements of spatial and temporal coverage. (orig.)

  19. 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

  20. NMR of bicelles: orientation and mosaic spread of the liquid-crystal director under sample rotation

    International Nuclear Information System (INIS)

    Zandomeneghi, Giorgia; Tomaselli, Marco; Williamson, Philip T.F.; Meier, Beat H.

    2003-01-01

    Model-membrane systems composed of liquid-crystalline bicellar phases can be uniaxially oriented with respect to a magnetic field, thereby facilitating structural and dynamics studies of membrane-associated proteins. Here we quantitatively characterize a method that allows the manipulation of the direction of this uniaxial orientation. Bicelles formed from DMPC/DHPC are examined by 31 P NMR under variable-angle sample-spinning (VAS) conditions, confirming that the orientation of the liquid-crystalline director can be influenced by sample spinning. The director is perpendicular to the rotation axis when Θ (the angle between the sample-spinning axis and the magnetic field direction) is smaller than the magic angle, and is parallel to the rotation axis when Θ is larger than the magic angle. The new 31 P NMR VAS data presented are considerably more sensitive to the orientation of the bicelle than earlier 2 H studies and the analysis of the sideband pattern allows the determination of the orientation of the liquid-crystal director and its variation over the sample, i.e., the mosaic spread. Under VAS, the mosaic spread is small if Θ deviates significantly from the magic angle but becomes very large at the magic angle

  1. Corrigendum to "Multiple-quantum spin counting in magic-angle-spinning NMR via low-power symmetry-based dipolar recoupling" [J. Magn. Reson. 236 (2013) 31-40

    Science.gov (United States)

    Teymoori, Gholamhasan; Pahari, Bholanath; Viswanathan, Elumalai; Edén, Mattias

    2017-03-01

    The authors regret that an inappropriate NMR data processing, not known to all authors at the time of publication, was used to produce the multiple-quantum coherence (MQC) spin counting data presented in our article: this lead to artificially enhanced results, particularly concerning those obtained at long MQC excitation intervals (τexc). Here we reproduce Figs. 4-7 with correctly processed data.

  2. Local Structure of Cationic Sites in Dehydrated Zeolites Inferred from 27Al Magic-Angle Spinning NMR and Density Functional Theory Calculations. A Study on Li-, Na-, and K-Chabazite

    Czech Academy of Sciences Publication Activity Database

    Klein, Petr; Pashková, Veronika; Thomas, Haunani M.; Whittleton, Sarah R.; Brus, Jiří; Kobera, Libor; Dědeček, Jiří; Sklenák, Štěpán

    2016-01-01

    Roč. 120, č. 26 (2016), s. 14216-14225 ISSN 1932-7447 R&D Projects: GA ČR GA15-13876S; GA ČR(CZ) GA15-14007S Institutional support: RVO:61388955 ; RVO:61389013 Keywords : zeolites * density functional theory * NMR spectroscopy Subject RIV: CF - Physical ; Theoretical Chemistry; CD - Macromolecular Chemistry (UMCH-V) Impact factor: 4.536, year: 2016

  3. Magic Angle Spinning 207 Pb and low temperature deuterium NMR as a tool for studying local order and dynamics in CH 3 NH 3 PbX 3 (X=Cl, Br, I) hybrid perovskites

    OpenAIRE

    Roiland , Claire; trippé-Allard , gaelle; Jemli , K; Alonso , C; ameline , jean-claude; Gautier , Regis; Le Pollès , Laurent; Deleporte , Emmanuelle; Even , Jacky; Katan , Claudine

    2016-01-01

    National audience; Presenting high solar energy conversion efficiencies (>21%), hybrid perovskites APbX 3 (A is a small organic cation, X=Cl, Br, I) have recently become one of the most promising material in the field of photovoltaic devices. Meanwhile, fundamental understanding of what makes these preovskites so smart for photovoltaics remains limited. More then three decades ago, Wasylishen et al. had already revealed the interest of deuterium NMR to investigate the temperature behaviour an...

  4. 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.

  5. Scoliosis angle

    International Nuclear Information System (INIS)

    Marklund, T.

    1978-01-01

    The most commonly used methods of assessing the scoliotic deviation measure angles that are not clearly defined in relation to the anatomy of the patient. In order to give an anatomic basis for such measurements it is proposed to define the scoliotic deviation as the deviation the vertebral column makes with the sagittal plane. Both the Cobb and the Ferguson angles may be based on this definition. The present methods of measurement are then attempts to measure these angles. If the plane of these angles is parallel to the film, the measurement will be correct. Errors in the measurements may be incurred by the projection. A hypothetical projection, called a 'rectified orthogonal projection', is presented, which correctly represents all scoliotic angles in accordance with these principles. It can be constructed in practice with the aid of a computer and by performing measurements on two projections of the vertebral column; a scoliotic curve can be represented independent of the kyphosis and lordosis. (Auth.)

  6. MRI of intracranial vertebral artery dissection: evaluation of intramural haematoma using a black blood, variable-flip-angle 3D turbo spin-echo sequence

    Energy Technology Data Exchange (ETDEWEB)

    Takano, Koichi; Yamashita, Shinnichi; Kuwabara, Yasuo; Yoshimitsu, Kengo [Fukuoka University, Department of Radiology, Faculty of Medicine, Fukuoka-shi, Fukuoka (Japan); Takemoto, Koichiro; Inoue, Tooru [Fukuoka University, Department of Neurosurgery, Faculty of Medicine, Fukuoka (Japan)

    2013-07-15

    We investigated the efficacy of three-dimensional black blood T1-weighted imaging (3D-BB-T1WI) using a variable refocusing flip angle turbo spin-echo sequence in the diagnosis of intracranial vertebral artery dissection (VAD). Sixteen consecutive patients diagnosed with intracranial VAD underwent magnetic resonance imaging that included 3D time-of-flight-MRA, axial spin-echo T1-weighted images (SE-T1WI) and oblique coronal 3D-BB-T1WI sequences. The visualization, morphology and extent of intramural haematomas were assessed and compared among the sequences. Results obtained by digital subtraction angiography (DSA), 3D-angiography and/or 3D-CT angiography (CTA) were used as standards of reference. 3D-BB-T1WI revealed intramural haematomas in all cases, whereas SE-T1WI and magnetic resonance angiography (MRA) failed to reveal a haematoma in one case and three cases, respectively. The mean visualization grading score for the intramural haematoma was the highest for 3D-BB-T1WI, and there was a statistically significant difference among the sequences (p < 0.001). At least a portion of the intramural haematoma was distinguishable from the lumen on 3D-BB-T1WI, whereas the haematomas were entirely indistinguishable from intraluminal signals on MRA in two cases (12.5 %) and on SE-T1WI in one case (6.3 %). 3D-BB-T1WI revealed the characteristic crescent shape of the intramural haematoma in 14 cases (87.5 %), whereas SE-T1WI and MRA revealed a crescent shape in only 7 cases (43.8 %) and 8 cases (50 %), respectively. In a consensus reading, 3D-BB-T1WI was considered the most consistent sequence in representing the extent and morphology of the lesion in 14 cases (87.5 %), compared to DSA and CTA. 3D-BB-T1WI is a promising method to evaluate intramural haematoma in patients with suspected intracranial VAD. (orig.)

  7. 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.

  8. Angles in hyperbolic lattices

    DEFF Research Database (Denmark)

    Risager, Morten S.; Södergren, Carl Anders

    2017-01-01

    It is well known that the angles in a lattice acting on hyperbolic n -space become equidistributed. In this paper we determine a formula for the pair correlation density for angles in such hyperbolic lattices. Using this formula we determine, among other things, the asymptotic behavior of the den......It is well known that the angles in a lattice acting on hyperbolic n -space become equidistributed. In this paper we determine a formula for the pair correlation density for angles in such hyperbolic lattices. Using this formula we determine, among other things, the asymptotic behavior...... of the density function in both the small and large variable limits. This extends earlier results by Boca, Pasol, Popa and Zaharescu and Kelmer and Kontorovich in dimension 2 to general dimension n . Our proofs use the decay of matrix coefficients together with a number of careful estimates, and lead...

  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. NMR system and method having a permanent magnet providing a rotating magnetic field

    Science.gov (United States)

    Schlueter, Ross D [Berkeley, CA; Budinger, Thomas F [Berkeley, CA

    2009-05-19

    Disclosed herein are systems and methods for generating a rotating magnetic field. The rotating magnetic field can be used to obtain rotating-field NMR spectra, such as magic angle spinning spectra, without having to physically rotate the sample. This result allows magic angle spinning NMR to be conducted on biological samples such as live animals, including humans.

  11. NMR of lignins

    Science.gov (United States)

    John Ralph; Larry L. Landucci

    2010-01-01

    This chapter will consider the basic aspects and findings of several forms of NMR spectroscopy, including separate discussions of proton, carbon, heteronuclear, and multidimensional NMR. Enhanced focus will be on 13C NMR, because of its qualitative and quantitative importance, followed by NMR’s contributions to our understanding of lignin...

  12. 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.

  13. An introduction to biological NMR spectroscopy

    International Nuclear Information System (INIS)

    Marion, Dominique

    2013-01-01

    NMR spectroscopy is a powerful tool for biologists interested in the structure, dynamics, and interactions of biological macromolecules. This review aims at presenting in an accessible manner the requirements and limitations of this technique. As an introduction, the history of NMR will highlight how the method evolved from physics to chemistry and finally to biology over several decades. We then introduce the NMR spectral parameters used in structural biology, namely the chemical shift, the J-coupling, nuclear Overhauser effects, and residual dipolar couplings. Resonance assignment, the required step for any further NMR study, bears a resemblance to jigsaw puzzle strategy. The NMR spectral parameters are then converted into angle and distances and used as input using restrained molecular dynamics to compute a bundle of structures. When interpreting a NMR-derived structure, the biologist has to judge its quality on the basis of the statistics provided. When the 3D structure is a priori known by other means, the molecular interaction with a partner can be mapped by NMR: information on the binding interface as well as on kinetic and thermodynamic constants can be gathered. NMR is suitable to monitor, over a wide range of frequencies, protein fluctuations that play a crucial role in their biological function. In the last section of this review, intrinsically disordered proteins, which have escaped the attention of classical structural biology, are discussed in the perspective of NMR, one of the rare available techniques able to describe structural ensembles. This Tutorial is part of the International Proteomics Tutorial Programme (IPTP 16 MCP). (authors)

  14. A combined variable temperature 600 MHz NMR/MD study of the calcium release agent cyclic adenosine diphosphate ribose (cADPR): Structure, conformational analysis, and thermodynamics of the conformational equilibria.

    Science.gov (United States)

    Javornik, Uroš; Plavec, Janez; Wang, Baifan; Graham, Steven M

    2018-01-02

    A combined variable temperature 600 MHz NMR/molecular dynamics study of the Ca 2+ -release agent cyclic adenosine 5'-diphosphate ribose (cADPR) was conducted. In addition to elucidating the major and minor orientations of the conformationally flexible furanose rings, γ- (C4'-C5'), and β- (C5'-O5') bonds, the thermodynamics (ΔH o , ΔS o ) associated with each of these conformational equilibria were determined. Both furanose rings were biased towards a south conformation (64-74%) and both β-bonds heavily favored trans conformations. The R-ring γ-bond was found to exist almost exclusively as the γ + conformer, whereas the A-ring γ-bond was a mixture of the γ + and γ t conformers, with the trans conformer being slightly favored. Enthalpic factors accounted for most of the observed conformational preferences, although the R-ring furanose exists as its major conformation based solely on entropic factors. There was excellent agreement between the NMR and MD results, particularly with regard to the conformer identities, but the MD showed a bias towards γ + conformers. The MD results showed that both N-glycosidic χ-bonds are exclusively syn. Collectively the data allowed for the construction of a model for cADPR in which many of the conformationally flexible units in fact effectively adopt single orientations and where most of the conformational diversity resides in its A-ring furanose and γ-bond. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Methods of NMR structure refinement: molecular dynamics simulations improve the agreement with measured NMR data of a C-terminal peptide of GCN4-p1

    Energy Technology Data Exchange (ETDEWEB)

    Dolenc, Jozica [Swiss Federal Institute of Technology, Laboratory of Physical Chemistry, ETH (Switzerland); Missimer, John H.; Steinmetz, Michel O. [Paul Scherrer Institut, Biomolecular Research (Switzerland); Gunsteren, Wilfred F. van, E-mail: wfvgn@igc.phys.chem.ethz.c [Swiss Federal Institute of Technology, Laboratory of Physical Chemistry, ETH (Switzerland)

    2010-07-15

    The C-terminal trigger sequence is essential in the coiled-coil formation of GCN4-p1; its conformational properties are thus of importance for understanding this process at the atomic level. A solution NMR model structure of a peptide, GCN4p16-31, encompassing the GCN4-p1 trigger sequence was proposed a few years ago. Derived using a standard single-structure refinement protocol based on 172 nuclear Overhauser effect (NOE) distance restraints, 14 hydrogen-bond and 11 {phi} torsional-angle restraints, the resulting set of 20 NMR model structures exhibits regular {alpha}-helical structure. However, the set slightly violates some measured NOE bounds and does not reproduce all 15 measured {sup 3}J(H{sub N}-H{sub C{alpha}})-coupling constants, indicating that different conformers of GCN4p16-31 might be present in solution. With the aim to resolve structures compatible with all NOE upper distance bounds and {sup 3}J-coupling constants, we executed several structure refinement protocols employing unrestrained and restrained molecular dynamics (MD) simulations with two force fields. We find that only configurational ensembles obtained by applying simultaneously time-averaged NOE distance and {sup 3}J-coupling constant restraining with either force field reproduce all the experimental data. Additionally, analyses of the simulated ensembles show that the conformational variability of GCN4p16-31 in solution admitted by the available set of 187 measured NMR data is larger than represented by the set of the NMR model structures. The conformations of GCN4p16-31 in solution differ in the orientation not only of the side-chains but also of the backbone. The inconsistencies between the NMR model structures and the measured NMR data are due to the neglect of averaging effects and the inclusion of hydrogen-bond and torsional-angle restraints that have little basis in the primary, i.e. measured NMR data.

  16. Detection of surface mobility of poly (2, 3, 4, 5, 6-pentafluorostyrene) films by in situ variable-temperature ToF-SIMS and contact angle measurements.

    Science.gov (United States)

    Fu, Yi; Lau, Yiu-Ting R; Weng, Lu-Tao; Ng, Kai-Mo; Chan, Chi-Ming

    2014-10-01

    Poly (2, 3, 4, 5, 6-pentafluorostyrene) (5FPS) was prepared by bulk radical polymerization. The spin-cast films of this polymer were analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS) at various temperatures ranging from room temperature to 120°C. Principal component analysis (PCA) of the ToF-SIMS data revealed a transition temperature (T(T)) at which the surface structure of 5FPS was rearranged. A comparison between the results of the PCA of ToF-SIMS spectra obtained on 5FPS and polystyrene (PS) indicate that the pendant groups of 5FPS and PS moved in exactly opposite directions as the temperature increased. More pendant groups of 5FPS and PS migrated from the bulk to the surface and verse versa, respectively, as the temperature increased. These results clearly support the view that the abrupt changes in the normalized principal component 1 value was caused by the surface reorientation of the polymers and not by a change in the ion fragmentation mechanism at temperatures above the T(T). Contact angle measurement, which is another extremely surface sensitive technique, was used to monitor the change in the surface tension as a function of temperature. A clear T(T) was determined by the contact angle measurements. The T(T) values determined by contact angle measurements and ToF-SIMS were very similar. Copyright © 2014 Elsevier Inc. All rights reserved.

  17. Variable Step Closed Loop Power Control with Space Diversity for Low Elevation Angle High Altitude Platforms Communication Channel [Langkah Variabel Kontrol Daya Loop Tertutup dengan Keragaman Ruang untuk Sudut Elevasi Rendah pada Kanal Komunikasi HAPs

    Directory of Open Access Journals (Sweden)

    Iskandar Iskandar

    2016-07-01

    Full Text Available This paper proposes variable step closed loop power control algorithm combined with space diversity to improve the performance of High Altitude Platforms (HAPs communication at low elevation angle using Code Division Multiple Access (CDMA. In this contribution, we first develop HAPs channel model which is derived from experimental measurement. From our experiment, we found HAPs channel characteristic can be modeled as a Ricean distribution because the presence of line of sight path. Different elevation angle resulting different K factor value.  This value is then used in Signal to Interference Ratio (SIR based closed loop power control evaluation. The variable step algorithm is simulated under various elevation angles with different speed of mobile user. The performance is presented in terms of user elevation angle, user speed, step size and space diversity order. We found that the performance of variable step closed-loop power control less effective at low elevation angle. However our simulation shows that space diversity is able to improve the performance of closed loop power control for HAPs channel at low elevation angle.*****Kajian ini mengusulkan suatu algoritma kontrol daya langkah variabel loop tertutup dikombinasikan dengan keragaman ruang untuk meningkatkan kinerja komunikasi High Altitude Platforms(HAPs pada sudut elevasi rendah menggunakan Code Division Multiple Access (CDMA. Kami berkontribusi untuk mengembangkan model kanal HAPs yang berasal dari pengukuran eksperimental sebelumnya. Dari percobaan tersebut, kami menemukan karakteristik kanal HAPs yang dapat dimodelkan sebagai distribusi Ricean karena kehadiran jalur tanpa penghalang. Eksperimen menunjukkan bahwa perbedaan sudut elevasi menghasilkan perbedaan nilai factor K. Nilai ini kemudian digunakan dalam Signal to Interference Ratio (SIR berbasiskan evaluasi kontrol daya loop tertutup. Algoritma langkah variabel disimulasikan dibawah sudut elevasi yang berbeda dengan kecepatan

  18. Communication: Wigner functions in action-angle variables, Bohr-Sommerfeld quantization, the Heisenberg correspondence principle, and a symmetrical quasi-classical approach to the full electronic density matrix

    International Nuclear Information System (INIS)

    Miller, William H.; Cotton, Stephen J.

    2016-01-01

    It is pointed out that the classical phase space distribution in action-angle (a-a) variables obtained from a Wigner function depends on how the calculation is carried out: if one computes the standard Wigner function in Cartesian variables (p, x), and then replaces p and x by their expressions in terms of a-a variables, one obtains a different result than if the Wigner function is computed directly in terms of the a-a variables. Furthermore, the latter procedure gives a result more consistent with classical and semiclassical theory—e.g., by incorporating the Bohr-Sommerfeld quantization condition (quantum states defined by integer values of the action variable) as well as the Heisenberg correspondence principle for matrix elements of an operator between such states—and has also been shown to be more accurate when applied to electronically non-adiabatic applications as implemented within the recently developed symmetrical quasi-classical (SQC) Meyer-Miller (MM) approach. Moreover, use of the Wigner function (obtained directly) in a-a variables shows how our standard SQC/MM approach can be used to obtain off-diagonal elements of the electronic density matrix by processing in a different way the same set of trajectories already used (in the SQC/MM methodology) to obtain the diagonal elements.

  19. Communication: Wigner functions in action-angle variables, Bohr-Sommerfeld quantization, the Heisenberg correspondence principle, and a symmetrical quasi-classical approach to the full electronic density matrix.

    Science.gov (United States)

    Miller, William H; Cotton, Stephen J

    2016-08-28

    It is pointed out that the classical phase space distribution in action-angle (a-a) variables obtained from a Wigner function depends on how the calculation is carried out: if one computes the standard Wigner function in Cartesian variables (p, x), and then replaces p and x by their expressions in terms of a-a variables, one obtains a different result than if the Wigner function is computed directly in terms of the a-a variables. Furthermore, the latter procedure gives a result more consistent with classical and semiclassical theory-e.g., by incorporating the Bohr-Sommerfeld quantization condition (quantum states defined by integer values of the action variable) as well as the Heisenberg correspondence principle for matrix elements of an operator between such states-and has also been shown to be more accurate when applied to electronically non-adiabatic applications as implemented within the recently developed symmetrical quasi-classical (SQC) Meyer-Miller (MM) approach. Moreover, use of the Wigner function (obtained directly) in a-a variables shows how our standard SQC/MM approach can be used to obtain off-diagonal elements of the electronic density matrix by processing in a different way the same set of trajectories already used (in the SQC/MM methodology) to obtain the diagonal elements.

  20. Communication: Wigner functions in action-angle variables, Bohr-Sommerfeld quantization, the Heisenberg correspondence principle, and a symmetrical quasi-classical approach to the full electronic density matrix

    Energy Technology Data Exchange (ETDEWEB)

    Miller, William H., E-mail: millerwh@berkeley.edu; Cotton, Stephen J., E-mail: StephenJCotton47@gmail.com [Department of Chemistry and Kenneth S. Pitzer Center for Theoretical Chemistry, University of California, and Chemical Sciences Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States)

    2016-08-28

    It is pointed out that the classical phase space distribution in action-angle (a-a) variables obtained from a Wigner function depends on how the calculation is carried out: if one computes the standard Wigner function in Cartesian variables (p, x), and then replaces p and x by their expressions in terms of a-a variables, one obtains a different result than if the Wigner function is computed directly in terms of the a-a variables. Furthermore, the latter procedure gives a result more consistent with classical and semiclassical theory—e.g., by incorporating the Bohr-Sommerfeld quantization condition (quantum states defined by integer values of the action variable) as well as the Heisenberg correspondence principle for matrix elements of an operator between such states—and has also been shown to be more accurate when applied to electronically non-adiabatic applications as implemented within the recently developed symmetrical quasi-classical (SQC) Meyer-Miller (MM) approach. Moreover, use of the Wigner function (obtained directly) in a-a variables shows how our standard SQC/MM approach can be used to obtain off-diagonal elements of the electronic density matrix by processing in a different way the same set of trajectories already used (in the SQC/MM methodology) to obtain the diagonal elements.

  1. 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)

  2. Bayesian Peak Picking for NMR Spectra

    KAUST Repository

    Cheng, Yichen

    2014-02-01

    Protein structure determination is a very important topic in structural genomics, which helps people to understand varieties of biological functions such as protein-protein interactions, protein–DNA interactions and so on. Nowadays, nuclear magnetic resonance (NMR) has often been used to determine the three-dimensional structures of protein in vivo. This study aims to automate the peak picking step, the most important and tricky step in NMR structure determination. We propose to model the NMR spectrum by a mixture of bivariate Gaussian densities and use the stochastic approximation Monte Carlo algorithm as the computational tool to solve the problem. Under the Bayesian framework, the peak picking problem is casted as a variable selection problem. The proposed method can automatically distinguish true peaks from false ones without preprocessing the data. To the best of our knowledge, this is the first effort in the literature that tackles the peak picking problem for NMR spectrum data using Bayesian method.

  3. 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

  4. 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

  5. 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

  6. Digital breast tomosynthesis: observer performance of clustered microcalcification detection on breast phantom images acquired with an experimental system using variable scan angles, angular increments, and number of projection views.

    Science.gov (United States)

    Chan, Heang-Ping; Goodsitt, Mitchell M; Helvie, Mark A; Zelakiewicz, Scott; Schmitz, Andrea; Noroozian, Mitra; Paramagul, Chintana; Roubidoux, Marilyn A; Nees, Alexis V; Neal, Colleen H; Carson, Paul; Lu, Yao; Hadjiiski, Lubomir; Wei, Jun

    2014-12-01

    To investigate the dependence of microcalcification cluster detectability on tomographic scan angle, angular increment, and number of projection views acquired at digital breast tomosynthesis ( DBT digital breast tomosynthesis ). A prototype DBT digital breast tomosynthesis system operated in step-and-shoot mode was used to image breast phantoms. Four 5-cm-thick phantoms embedded with 81 simulated microcalcification clusters of three speck sizes (subtle, medium, and obvious) were imaged by using a rhodium target and rhodium filter with 29 kV, 50 mAs, and seven acquisition protocols. Fixed angular increments were used in four protocols (denoted as scan angle, angular increment, and number of projection views, respectively: 16°, 1°, and 17; 24°, 3°, and nine; 30°, 3°, and 11; and 60°, 3°, and 21), and variable increments were used in three (40°, variable, and 13; 40°, variable, and 15; and 60°, variable, and 21). The reconstructed DBT digital breast tomosynthesis images were interpreted by six radiologists who located the microcalcification clusters and rated their conspicuity. The mean sensitivity for detection of subtle clusters ranged from 80% (22.5 of 28) to 96% (26.8 of 28) for the seven DBT digital breast tomosynthesis protocols; the highest sensitivity was achieved with the 16°, 1°, and 17 protocol (96%), but the difference was significant only for the 60°, 3°, and 21 protocol (80%, P .99). The conspicuity of subtle and medium clusters with the 16°, 1°, and 17 protocol was rated higher than those with other protocols; the differences were significant for subtle clusters with the 24°, 3°, and nine protocol and for medium clusters with 24°, 3°, and nine; 30°, 3°, and 11; 60°, 3° and 21; and 60°, variable, and 21 protocols (P tomosynthesis provided higher sensitivity and conspicuity than wide-angle DBT digital breast tomosynthesis for subtle microcalcification clusters. © RSNA, 2014.

  7. Quantifying the ocean, freshwater and human effects on year-to-year variability of one-sea-winter Atlantic salmon angled in multiple Norwegian rivers.

    Science.gov (United States)

    Otero, Jaime; Jensen, Arne J; L'Abée-Lund, Jan Henning; Stenseth, Nils Chr; Storvik, Geir O; Vøllestad, Leif Asbjørn

    2011-01-01

    Many Atlantic salmon, Salmo salar, populations are decreasing throughout the species' distributional range probably due to several factors acting in concert. A number of studies have documented the influence of freshwater and ocean conditions, climate variability and human impacts resulting from impoundment and aquaculture. However, most previous research has focused on analyzing single or only a few populations, and quantified isolated effects rather than handling multiple factors in conjunction. By using a multi-river mixed-effects model we estimated the effects of oceanic and river conditions, as well as human impacts, on year-to-year and between-river variability across 60 time series of recreational catch of one-sea-winter salmon (grilse) from Norwegian rivers over 29 years (1979-2007). Warm coastal temperatures at the time of smolt entrance into the sea and increased water discharge during upstream migration of mature fish were associated with higher rod catches of grilse. When hydropower stations were present in the course of the river systems the strength of the relationship with runoff was reduced. Catches of grilse in the river increased significantly following the reduction of the harvesting of this life-stage at sea. However, an average decreasing temporal trend was still detected and appeared to be stronger in the presence of salmon farms on the migration route of smolts in coastal/fjord areas. These results suggest that both ocean and freshwater conditions in conjunction with various human impacts contribute to shape interannual fluctuations and between-river variability of wild Atlantic salmon in Norwegian rivers. Current global change altering coastal temperature and water flow patterns might have implications for future grilse catches, moreover, positioning of aquaculture facilities as well as the implementation of hydropower schemes or other encroachments should be made with care when implementing management actions and searching for solutions to

  8. Quantifying the ocean, freshwater and human effects on year-to-year variability of one-sea-winter Atlantic salmon angled in multiple Norwegian rivers.

    Directory of Open Access Journals (Sweden)

    Jaime Otero

    Full Text Available Many Atlantic salmon, Salmo salar, populations are decreasing throughout the species' distributional range probably due to several factors acting in concert. A number of studies have documented the influence of freshwater and ocean conditions, climate variability and human impacts resulting from impoundment and aquaculture. However, most previous research has focused on analyzing single or only a few populations, and quantified isolated effects rather than handling multiple factors in conjunction. By using a multi-river mixed-effects model we estimated the effects of oceanic and river conditions, as well as human impacts, on year-to-year and between-river variability across 60 time series of recreational catch of one-sea-winter salmon (grilse from Norwegian rivers over 29 years (1979-2007. Warm coastal temperatures at the time of smolt entrance into the sea and increased water discharge during upstream migration of mature fish were associated with higher rod catches of grilse. When hydropower stations were present in the course of the river systems the strength of the relationship with runoff was reduced. Catches of grilse in the river increased significantly following the reduction of the harvesting of this life-stage at sea. However, an average decreasing temporal trend was still detected and appeared to be stronger in the presence of salmon farms on the migration route of smolts in coastal/fjord areas. These results suggest that both ocean and freshwater conditions in conjunction with various human impacts contribute to shape interannual fluctuations and between-river variability of wild Atlantic salmon in Norwegian rivers. Current global change altering coastal temperature and water flow patterns might have implications for future grilse catches, moreover, positioning of aquaculture facilities as well as the implementation of hydropower schemes or other encroachments should be made with care when implementing management actions and searching

  9. 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.

  10. {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)

  11. 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)

  12. 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

  13. 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

  14. 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.

  15. 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

  16. Two-dimensional NMR investigations of the dynamic conformations of phospholipids and liquid crystals

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Mei [Univ. of California, Berkeley, CA (United States). Applied Science and Technology

    1996-05-01

    Two-dimensional 13C, 1H, and 31P nuclear magnetic resonance (NMR) techniques are developed and used to study molecular structure and dynamics in liquid-crystalline systems, primarily phospholipids and nematic liquid crystals. NMR spectroscopy characterizes molecular conformation in terms of orientations and distances of molecular segments. In anisotropically mobile systems, this is achieved by measuring motionally-averaged nuclear dipolar couplings and chemical shift anisotropies. The short-range couplings yield useful bond order parameters, while the long-range interactions constrain the overall conformation. In this work, techniques for probing proton dipolar local fields are further developed to obtain highlyresolved dipolar couplings between protons and rare spins. By exploiting variable-angle sample spinning techniques, orientation-sensitive NMR spectra are resolved according to sitespecific isotropic chemical shifts. Moreover, the signs and magnitudes of various short-range dipolar couplings are obtained. They are used in novel theoretical analyses that provide information about segmental orientations and their distributions. Such information is obtained in a model-independent fashion or with physically reasonable assumptions. The structural investigation of phospholipids is focused on the dynam

  17. Rapid parametric mapping of the longitudinal relaxation time T1 using two-dimensional variable flip angle magnetic resonance imaging at 1.5 Tesla, 3 Tesla, and 7 Tesla.

    Science.gov (United States)

    Dieringer, Matthias A; Deimling, Michael; Santoro, Davide; Wuerfel, Jens; Madai, Vince I; Sobesky, Jan; von Knobelsdorff-Brenkenhoff, Florian; Schulz-Menger, Jeanette; Niendorf, Thoralf

    2014-01-01

    Visual but subjective reading of longitudinal relaxation time (T1) weighted magnetic resonance images is commonly used for the detection of brain pathologies. For this non-quantitative measure, diagnostic quality depends on hardware configuration, imaging parameters, radio frequency transmission field (B1+) uniformity, as well as observer experience. Parametric quantification of the tissue T1 relaxation parameter offsets the propensity for these effects, but is typically time consuming. For this reason, this study examines the feasibility of rapid 2D T1 quantification using a variable flip angles (VFA) approach at magnetic field strengths of 1.5 Tesla, 3 Tesla, and 7 Tesla. These efforts include validation in phantom experiments and application for brain T1 mapping. T1 quantification included simulations of the Bloch equations to correct for slice profile imperfections, and a correction for B1+. Fast gradient echo acquisitions were conducted using three adjusted flip angles for the proposed T1 quantification approach that was benchmarked against slice profile uncorrected 2D VFA and an inversion-recovery spin-echo based reference method. Brain T1 mapping was performed in six healthy subjects, one multiple sclerosis patient, and one stroke patient. Phantom experiments showed a mean T1 estimation error of (-63±1.5)% for slice profile uncorrected 2D VFA and (0.2±1.4)% for the proposed approach compared to the reference method. Scan time for single slice T1 mapping including B1+ mapping could be reduced to 5 seconds using an in-plane resolution of (2×2) mm2, which equals a scan time reduction of more than 99% compared to the reference method. Our results demonstrate that rapid 2D T1 quantification using a variable flip angle approach is feasible at 1.5T/3T/7T. It represents a valuable alternative for rapid T1 mapping due to the gain in speed versus conventional approaches. This progress may serve to enhance the capabilities of parametric MR based lesion detection and

  18. Instrumentation for cryogenic magic angle spinning dynamic nuclear polarization using 90L of liquid nitrogen per day.

    Science.gov (United States)

    Albert, Brice J; Pahng, Seong Ho; Alaniva, Nicholas; Sesti, Erika L; Rand, Peter W; Saliba, Edward P; Scott, Faith J; Choi, Eric J; Barnes, Alexander B

    2017-10-01

    Cryogenic sample temperatures can enhance NMR sensitivity by extending spin relaxation times to improve dynamic nuclear polarization (DNP) and by increasing Boltzmann spin polarization. We have developed an efficient heat exchanger with a liquid nitrogen consumption rate of only 90L per day to perform magic-angle spinning (MAS) DNP experiments below 85K. In this heat exchanger implementation, cold exhaust gas from the NMR probe is returned to the outer portion of a counterflow coil within an intermediate cooling stage to improve cooling efficiency of the spinning and variable temperature gases. The heat exchange within the counterflow coil is calculated with computational fluid dynamics to optimize the heat transfer. Experimental results using the novel counterflow heat exchanger demonstrate MAS DNP signal enhancements of 328±3 at 81±2K, and 276±4 at 105±2K. Copyright © 2017 Elsevier Inc. All rights reserved.

  19. DNA oligonucleotide conformations: high resolution NMR studies

    International Nuclear Information System (INIS)

    Mellema, J.-R.

    1984-01-01

    The present work describes a DNA double-helix model, which is well comparable with the models derived from fibre-diffraction studies. The model has a mononucleotide repeat with torsion angles in accordance with average geometries as derived from 1 H NMR studies. Special attention was paid to reduce the number of short H-H nonbonding contacts, which are abundantly present in the 'classical' fibre-diffraction models. Chapter 3 describes the first complete assignment of a 1 H NMR spectrum of a DNA tetramer, d(TAAT). Preliminary conformational data derived from the spectral parameters recorded at 27 0 C are given. A more detailed analysis employing temperature-dependence studies is given in Chapter 4. (Auth.)

  20. 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.)

  1. Probing molecular dynamics of metal borohydrides on the surface of mesoporous scaffolds by multinuclear high resolution solid state NMR

    Energy Technology Data Exchange (ETDEWEB)

    Hwang, Son-Jong, E-mail: Sonjong@cheme.caltech.edu [Division of Chemistry and Chemical Eng., California Institute of Technology, Pasadena, CA 91125 (United States); Lee, Hyun-Sook [High Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); To, Magnus [Division of Chemistry and Chemical Eng., California Institute of Technology, Pasadena, CA 91125 (United States); Lee, Young-Su; Cho, Young Whan [High Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seoul 136-791 (Korea, Republic of); Choi, Hyungkeun; Kim, Chul [Department of Chemistry, Hannam University, Daejeon 305-811 (Korea, Republic of)

    2015-10-05

    Graphical abstract: In situ variable temperature multinuclear solid state NMR allows to probe surface wetting, diffusivity, and confinement of metal borohydrides into nanopores. - Abstract: Understanding of surface interactions between borohydride molecules and the surfaces of porous supports have gained growing attention for successful development of nano-confinement engineering. By use of in situ variable temperature (VT) magic angle spinning (MAS) NMR, molecular mobility changes of LiBH{sub 4} crystalline solid has been investigated in the presence of silica based and carbonaceous surfaces. Spin–spin J-coupling of {sup 1}H–{sup 11}B in LiBH{sub 4} was monitored in series of VT NMR spectra to probe translational mobility of LiBH{sub 4} that appeared to be greatly enhanced upon surface contact. Such enhanced diffusivity was found to be effective in the formation of solid solution and co-confinement with other metal borohydrides. Co-confinement of LiBH{sub 4}–Ca(BH{sub 4}){sub 2} mixture was demonstrated at temperature as low as 100 °C, much lower than the reported bulk eutectic melting temperature. The discovery adds a novel property of LiBH{sub 4} that has been proven to be highly versatile in many energy related applications.

  2. 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

  3. NMR analog of Bell's inequalities violation test

    International Nuclear Information System (INIS)

    Souza, A M; Oliveira, I S; Sarthour, R S; Magalhaes, A; Teles, J; Azevedo, E R de; Bonagamba, T J

    2008-01-01

    In this paper, we present an analog of Bell's inequalities violation test for N qubits to be performed in a nuclear magnetic resonance (NMR) quantum computer. This can be used to simulate or predict the results for different Bell's inequality tests, with distinct configurations and a larger number of qubits. To demonstrate our scheme, we implemented a simulation of the violation of the Clauser, Horne, Shimony and Holt (CHSH) inequality using a two-qubit NMR system and compared the results to those of a photon experiment. The experimental results are well described by the quantum mechanics theory and a local realistic hidden variables model (LRHVM) that was specifically developed for NMR. That is why we refer to this experiment as a simulation of Bell's inequality violation. Our result shows explicitly how the two theories can be compatible with each other due to the detection loophole. In the last part of this work, we discuss the possibility of testing some fundamental features of quantum mechanics using NMR with highly polarized spins, where a strong discrepancy between quantum mechanics and hidden variables models can be expected

  4. Dynamics of solutions and fluid mixtures by NMR

    International Nuclear Information System (INIS)

    Delpuech, J.J.

    1994-01-01

    After a short introduction to NMR spectroscopy, with a special emphasis on dynamical aspects, an overview on two fundamental aspects of molecular dynamics, NMR relaxation and its relationship with molecular reorientation, and magnetization transfer phenomena induced by molecular rate processes (dynamic NMR) is presented, followed by specific mechanisms of relaxation encountered in paramagnetic systems or with quadrupolar nuclei. Application fields are then reviewed: solvent exchange on metal ions with a variable pressure NMR approach, applications of field gradients in NMR, aggregation phenomena and micro-heterogeneity in surfactant solutions, polymers and biopolymers in the liquid state, liquid-like molecules in rigid matrices and in soft matter (swollen polymers and gels, fluids in and on inorganic materials, food)

  5. Sealed magic angle spinning nuclear magnetic resonance probe and process for spectroscopy of hazardous samples

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Herman M.; Washton, Nancy M.; Mueller, Karl T.; Sears, Jr., Jesse A.; Townsend, Mark R.; Ewing, James R.

    2016-06-14

    A magic-angle-spinning (MAS) nuclear magnetic resonance (NMR) probe is described that includes double containment enclosures configured to seal and contain hazardous samples for analysis. The probe is of a modular design that ensures containment of hazardous samples during sample analysis while preserving spin speeds for superior NMR performance and convenience of operation.

  6. 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.)

  7. Filling Open Screw Holes in the Area of Metaphyseal Comminution Does Not Affect Fatigue Life of the Synthes Variable Angle Distal Femoral Locking Plate in the AO/OTA 33-A3 Fracture Model.

    Science.gov (United States)

    Grau, Luis; Collon, Kevin; Alhandi, Ali; Kaimrajh, David; Varon, Maria; Latta, Loren; Vilella, Fernando

    2018-06-01

    The aim of this study is to evaluate the biomechanical effect of filling locking variable angle (VA) screw holes at the area of metaphyseal fracture comminution in a Sawbones® (Sawbones USA, Vashon, Washington) model (AO/OTA 33A-3 fracture) using a Synthes VA locking compression plate (LCP) (Depuy Synthes, Warsaw, Indiana). Seven Sawbones® femur models had a Synthes VA-LCP placed as indicated by the manufacturers technique. A 4cm osteotomy was then created to simulate an AO/OTA 33-A3 femoral fracture pattern with metaphyseal comminution. The control group consisted of four constructs in which the open screw holes at the area of comminution were left unfilled; the experimental group consisted of three constructs in which the VA screw holes were filled with locking screws. One of the control constructs was statically loaded to failure at a rate of 5mm/min. A value equal to 75% of the ultimate load to failure was used as the loading force for fatigue testing of 250,000 cycles at 3Hz. Cycles to failure was recorded for each construct and averages were compared between groups. The average number of cycles to failure in the control and experimental groups were 37524±8187 and 43304±23835, respectively (p=0.72). No significant difference was observed with respect to cycles to failure or mechanism of failure between groups. In all constructs in both the control and experimental groups, plate failure reproducibly occurred with cracks through the variable angle holes in the area of bridged comminution. The Synthes VA-LCP in a simulated AO/OTA 33-A3 comminuted metaphyseal femoral fracture fails in a reproducible manner at the area of comminution through the "honeycomb" VA screw holes. Filling open VA screw holes at the site of comminution with locking screws does not increase fatigue life of the Synthes VA-LCP in a simulated AO/OTA 33-A3 distal femoral fracture. Further studies are necessary to determine whether use of this particular plate is contraindicated when bridging

  8. Glaucoma, Open-Angle

    Science.gov (United States)

    ... Home » Statistics and Data » Glaucoma, Open-angle Listen Glaucoma, Open-angle Open-angle Glaucoma Defined In open-angle glaucoma, the fluid passes ... 2010 2010 U.S. Age-Specific Prevalence Rates for Glaucoma by Age and Race/Ethnicity The prevalence of ...

  9. Auto-calibrated scanning-angle prism-type total internal reflection microscopy for nanometer-precision axial position determination and optional variable-illumination-depth pseudo total internal reflection microscopy

    Science.gov (United States)

    Fang, Ning; Sun, Wei

    2015-04-21

    A method, apparatus, and system for improved VA-TIRFM microscopy. The method comprises automatically controlled calibration of one or more laser sources by precise control of presentation of each laser relative a sample for small incremental changes of incident angle over a range of critical TIR angles. The calibration then allows precise scanning of the sample for any of those calibrated angles for higher and more accurate resolution, and better reconstruction of the scans for super resolution reconstruction of the sample. Optionally the system can be controlled for incident angles of the excitation laser at sub-critical angles for pseudo TIRFM. Optionally both above-critical angle and sub critical angle measurements can be accomplished with the same system.

  10. 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.

  11. 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.

  12. 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.

  13. Rhodopsin-lipid interactions studied by NMR.

    Science.gov (United States)

    Soubias, Olivier; Gawrisch, Klaus

    2013-01-01

    The biophysical properties of the lipid matrix are known to influence function of integral membrane proteins. We report on a sample preparation method for reconstitution of membrane proteins which uses porous anodic aluminum oxide (AAO) filters with 200-nm-wide pores of high density. The substrate permits formation of tubular, single membranes that line the inner surface of pores. One square centimeter of filter with a thickness of 60μm yields on the order of 500cm(2) of solid-supported single bilayer surface, sufficient for NMR studies. The tubular bilayers are free of detergent, fully hydrated, and accessible for ligands from one side of the membrane. The use of AAO filters greatly improves reproducibility of the reconstitution process such that the influence of protein on lipid order parameters can be studied with high resolution. As an example, results for the G protein-coupled receptor of class A, bovine rhodopsin, are shown. By (2)H NMR order parameter measurements, it is detected that rhodopsin insertion elastically deforms membranes near the protein. Furthermore, by (1)H saturation-transfer NMR under conditions of magic angle spinning, we demonstrate detection of preferences in interactions of rhodopsin with particular lipid species. It is assumed that function of integral membrane proteins depends on both protein-induced elastic deformations of the lipid matrix and preferences for interaction of the protein with particular lipid species in the first layer of lipids surrounding the protein. Copyright © 2013 Elsevier Inc. All rights reserved.

  14. Principles of high resolution NMR in solids

    CERN Document Server

    Mehring, Michael

    1983-01-01

    The field of Nuclear Magnetic Resonance (NMR) has developed at a fascinating pace during the last decade. It always has been an extremely valuable tool to the organic chemist by supplying molecular "finger print" spectra at the atomic level. Unfortunately the high resolution achievable in liquid solutions could not be obtained in solids and physicists and physical chemists had to live with unresolved lines open to a wealth of curve fitting procedures and a vast amount of speculations. High resolution NMR in solids seemed to be a paradoxon. Broad structure­ less lines are usually encountered when dealing with NMR in solids. Only with the recent advent of mUltiple pulse, magic angle, cross-polarization, two-dimen­ sional and multiple-quantum spectroscopy and other techniques during the last decade it became possible to resolve finer details of nuclear spin interactions in solids. I have felt that graduate students, researchers and others beginning to get involved with these techniques needed a book which trea...

  15. 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.)

  16. Small angle spectrometers: Summary

    International Nuclear Information System (INIS)

    Courant, E.; Foley, K.J.; Schlein, P.E.

    1986-01-01

    Aspects of experiments at small angles at the Superconducting Super Collider are considered. Topics summarized include a small angle spectrometer, a high contingency spectrometer, dipole and toroid spectrometers, and magnet choices

  17. Contact Angle Goniometer

    Data.gov (United States)

    Federal Laboratory Consortium — Description:The FTA32 goniometer provides video-based contact angle and surface tension measurement. Contact angles are measured by fitting a mathematical expression...

  18. Conformational variability of the stationary phase survival protein E from Xylella fastidiosa revealed by X-ray crystallography, small-angle X-ray scattering studies, and normal mode analysis.

    Science.gov (United States)

    Machado, Agnes Thiane Pereira; Fonseca, Emanuella Maria Barreto; Reis, Marcelo Augusto Dos; Saraiva, Antonio Marcos; Santos, Clelton Aparecido Dos; de Toledo, Marcelo Augusto Szymanski; Polikarpov, Igor; de Souza, Anete Pereira; Aparicio, Ricardo; Iulek, Jorge

    2017-10-01

    Xylella fastidiosa is a xylem-limited bacterium that infects a wide variety of plants. Stationary phase survival protein E is classified as a nucleotidase, which is expressed when bacterial cells are in the stationary growth phase and subjected to environmental stresses. Here, we report four refined X-ray structures of this protein from X. fastidiosa in four different crystal forms in the presence and/or absence of the substrate 3'-AMP. In all chains, the conserved loop verified in family members assumes a closed conformation in either condition. Therefore, the enzymatic mechanism for the target protein might be different of its homologs. Two crystal forms exhibit two monomers whereas the other two show four monomers in the asymmetric unit. While the biological unit has been characterized as a tetramer, differences of their sizes and symmetry are remarkable. Four conformers identified by Small-Angle X-ray Scattering (SAXS) in a ligand-free solution are related to the low frequency normal modes of the crystallographic structures associated with rigid body-like protomer arrangements responsible for the longitudinal and symmetric adjustments between tetramers. When the substrate is present in solution, only two conformers are selected. The most prominent conformer for each case is associated to a normal mode able to elongate the protein by moving apart two dimers. To our knowledge, this work was the first investigation based on the normal modes that analyzed the quaternary structure variability for an enzyme of the SurE family followed by crystallography and SAXS validation. The combined results raise new directions to study allosteric features of XfSurE protein. © 2017 Wiley Periodicals, Inc.

  19. 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)

  20. A fragment separator at LBL for beta-NMR experiment

    International Nuclear Information System (INIS)

    Matsuta, K.; Ozawa, A.; Nojiri, Y.; Minamisono, T.; Fukuda, M.; Kitagawa, A.; Ohtsubo, T.; Momota, S.; Fukuda, S.; Matsuo, Y.; Takechi, H.; Minami, I.; Sugimoto, K.; Tanihata, I.; Omata, K.; Alonso, J.R.; Krebs, G.F.; Symons, T.J.M.

    1992-03-01

    The Beam 44 fragment separator was built at the Bevalac of LBL for NMR studies of beta emitting nuclei. 37 K, 39 Ca, and 43 Ti fragments originating from 40 Ca and 46 Ti primary beams were separated by the separator for NMR studies on these nuclei. Nuclear spin polarization was created in 39 Ca and 43 Ti using the tilted foil technique (TFT), and the magnetic moment of 43 Ti was deduced. Fragment polarization was measured for 37 K and 39 Ca emitted to finite deflection angles. The Beam 44 fragment separator in combination with a proper polarization technique, such as TFT or fragment polarization, has been very effective for such NMR studies

  1. 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

  2. PGI chicory (Cichorium intybus L.) traceability by means of HRMAS-NMR spectroscopy: a preliminary study.

    Science.gov (United States)

    Ritota, Mena; Casciani, Lorena; Valentini, Massimiliano

    2013-05-01

    Analytical traceability of PGI and PDO foods (Protected Geographical Indication and Protected Denomination Origin respectively) is one of the most challenging tasks of current applied research. Here we proposed a metabolomic approach based on the combination of (1)H high-resolution magic angle spinning-nuclear magnetic resonance (HRMAS-NMR) spectroscopy with multivariate analysis, i.e. PLS-DA, as a reliable tool for the traceability of Italian PGI chicories (Cichorium intybus L.), i.e. Radicchio Rosso di Treviso and Radicchio Variegato di Castelfranco, also known as red and red-spotted, respectively. The metabolic profile was gained by means of HRMAS-NMR, and multivariate data analysis allowed us to build statistical models capable of providing clear discrimination among the two varieties and classification according to the geographical origin. Based on Variable Importance in Projection values, the molecular markers for classifying the different types of red chicories analysed were found accounting for both the cultivar and the place of origin. © 2012 Society of Chemical Industry.

  3. Chirp echo Fourier transform EPR-detected NMR.

    Science.gov (United States)

    Wili, Nino; Jeschke, Gunnar

    2018-04-01

    A new ultra-wide band (UWB) pulse EPR method is introduced for observing all nuclear frequencies of a paramagnetic center in a single shot. It is based on burning spectral holes with a high turning angle (HTA) pulse that excites forbidden transitions and subsequent detection of the hole pattern by a chirp echo. We term this method Chirp Echo Epr SpectroscopY (CHEESY)-detected NMR. The approach is a revival of FT EPR-detected NMR. It yields similar spectra and the same type of information as electron-electron double resonance (ELDOR)-detected NMR, but with a multiplex advantage. We apply CHEESY-detected NMR in Q band to nitroxides and correlate the hyperfine spectrum to the EPR spectrum by varying the frequency of the HTA pulse. Furthermore, a selective π pulse before the HTA pulse allows for detecting hyperfine sublevel correlations between transitions of one nucleus and for elucidating the coupling regime, the same information as revealed by the HYSCORE experiment. This is demonstrated on hexaaquamanganese(II). We expect that CHEESY-detected NMR is generally applicable to disordered systems and that our results further motivate the development of EPR spectrometers capable of coherent UWB excitation and detection, especially at higher fields and frequencies. Copyright © 2018 The Author(s). Published by Elsevier Inc. All rights reserved.

  4. 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.

  5. Chirp echo Fourier transform EPR-detected NMR

    Science.gov (United States)

    Wili, Nino; Jeschke, Gunnar

    2018-04-01

    A new ultra-wide band (UWB) pulse EPR method is introduced for observing all nuclear frequencies of a paramagnetic center in a single shot. It is based on burning spectral holes with a high turning angle (HTA) pulse that excites forbidden transitions and subsequent detection of the hole pattern by a chirp echo. We term this method Chirp Echo Epr SpectroscopY (CHEESY)-detected NMR. The approach is a revival of FT EPR-detected NMR. It yields similar spectra and the same type of information as electron-electron double resonance (ELDOR)-detected NMR, but with a multiplex advantage. We apply CHEESY-detected NMR in Q band to nitroxides and correlate the hyperfine spectrum to the EPR spectrum by varying the frequency of the HTA pulse. Furthermore, a selective π pulse before the HTA pulse allows for detecting hyperfine sublevel correlations between transitions of one nucleus and for elucidating the coupling regime, the same information as revealed by the HYSCORE experiment. This is demonstrated on hexaaquamanganese(II). We expect that CHEESY-detected NMR is generally applicable to disordered systems and that our results further motivate the development of EPR spectrometers capable of coherent UWB excitation and detection, especially at higher fields and frequencies.

  6. 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)

  7. 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.

  8. 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

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. NMR metabolomics of human lung tumours reveals distinct metabolic signatures for adenocarcinoma and squamous cell carcinoma

    OpenAIRE

    Rocha, CM; Barros, AS; Goodfellow, BJ; Carreira, IM; Gomes, AA; Sousa, V; Bernardo, J; Carvalho, L; Gil, AM; Duarte, IF

    2015-01-01

    Lung tumour subtyping, particularly the distinction between adenocarcinoma (AdC) and squamous cell carcinoma (SqCC), is a critical diagnostic requirement. In this work, the metabolic signatures of lung carcinomas were investigated through (1)H NMR metabolomics, with a view to provide additional criteria for improved diagnosis and treatment planning. High Resolution Magic Angle Spinning Nuclear Magnetic Resonance (NMR) spectroscopy was used to analyse matched tumour and adjacent control tissue...

  15. 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

  16. 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.

  17. Vivaldi: Visualization and validation of biomacromolecular NMR structures from the PDB

    Science.gov (United States)

    Hendrickx, Pieter M S; Gutmanas, Aleksandras; Kleywegt, Gerard J

    2013-01-01

    We describe Vivaldi (VIsualization and VALidation DIsplay; http://pdbe.org/vivaldi), a web-based service for the analysis, visualization, and validation of NMR structures in the Protein Data Bank (PDB). Vivaldi provides access to model coordinates and several types of experimental NMR data using interactive visualization tools, augmented with structural annotations and model-validation information. The service presents information about the modeled NMR ensemble, validation of experimental chemical shifts, residual dipolar couplings, distance and dihedral angle constraints, as well as validation scores based on empirical knowledge and databases. Vivaldi was designed for both expert NMR spectroscopists and casual non-expert users who wish to obtain a better grasp of the information content and quality of NMR structures in the public archive. © Proteins 2013. © 2012 Wiley Periodicals, Inc. PMID:23180575

  18. Probing the Structure and Dynamics of Proteins by Combining Molecular Dynamics Simulations and Experimental NMR Data.

    Science.gov (United States)

    Allison, Jane R; Hertig, Samuel; Missimer, John H; Smith, Lorna J; Steinmetz, Michel O; Dolenc, Jožica

    2012-10-09

    NMR experiments provide detailed structural information about biological macromolecules in solution. However, the amount of information obtained is usually much less than the number of degrees of freedom of the macromolecule. Moreover, the relationships between experimental observables and structural information, such as interatomic distances or dihedral angle values, may be multiple-valued and may rely on empirical parameters and approximations. The extraction of structural information from experimental data is further complicated by the time- and ensemble-averaged nature of NMR observables. Combining NMR data with molecular dynamics simulations can elucidate and alleviate some of these problems, as well as allow inconsistencies in the NMR data to be identified. Here, we use a number of examples from our work to highlight the power of molecular dynamics simulations in providing a structural interpretation of solution NMR data.

  19. 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.

  20. 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...

  1. Mapping of unfolding states of integral helical membrane proteins by GPS-NMR and scattering techniques

    DEFF Research Database (Denmark)

    Calcutta, Antonello; Jessen, Christian M; Behrens, Manja Annette

    2012-01-01

    induced by unfolding of an integral membrane protein, namely TFE-induced unfolding of KcsA solubilized by the n-dodecyl ß-d-maltoside (DDM) surfactant is investigated by the recently introduced GPS-NMR (Global Protein folding State mapping by multivariate NMR) (Malmendal et al., PlosONE 5, e10262 (2010......)) along with dynamic light scattering (DLS) and small-angle X-ray scattering (SAXS). GPS-NMR is used as a tool for fast analysis of the protein unfolding processes upon external perturbation, and DLS and SAXS are used for further structural characterization of the unfolding states. The combination allows...

  2. Optimal reconstruction angles

    International Nuclear Information System (INIS)

    Cook, G.O. Jr.; Knight, L.

    1979-07-01

    The question of optimal projection angles has recently become of interest in the field of reconstruction from projections. Here, studies are concentrated on the n x n pixel space, where literative algorithms such as ART and direct matrix techniques due to Katz are considered. The best angles are determined in a Gauss--Markov statistical sense as well as with respect to a function-theoretical error bound. The possibility of making photon intensity a function of angle is also examined. Finally, the best angles to use in an ART-like algorithm are studied. A certain set of unequally spaced angles was found to be preferred in several contexts. 15 figures, 6 tables

  3. 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

  4. 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.

  5. 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...

  6. 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

  7. Longitudinal changes of angle configuration in primary angle-closure suspects: the Zhongshan Angle-Closure Prevention Trial.

    Science.gov (United States)

    Jiang, Yuzhen; Chang, Dolly S; Zhu, Haogang; Khawaja, Anthony P; Aung, Tin; Huang, Shengsong; Chen, Qianyun; Munoz, Beatriz; Grossi, Carlota M; He, Mingguang; Friedman, David S; Foster, Paul J

    2014-09-01

    To determine longitudinal changes in angle configuration in the eyes of primary angle-closure suspects (PACS) treated by laser peripheral iridotomy (LPI) and in untreated fellow eyes. Longitudinal cohort study. Primary angle-closure suspects aged 50 to 70 years were enrolled in a randomized, controlled clinical trial. Each participant was treated by LPI in 1 randomly selected eye, with the fellow eye serving as a control. Angle width was assessed in a masked fashion using gonioscopy and anterior segment optical coherence tomography (AS-OCT) before and at 2 weeks, 6 months, and 18 months after LPI. Angle width in degrees was calculated from Shaffer grades assessed under static gonioscopy. Angle configuration was also evaluated using angle opening distance (AOD250, AOD500, AOD750), trabecular-iris space area (TISA500, TISA750), and angle recess area (ARA) measured in AS-OCT images. No significant difference was found in baseline measures of angle configuration between treated and untreated eyes. At 2 weeks after LPI, the drainage angle on gonioscopy widened from a mean of 13.5° at baseline to a mean of 25.7° in treated eyes, which was also confirmed by significant increases in all AS-OCT angle width measures (Pgonioscopy (P = 0.18), AOD250 (P = 0.167) and ARA (P = 0.83). In untreated eyes, angle width consistently decreased across all follow-up visits after LPI, with a more rapid longitudinal decrease compared with treated eyes (P values for all variables ≤0.003). The annual rate of change in angle width was equivalent to 1.2°/year (95% confidence interval [CI], 0.8-1.6) in treated eyes and 1.6°/year (95% CI, 1.3-2.0) in untreated eyes (P<0.001). Angle width of treated eyes increased markedly after LPI, remained stable for 6 months, and then decreased significantly by 18 months after LPI. Untreated eyes experienced a more consistent and rapid decrease in angle width over the same time period. Copyright © 2014 American Academy of Ophthalmology. Published by

  8. Additivity, redundancy, and complementarity between structural information from NMR and SAXS data

    International Nuclear Information System (INIS)

    Kojima, Masaki; Nonaka, Takamasa; Morimoto, Yasumasa; Nakagawa, Takashi; Yanagi, Shigeru; Kihara, Hiroshi

    2009-01-01

    At present protein structure in solution is determined by restrained molecular dynamics with distance restraints mainly derived from NMR. Although the small-angle X-ray scattering (SAXS) method also confers the structural information, its content is too small to determine the structure by itself. We previously developed a new algorithm that refines the protein structure by restrained molecular dynamics with SAXS constrains. In the present study we performed the protein structure calculation by restrained molecular dynamics with both NMR and SAXS constraints, in order to elucidate the essential structural information that defines the protein architecture. We used RNase T1 as a model protein, which has already been determined by NMR alone. At first we added SAXS constraints (h -1 ) into the original NMR-derived restraints for the calculation. The quality of the structure ensemble was significantly increased. Next we removed the original NMR restraints randomly in order to estimate the redundancy among the NMR-derived information. The essential topology of the resultant structures was hardly changed until the restraints were reduced below the half. Then we added the SAXS constraints into the remaining NMR restraints to expect they could complement the lost structural information. However, the structure was not recovered properly. By removing various types of structural information exclusively from the original NMR data set, we investigated whether the SAXS constraints could complement some kinds of structural information. The results showed that the SAXS could complement the tertiary structure to some extent while it could not secondary structure. (author)

  9. 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.

  10. 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 ).

  11. 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 ).

  12. 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

  13. Structural properties of carbon nanotubes derived from 13C NMR

    KAUST Repository

    Abou-Hamad, E.

    2011-10-10

    We present a detailed experimental and theoretical study on how structural properties of carbon nanotubes can be derived from 13C NMR investigations. Magic angle spinning solid state NMR experiments have been performed on single- and multiwalled carbon nanotubes with diameters in the range from 0.7 to 100 nm and with number of walls from 1 to 90. We provide models on how diameter and the number of nanotube walls influence NMR linewidth and line position. Both models are supported by theoretical calculations. Increasing the diameter D, from the smallest investigated nanotube, which in our study corresponds to the inner nanotube of a double-walled tube to the largest studied diameter, corresponding to large multiwalled nanotubes, leads to a 23.5 ppm diamagnetic shift of the isotropic NMR line position δ. We show that the isotropic line follows the relation δ = 18.3/D + 102.5 ppm, where D is the diameter of the tube and NMR line position δ is relative to tetramethylsilane. The relation asymptotically tends to approach the line position expected in graphene. A characteristic broadening of the line shape is observed with the increasing number of walls. This feature can be rationalized by an isotropic shift distribution originating from different diamagnetic shielding of the encapsulated nanotubes together with a heterogeneity of the samples. Based on our results, NMR is shown to be a nondestructive spectroscopic method that can be used as a complementary method to, for example, transmission electron microscopy to obtain structural information for carbon nanotubes, especially bulk samples.

  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. 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

  19. The rates and mechanisms of water exchange of actinide aqua ions: A variable temperature 17O NMR study of U(H2O)104+, UF(H2O)93+, and Th(H2O)104+

    International Nuclear Information System (INIS)

    Farkas, I.; Grenthe, I.; Banyai, I.

    2000-01-01

    The rate constants and the activation parameters for the exchange between water solvent and [U(H 2 O) 10 ] 4+ and [UF(H 2 O) 9 ] 3+ , and a lower limit for the rate constant at room temperature for [Th(H 2 O) 10 ] 4+ , were determined by 17 O NMR spectroscopy in the temperature range 255--305 K. The experiments were made at different constant hydrogen ion concentrations, which varied between 0.16 and 0.8 mol kg -1 . The Th(IV) system was investigated using Tb 3+ as a shift reagent. The following kinetic parameters at 25 C were obtained: k ex = (5.4 ± 0.6) 10 6 x -1 , ΔH double dagger = 34 ± 3 kJ mol -1 , ΔS ++ = -16 ± 10 J mol -1 K -1 for U 4+ (aq), k ex = (5.5 ± 0.7) 10 6 x -1 , ΔH d ouble dagger = 34 ± 3 kJ mol -1 , ΔS ++ = 3 ± 15 J mol -1 K -1 for UF 3+ (Iaq), and k ex > 5 10 7 s -1 for Th 4+ (aq), where the uncertainty is given at the 2σ-level. This is the first experimental information on the kinetic parameters for the exchange of water for any M 4+ ion. There is no information on the rates and mechanisms of ligand substitutions involving other mono-dentate ligands, hence the mechanistic interpretation of the data is by necessity provisional. The kinetic data and the known ground-state geometry with a coordination number of 10 ± 1 for the Th(IV) and U(IV) complexes suggest a dissociatively activated interchange mechanism. There is no noticeable effect of coordination of one fluoride or one hydroxide to U(IV) on the water exchange rate. This is unusual, for other metal ions there is a strong labilizing of coordinated water when a second ligand is bonded, e.g., in complexes of aluminum and some d-transition elements. In previous studies of the rates and mechanisms of ligand exchange in uranium (VI) systems the authors found a strong decrease in the lability of coordinated water in some fluoride containing complexes

  20. Adiabatic-passage cross polarization in N-15 NMR spectroscopy of peptides weakly associated to phospholipids: Determination of large RDC

    International Nuclear Information System (INIS)

    Zandomeneghi, Giorgia; Meier, Beat H.

    2004-01-01

    Structural information can be extracted from one-bond residual dipolar couplings (RDC) measured in NMR spectra of systems in field-ordered media. RDC can be on the order of J-couplings if the anisotropy of alignment is ∼ 10 -2 , 10-fold stronger than that typically used for structural studies of water-soluble proteins. In such systems the performance of 1 H → 15 N polarization transfer methods of the INEPT type is not satisfactory. In this study we show the effectiveness of adiabatic-passage cross-polarization (APCP) in transferring the 1 H → 15 N polarization in the bicelle-associated peptide Leucine Enkephalin (Lenk). APCP is efficient both in static samples and in samples spun at the magic angle (MAS) or any other angle of the spinning axis to the magnetic field (variable-angle spinning, VAS). The anisotropic spectrum of an aligned static sample and the isotropic spectrum of the sample under MAS provide a set of possible values for the 1 H- 15 N RDC of phospholipid-associated Lenk. The unambiguous determination of the 1 H- 15 N RDC was accomplished by means of VAS experiments

  1. Unraveling the meaning of chemical shifts in protein NMR.

    Science.gov (United States)

    Berjanskii, Mark V; Wishart, David S

    2017-11-01

    Chemical shifts are among the most informative parameters in protein NMR. They provide wealth of information about protein secondary and tertiary structure, protein flexibility, and protein-ligand binding. In this report, we review the progress in interpreting and utilizing protein chemical shifts that has occurred over the past 25years, with a particular focus on the large body of work arising from our group and other Canadian NMR laboratories. More specifically, this review focuses on describing, assessing, and providing some historical context for various chemical shift-based methods to: (1) determine protein secondary and super-secondary structure; (2) derive protein torsion angles; (3) assess protein flexibility; (4) predict residue accessible surface area; (5) refine 3D protein structures; (6) determine 3D protein structures and (7) characterize intrinsically disordered proteins. This review also briefly covers some of the methods that we previously developed to predict chemical shifts from 3D protein structures and/or protein sequence data. It is hoped that this review will help to increase awareness of the considerable utility of NMR chemical shifts in structural biology and facilitate more widespread adoption of chemical-shift based methods by the NMR spectroscopists, structural biologists, protein biophysicists, and biochemists worldwide. This article is part of a Special Issue entitled: Biophysics in Canada, edited by Lewis Kay, John Baenziger, Albert Berghuis and Peter Tieleman. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. 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.

  3. 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

  4. NMR-Metabolic Methodology in the Study of GM Foods

    Directory of Open Access Journals (Sweden)

    Irene D’Amico

    2010-01-01

    Full Text Available The 1H-NMR methodology used in the study of genetically modified (GM foods is discussed. Transgenic lettuce (Lactuca sativa cv "Luxor" over-expressing the Arabidopsis KNAT1 gene is presented as a case study. Twenty-two water-soluble metabolites (amino acids, organic acids, sugars present in leaves of conventional and GM lettuce were monitored by NMR and quantified at two developmental stages. The NMR spectra did not reveal any difference in metabolite composition between the GM lettuce and the wild type counterpart. Statistical analyses of metabolite variables highlighted metabolism variation as a function of leaf development as well as the transgene. A main effect of the transgene was in altering sugar metabolism.

  5. The method of the gas-dynamic centrifugal compressor stage characteristics recalculation for variable rotor rotational speeds and the rotation angle of inlet guide vanes blades if the kinematic and dynamic similitude conditions are not met

    Science.gov (United States)

    Vanyashov, A. D.; Karabanova, V. V.

    2017-08-01

    A mathematical description of the method for obtaining gas-dynamic characteristics of a centrifugal compressor stage is proposed, taking into account the control action by varying the rotor speed and the angle of rotation of the guide vanes relative to the "basic" characteristic, if the kinematic and dynamic similitude conditions are not met. The formulas of the correction terms for the non-dimensional coefficients of specific work, consumption and efficiency are obtained. A comparative analysis of the calculated gas-dynamic characteristics of a high-pressure centrifugal stage with experimental data is performed.

  6. 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

  7. Investigation of the dynamic NMR frequency shift for Fe57 in FeBO3

    International Nuclear Information System (INIS)

    Bun'kov, Yu.M.; Punkkinen, M.; Yulinen, E.E.

    1978-01-01

    NMR of Fe 57 in FeBO 3 is investigated by pulsed magnetic resonance techniques in the 2 to 70 K temperature range. A dynamic NMR frequency shift is observed which is due to coupling between the NMR oscillations and the low-frequency AFMR mode, the magnitude of which only slightly exceeds the micro-inhomogeneous broadening of the NMR line caused by the spread of the value of hyperfine field at the nuclei. Under these conditions the nuclear spin system possesses a number of unusual properties. Thus, broadening of the magnetic resonance line is uniform, the magnitude of the homogeneous broadening depends on the angle of deviation of the nuclear magnetization from the equilibrium axis, and an echo signal is detected which is similar to the ''solid echo'' in substances with dipole broadening of the magnetic resonance line

  8. 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

  9. Solid-state 27Al and 29Si NMR investigations on Si-substituted hydrogarnets

    International Nuclear Information System (INIS)

    Rivas Mercury, J.M.; Pena, P.; Aza, A.H. de; Turrillas, X.; Sobrados, I.; Sanz, J.

    2007-01-01

    Partially deuterated Ca 3 Al 2 (SiO 4 ) 3-x (OH) 4x hydrates prepared by a reaction in the presence of D 2 O of synthetic tricalcium aluminate with different amounts of amorphous silica were characterized by 29 Si and 27 Al magic-angle spinning nuclear magnetic resonance (NMR) spectroscopy. The 29 Si NMR spectroscopy was used for quantifying the non-reacted silica and the resulting hydrated products. The incorporation of Si into Ca 3 Al 2 (SiO 4 ) 3-x (OH) 4x was followed by 27 Al NMR spectroscopy: Si:OH ratios were determined quantitatively from octahedral Al signals ascribed to Al(OH) 6 and Al(OSi)(OH) 5 environments. The NMR data obtained were consistent with the concentrations of the Al and Si species deduced from transmission electron microscopy energy-dispersive spectrometry and Rietveld analysis of both X-ray and neutron diffraction data

  10. In vivo quantitative NMR imaging of fruit tissues during growth using Spoiled Gradient Echo sequence

    DEFF Research Database (Denmark)

    Kenouche, S.; Perrier, M.; Bertin, N.

    2014-01-01

    of this study was to design a robust and accurate quantitative measurement method based on NMR imaging combined with contrast agent (CA) for mapping and quantifying water transport in growing cherry tomato fruits. A multiple flip-angle Spoiled Gradient Echo (SGE) imaging sequence was used to evaluate...

  11. High-resolution proton and carbon-13 NMR of membranes: why sonicate?

    International Nuclear Information System (INIS)

    Oldfield, E.; Bowers, J.L.; Forbes, J.

    1987-01-01

    The authors have obtained high-field (11.7-T) proton and carbon-13 Fourier transform (FT) nuclear magnetic resonance (NMR) spectra of egg lecithin and egg lecithin-chloresterol (1:1) multibilayers, using magic-angle sample spinning (MASS) techniques, and sonicated egg lecithin and egg lecithin-cholesterol (1:1) vesicles, using conventional FT NMR methods. Resolution of the proton and carbon-13 MASS NMR spectra of the pure egg lecithin samples is essentially identical with that of sonicated samples, but spectra of the unsonicated lipid, using MASS, can be obtained very much faster than with the more dilute, sonicated systems. With the 1:1 lecithin-cholesterol system, proton MASS NMR spectra are virtually identical with conventional FT spectra of sonicated samples, while the 13 C NMR, the authors demonstrate that most 13 C nuclei in the cholesterol moiety can be monitored, even though these same nuclei are essentially invisible, i.e., are severely broadened, in the corresponding sonicated systems. In addition, 13 C MASS NMR spectra can again be recorded much faster than with sonicated samples, due to concentration effects. Taken together, these results strongly suggest there will seldom be need in the future to resort to ultransonic disruption of lipid bilayer membranes in order to obtain high-resolution proton or carbon-13 NMR spectra

  12. 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.

  13. 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.

  14. Metabolomics by Proton High-Resolution Magic-Angle-Spinning Nuclear Magnetic Resonance of Tomato Plants Treated with Two Secondary Metabolites Isolated from Trichoderma.

    Science.gov (United States)

    Mazzei, Pierluigi; Vinale, Francesco; Woo, Sheridan Lois; Pascale, Alberto; Lorito, Matteo; Piccolo, Alessandro

    2016-05-11

    Trichoderma fungi release 6-pentyl-2H-pyran-2-one (1) and harzianic acid (2) secondary metabolites to improve plant growth and health protection. We isolated metabolites 1 and 2 from Trichoderma strains, whose different concentrations were used to treat seeds of Solanum lycopersicum. The metabolic profile in the resulting 15 day old tomato leaves was studied by high-resolution magic-angle-spinning nuclear magnetic resonance (HRMAS NMR) spectroscopy directly on the whole samples without any preliminary extraction. Principal component analysis (PCA) of HRMAS NMR showed significantly enhanced acetylcholine and γ-aminobutyric acid (GABA) content accompanied by variable amount of amino acids in samples treated with both Trichoderma secondary metabolites. Seed germination rates, seedling fresh weight, and the metabolome of tomato leaves were also dependent upon doses of metabolites 1 and 2 treatments. HRMAS NMR spectroscopy was proven to represent a rapid and reliable technique for evaluating specific changes in the metabolome of plant leaves and calibrating the best concentration of bioactive compounds required to stimulate plant growth.

  15. The quadriceps angle

    DEFF Research Database (Denmark)

    Miles, James Edward; Frederiksen, Jane V.; Jensen, Bente Rona

    2012-01-01

    : Pelvic limbs from red foxes (Vulpes vulpes). METHODS: Q angles were measured on hip dysplasia (HD) and whole limb (WL) view radiographs of each limb between the acetabular rim, mid-point (Q1: patellar center, Q2: femoral trochlea), and tibial tuberosity. Errors of 0.5-2.0 mm at measurement landmarks...

  16. open angle glaucoma (poag)?

    African Journals Online (AJOL)

    there is a build up of pressure due to poor outflow of aqueous humor. The outflow obstruction could occur at the trabecular meshwork of the anterior chamber angle or subsequently in the episcleral vein due to raised venous pressure. Such build up of pressure results in glaucoma . Elevated intraocular pressure remains the ...

  17. The lateral angle revisited

    DEFF Research Database (Denmark)

    Morgan, Jeannie; Lynnerup, Niels; Hoppa, R.D.

    2013-01-01

    measurements taken from computed tomography (CT) scans. Previous reports have observed that the lateral angle size in females is significantly larger than in males. The method was applied to an independent series of 77 postmortem CT scans (42 males, 35 females) to validate its accuracy and reliability...... method appears to be of minimal practical use in forensic anthropology and archeology....

  18. At Right Angles

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 17; Issue 9. At Right Angles. Shailesh A Shirali. Information and Announcements Volume 17 Issue 9 September 2012 pp 920-920. Fulltext. Click here to view fulltext PDF. Permanent link: https://www.ias.ac.in/article/fulltext/reso/017/09/0920-0920 ...

  19. Wide angle isotope separator

    International Nuclear Information System (INIS)

    Kantrowitz, A.

    1976-01-01

    A method and apparatus is described for particle separation. The method uses a wide angle radially expanding vapor of a particle mixture. In particular, selective ionization of one isotope type in the particle mixture is produced in a multichamber separator and the ionized isotope type is accelerated out of the path of the vapor expansion for separate collection

  20. NMR signal transducer

    International Nuclear Information System (INIS)

    Kucheryaev, A.G.; Oliferchuk, N.L.

    1975-01-01

    A signal transducer of nuclear magnetic resonance for simultaneously measuring frequency and intensitivity of two various isotope signals, which are in one specimen is described. The transducer represents radiofrequency circuit with two resonance frequences, which is common for two autodyne generators. To decrease measuring time and to increase recording diagram stability the radiofrequency circuit has LC netork, in the inductivity of which investigated specimen is located; a circuit variable capacity is connected in parallel with one of the autodyne generators. Besides the radiofrequency circuit has an inductance coil in series with a standard specimen inside as well as a variable capacitor connected in parallel with the second autodyne generator. An amplitude of oscillation of each resonance frequency is controlled and adjusted separately. The transducer described can be used for the measurement of a nuclei concentration, isotope concentration and for the spin determination

  1. 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

  2. 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

  3. Neural Network Control for Variable Pitch Angle in Grid Connected Wind Turbine%并网风力机中基于变桨距角的神经网络控制方法

    Institute of Scientific and Technical Information of China (English)

    王凌云; 张涛; 孟娟

    2012-01-01

    针对并网风力机的运行特性,在其传动系统和发电机的动态模型基础上设计控制器.当外界风速较大,提出采用基于神经网络的风力机叶片桨距角控制器抑制多余的风能进入发电系统,维持风力发电机馈送到电网的功率稳定;当风速较低时,风力机转速需要跟随风速变化,调整叶片桨距角处于捕捉最大风能位置处,保证风力机的风能转换效率最优,提高其运行效率.仿真结果验证了该控制方法的有效性.%For the operation characteristics of a grid connected wind turbine, two controllers are designed based on the dynamical model of the wind turbine drive system and generator. When the wind speed is higher, the neural network controller of the turbine blades pitch angle is proposed to restrict the excess wind energy entering the generation system in order to keep the power injected into the grid stable. Meanwhile, when the wind speed is lower, the turbine speed is changed with the variation of wind speed by adjusting the blades angle at the value of capturing maximum wind power, then the optimal wind energy conversion efficiency is guaranteed. The simulation results verify this control method is highly effective.

  4. Effect of water injection and off scheduling of variable inlet guide vanes, gas generator speed and power turbine nozzle angle on the performance of an automotive gas turbine engine

    Science.gov (United States)

    Warren, E. L.

    1980-01-01

    The Chrysler/ERDA baseline automotive gas turbine engine was used to experimentally determine the power augmentation and emissions reductions achieved by the effect of variable compressor and power engine geometry, water injection downstream of the compressor, and increases in gas generator speed. Results were dependent on the mode of variable geometry utilization. Over 20 percent increase in power was accompanied by over 5 percent reduction in SFC. A fuel economy improvement of at least 6 percent was estimated for a vehicle with a 75 kW (100 hp) engine which could be augmented to 89 kW (120 hp) relative to an 89 Kw (120 hp) unaugmented engine.

  5. 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...

  6. 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.

  7. 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

  8. 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

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. 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...

  14. Small angle neutron scattering

    International Nuclear Information System (INIS)

    Bernardini, G.; Cherubini, G.; Fioravanti, A.; Olivi, A.

    1976-09-01

    A method for the analysis of the data derived from neutron small angle scattering measurements has been accomplished in the case of homogeneous particles, starting from the basic theory without making any assumption on the form of particle size distribution function. The experimental scattering curves are interpreted with the aid the computer by means of a proper routine. The parameters obtained are compared with the corresponding ones derived from observations at the transmission electron microscope

  15. Determination of solid angle

    International Nuclear Information System (INIS)

    Qiu, S.; Amano, H.; Kasai, A.

    1988-01-01

    The solid angle in extended alpha source measurement for a series of counting geometries has been obtained by two methods: (1) calculated by means of the Nelson Blachmen series; (2) interpolated from the data table given by Gardner. A particular consequence of the application of the Nelson Blachmen series was deduced which was different from that given by the original author. The applicability of these two methods, as well as an experimentally measured method, is also evaluated. (author)

  16. Longitudinal Changes of Angle Configuration in Primary Angle-Closure Suspects

    Science.gov (United States)

    Jiang, Yuzhen; Chang, Dolly S.; Zhu, Haogang; Khawaja, Anthony P.; Aung, Tin; Huang, Shengsong; Chen, Qianyun; Munoz, Beatriz; Grossi, Carlota M.

    2015-01-01

    Objective To determine longitudinal changes in angle configuration in the eyes of primary angle-closure suspects (PACS) treated by laser peripheral iridotomy (LPI) and in untreated fellow eyes. Design Longitudinal cohort study. Participants Primary angle-closure suspects aged 50 to 70 years were enrolled in a randomized, controlled clinical trial. Methods Each participant was treated by LPI in 1 randomly selected eye, with the fellow eye serving as a control. Angle width was assessed in a masked fashion using gonioscopy and anterior segment optical coherence tomography (AS-OCT) before and at 2 weeks, 6 months, and 18 months after LPI. Main Outcome Measures Angle width in degrees was calculated from Shaffer grades assessed under static gonioscopy. Angle configuration was also evaluated using angle opening distance (AOD250, AOD500, AOD750), trabecular-iris space area (TISA500, TISA750), and angle recess area (ARA) measured in AS-OCT images. Results No significant difference was found in baseline measures of angle configuration between treated and untreated eyes. At 2 weeks after LPI, the drainage angle on gonioscopy widened from a mean of 13.5° at baseline to a mean of 25.7° in treated eyes, which was also confirmed by significant increases in all AS-OCT angle width measures (Pgonioscopy (P = 0.18), AOD250 (P = 0.167) and ARA (P = 0.83). In untreated eyes, angle width consistently decreased across all follow-up visits after LPI, with a more rapid longitudinal decrease compared with treated eyes (P values for all variables ≤0.003). The annual rate of change in angle width was equivalent to 1.2°/year (95% confidence interval [CI], 0.8–1.6) in treated eyes and 1.6°/year (95% CI, 1.3–2.0) in untreated eyes (P<0.001). Conclusions Angle width of treated eyes increased markedly after LPI, remained stable for 6 months, and then decreased significantly by 18 months after LPI. Untreated eyes experienced a more consistent and rapid decrease in angle width over the

  17. Visualization of cerebellopontine angle lesions by nuclear magnetic resonance imaging

    International Nuclear Information System (INIS)

    Ochiai, Chikayuki; Takakura, Kintomo; Machida, Tohru; Araki, Tsutomu; Iio, Masahiro; Basugi, Norihiko.

    1983-01-01

    The preliminary results from the clinical use a prototype whole body nuclear magnetic resonance (NMR) machine constructed by Toshiba Inc. are presented. Cranial NMR scans were performed on more than 30 cases with broad spectrum of neurologic diseases using saturation-recovery and inversion-recovery sequences with a field strength of 1500 Gauss. Selective excitation sequence was used for the slice selection and filtered backprojection was used to reconstruct the images. They were displayed on a 256 x 256 matrix as 12 mm thick sections. Data aquisition time varied between 3 and 12 minutes. Our initial experiences with six cases harboring cerebellopontine angle lesions discolsed advantages and disadvantages of NMR imaging in comparison with X-ray CT. The advantages were the absence of linear artifacts from the surrounding bone, the marked gray-white matter differentiation, and the variety of tomographic planes available. The disadvantages included the lack of bone detail, the lack of visualization of the major intracranial vessels, and the long time required for scanning (several minutes per slice). Although much continued evaluation is necessary, NMR seems to have vast potential as a diagnostic tool. (author)

  18. Note on sideband intensities in one-dimensional magic angle spinning nuclear magnetic resonance

    NARCIS (Netherlands)

    Well, van H.F.J.M.; Vankan, J.M.J.; Janssen, A.J.E.M.

    1991-01-01

    It is well known that in the NMR spectra of solid samples spinning at the magic angle centrebands and sidebands occur. The centrebands are found at the isotropic value of the chemical shift and the sidebands are found at integral multiples of the spinning frequency as long as the spinning frequency

  19. The Dual-Angle Method for Fast, Sensitive T1 Measurement in Vivo with Low-Angle Adiabatic Pulses

    Science.gov (United States)

    Bottomley, P. A.; Ouwerkerk, R.

    A new method for measuring T1 based on a measurement of the ratio, R, of the steady-state partially saturated NMR signals acquired at two fixed low flip angles (hip-angle and excitation-field ( B1) inhomogeneity result in roughly proportionate errors in the apparent T1. The method is best implemented with adiabatic low-angle pulses such as B1-independent rotation (BIR-4) or BIR-4 phase-cycled (BIRP) pulses, which permit measurements with surface coils. Experimental validation was obtained at 2 T by comparison of unlocalized inversion-recovery and dual-angle proton ( 1H) and phosphorus ( 31P) measurements from vials containing doped water with 0.04 ≤ T1 ≤ 2.8 s and from the metabolites in the calf muscles of eight human volunteers. Calf muscle values of 6 ± 0.5 s for phosphocreatine and around 3.7 ± 0.8 s for the adenosine triphosphates (ATP) were in good agreement with inversion-recovery T1 values and values from the literature. Use of the dual-angle method accelerated T1 measurement time by about fivefold over inversion recovery. The dual-angle method was implemented in a one-dimensional localized surface-coil 31P spectroscopy sequence, producing consistent T1 measurements from phantoms, the calf muscle, and the human liver. 31P T1 values of ATP in the livers of six volunteers were about 0.5 ± 0.1 to 0.6 ± 0.2 s: the total exam times were about 35 minutes per subject. The method is ideally suited to low-sensitivity and/or low-concentration moieties, such as in 31P NMR in vivo, where study-time limitations are critical, and for rapid 1H T1 imaging.

  20. Computer software for linear and nonlinear regression in organic NMR

    International Nuclear Information System (INIS)

    Canto, Eduardo Leite do; Rittner, Roberto

    1991-01-01

    Calculation involving two variable linear regressions, require specific procedures generally not familiar to chemist. For attending the necessity of fast and efficient handling of NMR data, a self explained and Pc portable software has been developed, which allows user to produce and use diskette recorded tables, containing chemical shift or any other substituent physical-chemical measurements and constants (σ T , σ o R , E s , ...)

  1. The influence of flip angle on the magic angle effect

    International Nuclear Information System (INIS)

    Zurlo, J.V.; Blacksin, M.F.; Karimi, S.

    2000-01-01

    Objective. To assess the impact of flip angle with gradient sequences on the ''magic angle effect''. We characterized the magic angle effect in various gradient echo sequences and compared the signal- to-noise ratios present on these sequences with the signal-to-noise ratios of spin echo sequences.Design. Ten normal healthy volunteers were positioned such that the flexor hallucis longus tendon remained at approximately at 55 to the main magnetic field (the magic angle). The tendon was imaged by a conventional spin echo T1- and T2-weighted techniques and by a series of gradient techniques. Gradient sequences were altered by both TE and flip angle. Signal-to-noise measurements were obtained at segments of the flexor hallucis longus tendon demonstrating the magic angle effect to quantify the artifact. Signal-to-noise measurements were compared and statistical analysis performed. Similar measurements were taken of the anterior tibialis tendon as an internal control.Results and conclusions. We demonstrated the magic angle effect on all the gradient sequences. The intensity of the artifact was affected by both the TE and flip angle. Low TE values and a high flip angle demonstrated the greatest magic angle effect. At TE values less than 30 ms, a high flip angle will markedly increase the magic angle effect. (orig.)

  2. 11B NMR study of calcium-hexaborides

    International Nuclear Information System (INIS)

    Mean, B.J.; Lee, K.H.; Kang, K.H.; Lee, Moohee; Rhee, J.S.; Cho, B.K.

    2005-01-01

    We have performed 11 B nuclear magnetic resonance (NMR) measurements to look for microscopic evidence of the ferromagnetic state in several CaB 6 single crystals. A number of 11 B NMR resonance peaks are observed with the frequency and intensity of those peaks distinctively changing depending on the angle between the crystalline axis and a magnetic field. Analyzing this behavior, we find that the electric field gradient tensor at the boron has its principal axis perpendicular to the six cubic faces with a quadrupole resonance frequency ν Q ∼600kHz. However, the satellite resonances are found to be made of two peaks. Detailed analysis of the four composite satellite peaks confirms that there are two different boron sites with slightly different ν Q 's. This suggests that the boron octahedron cages are locally distorted. However, this distortion is not directly related to ferromagnetism. Even though the magnetization data highlight the ferromagnetic hysteresis, 11 B NMR linewidth and shift data show no clear microscopic evidence of the ferromagnetic state in several different compositions of CaB 6 single crystals

  3. High resolution NMR theory and chemical applications

    CERN Document Server

    Becker, Edwin D

    1999-01-01

    High Resolution NMR provides a broad treatment of the principles and theory of nuclear magnetic resonance (NMR) as it is used in the chemical sciences. It is written at an "intermediate" level, with mathematics used to augment, rather than replace, clear verbal descriptions of the phenomena. The book is intended to allow a graduate student, advanced undergraduate, or researcher to understand NMR at a fundamental level, and to see illustrations of the applications of NMR to the determination of the structure of small organic molecules and macromolecules, including proteins. Emphasis is on the study of NMR in liquids, but the treatment also includes high resolution NMR in the solid state and the principles of NMR imaging and localized spectroscopy. Careful attention is given to developing and interrelating four approaches - steady state energy levels, the rotating vector picture, the density matrix, and the product operator formalism. The presentation is based on the assumption that the reader has an acquaintan...

  4. Uniform and selective deuteration in two-dimensional NMR of proteins

    International Nuclear Information System (INIS)

    LeMaster, D.M.

    1990-01-01

    This paper reports on the practicality of isotopic labeling, particularly deuteration, that has received considerable impetus from advances in molecular biology, which have allowed ready production of NMR quantities of labeled proteins. Protein expression in Escherichia coli allows use of the considerable metabolic genetics known for the organism in shaping the biosynthetic process to meet the labeling demands of the NMR experiments. In addition to deuteration's common use in spectral assignment problems, it also offers considerable potential for enhancing the quality of the nuclear Overhauser effect (NOE) distance and dihedral angle constraints used for solution structural analysis of proteins. Recent reviews emphasize the sample preparation and spectral benefits of protein deuteration

  5. PVT Degradation Studies: NMR Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Herman M. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Kouzes, Richard T. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2017-06-06

    Under certain environmental conditions, polyvinyl toluene (PVT) plastic scintillator has been observed to undergo internal fogging. Nuclear magnetic resonance spectroscopy has been used to elucidate the state of water inside the PVT. The deuterium NMR results show that water absorbed by PVT under warm, humid conditions enters several distinct environments, and when the PVT is transferred from incubation to ambient temperature and humidity the water is lost on a time scale of a few hours from these samples. Most of the deuterium NMR peaks can be assigned to bulk liquid water, but almost 35% of the detected signal intensity is contained in a resonance that resembles spectra of water contained in nanometer-scale pores in mesoporous carbon.

  6. NMR imaging of human atherosclerosis

    International Nuclear Information System (INIS)

    Toussaint, J.F.

    1995-01-01

    Diagnosis and prognosis of atherosclerosis can no longer be evaluated with morphological parameters only. A description of atherosclerotic plaque composition is necessary to study the mechanisms of plaque rupture, which depends on collagenous cap and lipid core thicknesses. NMR, as a biochemical imaging technique, allows visualization of these components using T1 contrast (mobile lipids), T2 contrast (cap vs. core), spin density (calcifications), diffusion imaging, 1H and 13C spectroscopy. Today, these imaging sequences allow to study in vitro the effects of interventional techniques such as angioplasty or atherectomy. Clinical investigations begin, which will attempt to develop in vivo microscopy and test the ability of NMR to predict plaque rupture. (author). 13 refs., 7 figs

  7. High resolution NMR in zeolites

    Energy Technology Data Exchange (ETDEWEB)

    Diaz, Anix [INTEVEP, Filial de Petroleos de Venezuela, SA, Caracas (Venezuela). Dept. de Analisis y Evalucion

    1992-12-31

    In this work {sup 29} Si and {sup 27} Al NMR spectroscopy was used to study various types of zeolites. The corresponding spectra were used to measure the Si/Al ratios, to follow chemical modifications induced by acid and hydrothermal treatments, to determine non-equivalent crystallographic sites in highly dealuminated mordenites, and to detect modifications of faujasites due to the insertion of titanium atoms in the lattice. (author) 7 refs., 7 figs., 2 tabs.

  8. High resolution NMR in zeolites

    International Nuclear Information System (INIS)

    Diaz, Anix

    1991-01-01

    In this work 29 Si and 27 Al NMR spectroscopy was used to study various types of zeolites. The corresponding spectra were used to measure the Si/Al ratios, to follow chemical modifications induced by acid and hydrothermal treatments, to determine non-equivalent crystallographic sites in highly dealuminated mordenites, and to detect modifications of faujasites due to the insertion of titanium atoms in the lattice. (author)

  9. Trispyrazolylborate Complexes: An Advanced Synthesis Experiment Using Paramagnetic NMR, Variable-Temperature NMR, and EPR Spectroscopies

    Science.gov (United States)

    Abell, Timothy N.; McCarrick, Robert M.; Bretz, Stacey Lowery; Tierney, David L.

    2017-01-01

    A structured inquiry experiment for inorganic synthesis has been developed to introduce undergraduate students to advanced spectroscopic techniques including paramagnetic nuclear magnetic resonance and electron paramagnetic resonance. Students synthesize multiple complexes with unknown first row transition metals and identify the unknown metals by…

  10. IR and NMR spectroscopic correlation of enterobactin by DFT

    Science.gov (United States)

    Moreno, M.; Zacarias, A.; Porzel, A.; Velasquez, L.; Gonzalez, G.; Alegría-Arcos, M.; Gonzalez-Nilo, F.; Gross, E. K. U.

    2018-06-01

    Emerging and re-emerging epidemic diseases pose an ongoing threat to global health. Currently, Enterobactin and Enterobactin derivatives have gained interest, owing to their potential application in the pharmaceutical field. As it is known [J. Am. Chem. Soc (1979) 101, 20, 6097-6104], Enterobactin (H6EB) is an efficient iron carrier synthesized and secreted by many microbial species. In order to facilitate the elucidation of enterobactin and its analogues, here we propose the creation of a H6EB standard set using Density Functional Theory Infrared (IR) and NMR spectra. We used two exchange-correlation (xc) functionals (PBE including long-range corrections sbnd LC-PBEsbnd and mPW1), 2 basis sets (QZVP and 6-31G(d)) and 2 grids (fine and ultrafine) for most of the H6EB structures dependent of dihedral angles. The results show a significant difference between the Osbnd H and Nsbnd H bands, while the Cdbnd O amide and Osbnd (Cdbnd O)sbnd IR bands are often found on top of each other. The NMR DFT calculations show a strong dependence on the xc functional, basis set, and grid used for the H6EB structure. Calculated 1H and 13C NMR spectra enable the effect of the solvent to be understood in the context of the experimental measurements. The good agreement between the experimental and the calculated spectra using LC-PBE/QZVP and ultrafine grid suggest the possibility of the systems reported here to be considered as a standard set. The dependence of electrostatic potential and frontier orbitals with the catecholamide dihedral angles of H6EB is described. The matrix-assisted laser desorption/ionization time of the flight mass spectrometry (MALDI-TOF MS) of H6EB is also reported of manner to enrich the knowledge about its reactivity.

  11. Advanced NMR technology for bioscience and biotechnology

    Energy Technology Data Exchange (ETDEWEB)

    Hammel, P.C.; Hernandez, G.; Trewhella, J.; Unkefer, C.J. [Los Alamos National Lab., NM (US); Boumenthal, D.K. [Univ. of Utah, Salt Lake City, UT (US); Kennedy, M.A. [Pacific Northwest National Lab., Richland, WA (US); Moore, G.J. [Wayne State Univ., Detroit, MI (US)

    1998-11-01

    This is the final report of a three-year, Laboratory Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). NMR plays critical roles in bioscience and biotechnology in both imaging and structure determination. NMR is limited, however, by the inherent low sensitivity of the NMR experiment and the demands for spectral resolution required to study biomolecules. The authors addressed both of these issues by working on the development of NMR force microscopy for molecular imaging, and high field NMR with isotope labeling to overcome limitations in the size of biomolecules that can be studied using NMR. A novel rf coil design for NMR force microscopy was developed that increases the limits of sensitivity in magnetic resonance detection for imaging, and the authors demonstrated sub-surface spatial imaging capabilities. The authors also made advances in the miniaturization of two critical NMR force microscope components. They completed high field NMR and isotope labeling studies of a muscle protein complex which is responsible for regulating muscle contraction and is too large for study using conventional NMR approaches.

  12. Solid-state NMR of inorganic semiconductors.

    Science.gov (United States)

    Yesinowski, James P

    2012-01-01

    Studies of inorganic semiconductors by solid-state NMR vary widely in terms of the nature of the samples investigated, the techniques employed to observe the NMR signal, and the types of information obtained. Compared with the NMR of diamagnetic non-semiconducting substances, important differences often result from the presence of electron or hole carriers that are the hallmark of semiconductors, and whose theoretical interpretation can be involved. This review aims to provide a broad perspective on the topic for the non-expert by providing: (1) a basic introduction to semiconductor physical concepts relevant to NMR, including common crystal structures and the various methods of making samples; (2) discussions of the NMR spin Hamiltonian, details of some of the NMR techniques and strategies used to make measurements and theoretically predict NMR parameters, and examples of how each of the terms in the Hamiltonian has provided useful information in bulk semiconductors; (3) a discussion of the additional considerations needed to interpret the NMR of nanoscale semiconductors, with selected examples. The area of semiconductor NMR is being revitalized by this interest in nanoscale semiconductors, the great improvements in NMR detection sensitivity and resolution that have occurred, and the current interest in optical pumping and spintronics-related studies. Promising directions for future research will be noted throughout.

  13. A 125Te and 23Na NMR investigation of the structure and crystallisation of sodium tellurite glasses.

    Science.gov (United States)

    Holland, D; Bailey, J; Ward, G; Turner, B; Tierney, P; Dupree, R

    2005-01-01

    125Te static nuclear magnetic resonance (NMR) and 23Na and 125Te magic angle spinning (MAS) NMR have been used, in conjunction with X-ray diffraction, to examine the structure and crystallisation behaviour of glasses of composition xNa2O.(1-x)TeO2 (0.075 x 0.4). The MAS NMR 23Na spectra from the glasses are broad and featureless but shift by approximately +5 ppm with increased x, i.e. as the system becomes more ionic. The static 125Te NMR spectra show an increase in axial symmetry with increasing x, indicating a shift from predominantly [TeO4] to [TeO3] structural units. The 23Na and 125Te spectra from the crystallised samples have been fitted to obtain information on the sites in the metastable crystal phases, which are the first to form on heating and which are therefore more closely related to the glass structure than thermodynamically stable crystal phases. New sodium tellurite phases are reported, including a sodium stabilised, face centred cubic phase related to delta-TeO2; a metastable form of Na2Te4O9 containing 3 sodium and 4 tellurium sites; and a metastable form of Na2Te2O5 containing 2 sodium sites. There is evidence of oxidation of TeIV to TeVI occurring in glasses with high values of x and, at x=0.40 and 0.50 (outside the glass forming range), some sodium metatellurate (Na2TeO4) is formed at the same time as sodium metatellurite (Na2TeO3). The 125Te shift is very sensitive to environment within the sodium tellurite system, covering more than 320 ppm, with anisotropies varying from 640 to 1540 ppm. The lack of features in the 125Te spectra of the glass phases, combined with the large shift range and high but variable anisotropy, means than it is not possible to obtain a unique fit to any presumed species present. Furthermore, the chemical shift anisotropy parameters for three of the four Te sites in the Na2Te4O9 phase are found to lie outside the range used for previous simulations of glass spectra.

  14. Equilibrium contact angle or the most-stable contact angle?

    Science.gov (United States)

    Montes Ruiz-Cabello, F J; Rodríguez-Valverde, M A; Cabrerizo-Vílchez, M A

    2014-04-01

    It is well-established that the equilibrium contact angle in a thermodynamic framework is an "unattainable" contact angle. Instead, the most-stable contact angle obtained from mechanical stimuli of the system is indeed experimentally accessible. Monitoring the susceptibility of a sessile drop to a mechanical stimulus enables to identify the most stable drop configuration within the practical range of contact angle hysteresis. Two different stimuli may be used with sessile drops: mechanical vibration and tilting. The most stable drop against vibration should reveal the changeless contact angle but against the gravity force, it should reveal the highest resistance to slide down. After the corresponding mechanical stimulus, once the excited drop configuration is examined, the focus will be on the contact angle of the initial drop configuration. This methodology needs to map significantly the static drop configurations with different stable contact angles. The most-stable contact angle, together with the advancing and receding contact angles, completes the description of physically realizable configurations of a solid-liquid system. Since the most-stable contact angle is energetically significant, it may be used in the Wenzel, Cassie or Cassie-Baxter equations accordingly or for the surface energy evaluation. © 2013 Elsevier B.V. All rights reserved.

  15. 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.

  16. The characterization of NMR signal for blood pressure monitoring system and its testing

    Directory of Open Access Journals (Sweden)

    Bambang Murdaka Eka Jati

    2016-02-01

    Full Text Available ABSTRACT A blood monitoring system based on NMR method has been designed on constructed. This set-up of equipment used magnetic permanent, radio frequency (RF, receiver coil (RC, function generator (FG, amplifier which included the filter, as well as the oscilloscope digital storage. The background of this research was based on the sensitivity of NMR signal. The signal must be separated from signals background. This method was done by adjusting the frequency on FG, which was connected to radio frequency (RF coil, on empty sample. Subsequently, NMR signal was received by RC, and that signal could be shown on oscilloscope at resonance condition. The true frequency on NMR signal was Larmor frequency, and the other was background. The two variables of this experiment were the position of RF coil and the location temperature (20 up to 30oC. In conclusion, the resonance frequency of NMR signal (as Larmor frequency was 4.7 MHz (at static magnetic field of 1,600 gauss and it could be separated from background signals (3.4 and 6.2 MHz, and that signal was almost constant to room temperature. The equipment was used for sample testing. It gave systole/diastole data of 110/70 mmHg (on sphygmomanometer that was similar to 17/9 mV (on NMR signal. ABSTRAK Telah dikembangkan alat pemantauan tekanan darah berdasar prinsip NMR.

  17. Teaching NMR spectra analysis with nmr.cheminfo.org.

    Science.gov (United States)

    Patiny, Luc; Bolaños, Alejandro; Castillo, Andrés M; Bernal, Andrés; Wist, Julien

    2018-06-01

    Teaching spectra analysis and structure elucidation requires students to get trained on real problems. This involves solving exercises of increasing complexity and when necessary using computational tools. Although desktop software packages exist for this purpose, nmr.cheminfo.org platform offers students an online alternative. It provides a set of exercises and tools to help solving them. Only a small number of exercises are currently available, but contributors are invited to submit new ones and suggest new types of problems. Copyright © 2018 John Wiley & Sons, Ltd.

  18. Mapping of low flip angles in magnetic resonance

    International Nuclear Information System (INIS)

    Balezeau, Fabien; Saint-Jalmes, Herve; Eliat, Pierre-Antoine; Cayamo, Alejandro Bordelois

    2011-01-01

    Errors in the flip angle have to be corrected in many magnetic resonance imaging applications, especially for T1 quantification. However, the existing methods of B1 mapping fail to measure lower values of the flip angle despite the fact that these are extensively used in dynamic acquisition and 3D imaging. In this study, the nonlinearity of the radiofrequency (RF) transmit chain, especially for very low flip angles, is investigated and a simple method is proposed to accurately determine both the gain of the RF transmitter and the B1 field map for low flip angles. The method makes use of the spoiled gradient echo sequence with long repetition time (TR), such as applied in the double-angle method. It uses an image acquired with a flip angle of 90 0 as a reference image that is robust to B1 inhomogeneity. The ratio of the image at flip angle alpha to the image at a flip angle of 90 0 enables us to calculate the actual value of alpha. This study was carried out at 1.5 and 4.7 T, showing that the linearity of the RF supply system is highly dependent on the hardware. The method proposed here allows us to measure the flip angle from 1 0 to 60 0 with a maximal uncertainty of 10% and to correct T1 maps based on the variable flip angle method.

  19. Dynamic pulsed-field-gradient NMR

    CERN Document Server

    Sørland, Geir Humborstad

    2014-01-01

    Dealing with the basics, theory and applications of dynamic pulsed-field-gradient NMR NMR (PFG NMR), this book describes the essential theory behind diffusion in heterogeneous media that can be combined with NMR measurements to extract important information of the system being investigated. This information could be the surface to volume ratio, droplet size distribution in emulsions, brine profiles, fat content in food stuff, permeability/connectivity in porous materials and medical applications currently being developed. Besides theory and applications it will provide the readers with background knowledge on the experimental set-ups, and most important, deal with the pitfalls that are numerously present in work with PFG-NMR. How to analyze the NMR data and some important basic knowledge on the hardware will be explained, too.

  20. An Inversion Recovery NMR Kinetics Experiment

    OpenAIRE

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this article will enable instructors to use inversion recovery as a laboratory activity in applied NMR classes and provide research students with a conveni...

  1. Solid-state NMR studies of form I of atorvastatin calcium.

    Science.gov (United States)

    Wang, Wei David; Gao, Xudong; Strohmeier, Mark; Wang, Wei; Bai, Shi; Dybowski, Cecil

    2012-03-22

    Solid-state (13)C, (19)F, and (15)N magic angle spinning NMR studies of Form I of atorvastatin calcium are reported, including chemical shift tensors of all resolvable carbon sites and fluorine sites. The complete (13)C and (19)F chemical shift assignments are given based on an extensive analysis of (13)C-(1)H HETCOR and (13)C-(19)F HETCOR results. The solid-state NMR data indicate that the asymmetric unit of this material contains two atorvastatin molecules. A possible structure of Form I of atorvastatin calcium (ATC-I), derived from solid-state NMR data and density functional theory calculations of various structures, is proposed for this important active pharmaceutical ingredient (API).

  2. Discrimination of sugarcane according to cultivar by 1H NMR and chemometric analyses

    Energy Technology Data Exchange (ETDEWEB)

    Alves Filho, Elenilson G.; Silva, Lorena M.A.; Choze, Rafael; Liao, Luciano M. [Laboratorio de Ressonancia Magnetica Nuclear, Instituto de Quimica, Universidade Federal de Goias (UFG), Goiania, GO (Brazil); Honda, Neli K.; Alcantara, Glaucia B. [Departamento de Quimica, Universidade Federal de Mato Grosso do Sul (UFMS), Campo Grande, MS (Brazil)

    2012-07-01

    Several technologies for the development of new sugarcane cultivars have mainly focused on the increase in productivity and greater disease resistance. Sugarcane cultivars are usually identified by the organography of the leaves and stems, the analysis of peroxidase and esterase isoenzyme activities and the total soluble protein as well as soluble solid content. Nuclear magnetic resonance (NMR) associated with chemometric analysis has proven to be a valuable tool for cultivar assessment. Thus, this article describes the potential of chemometric analysis applied to 1H high resolution magic angle spinning (HRMAS) and NMR in solution for the investigation of sugarcane cultivars. For this purpose, leaves from eight different cultivars of sugarcane were investigated by {sup 1}H NMR spectroscopy in combination with chemometric analysis. The approach shows to be a useful tool for the distinction and classification of different sugarcane cultivars as well as to access the differences on its chemical composition. (author)

  3. NMR in structure-based drug design.

    Science.gov (United States)

    Carneiro, Marta G; Ab, Eiso; Theisgen, Stephan; Siegal, Gregg

    2017-11-08

    NMR spectroscopy is a powerful technique that can provide valuable structural information for drug discovery endeavors. Here, we discuss the strengths (and limitations) of NMR applications to structure-based drug discovery, highlighting the different levels of resolution and throughput obtainable. Additionally, the emerging field of paramagnetic NMR in drug discovery and recent developments in approaches to speed up and automate protein-observed NMR data collection and analysis are discussed. © 2017 The Author(s). Published by Portland Press Limited on behalf of the Biochemical Society.

  4. NMR spectroscopy using liquid crystal solvents

    CERN Document Server

    Emsley, JW

    2013-01-01

    NMR Spectroscopy using Liquid Crystal Solvents covers the importance of using a liquid crystal solvent in NMR to derive nuclear dipolar spin-spin coupling constants. This book is composed of ten chapters, and begins with a brief description of the features and benefits of liquid crystal in NMR spectroscopic analysis. The succeeding chapters deal with the mode of operation of nuclear spin Hamiltonian for partially oriented molecules and the analysis of NMR spectra of partially oriented molecules, as well as the determination of rigid molecule structure. These topics are followed by discussions

  5. Solution NMR structure determination of proteins revisited

    International Nuclear Information System (INIS)

    Billeter, Martin; Wagner, Gerhard; Wuethrich, Kurt

    2008-01-01

    This 'Perspective' bears on the present state of protein structure determination by NMR in solution. The focus is on a comparison of the infrastructure available for NMR structure determination when compared to protein crystal structure determination by X-ray diffraction. The main conclusion emerges that the unique potential of NMR to generate high resolution data also on dynamics, interactions and conformational equilibria has contributed to a lack of standard procedures for structure determination which would be readily amenable to improved efficiency by automation. To spark renewed discussion on the topic of NMR structure determination of proteins, procedural steps with high potential for improvement are identified

  6. NMR studies of isotopically labeled RNA

    Energy Technology Data Exchange (ETDEWEB)

    Pardi, A. [Univ. of Colorado, Boulder, CO (United States)

    1994-12-01

    In summary, the ability to generate NMR quantities of {sup 15}N and {sup 13}C-labeled RNAs has led to the development of heteronuclear multi-dimensional NMR techniques for simplifying the resonance assignment and structure determination of RNAs. These methods for synthesizing isotopically labeled RNAs are only several years old, and thus there are still relatively few applications of heteronuclear multi-dimensional NMR techniques to RNA. However, given the critical role that RNAs play in cellular function, one can expect to see an increasing number of NMR structural studies of biologically active RNAs.

  7. Ligand-receptor Interactions by NMR Spectroscopy

    Directory of Open Access Journals (Sweden)

    Novak. P.

    2008-04-01

    Full Text Available Today NMR spectroscopy is a method of choice for elucidation of interactions between biomolecules and the potential ligands. Knowledge on these interactions is an essential prerequisite for the rational drug design. The most important contribution of NMR to drug design a few years ago was the 3D structure determination of proteins. Besides delivering the 3D structures of the free proteins as a raw material for the modeling studies on ligand binding, NMR can directly yield valuable experimental data on the biologically important protein-ligand complexes. In addition to X-ray diffraction, NMR spectroscopy can provide information on the internal protein dynamics ordynamics of intermolecular interactions. Changes in NMR parameters allow us to detect ("SAR by NMR" and quantitatively determine binding affinities (titration, diffusion NMR experiments, etc. of potential ligands. Also, it is possible to determine the binding site and conformations of ligands, receptors and receptor-ligand complexes with the help of NMR methods such as tr-NOESY. Epitopes or functional groups responsible for binding of ligands to the receptor can be identified by employing STD or WaterLOGSY experiments. In this review are described some of the most frequent NMR methods for the characterization of the interactions between biomolecules and ligands, together with their advantages and disadvantages.

  8. NMR characterization of pituitary tumors

    International Nuclear Information System (INIS)

    Osbakken, M.; Gonzales, J.; Page, R.

    1984-01-01

    Twelve patients (5 male, 7 female, mean age 37.9 +- 20) with pituitary tumors were extensively evaluated with NMR imaging using a 1.5K gauss resistive magnet. Saturation recovery (SR), inversion recovery (IR) and spin echo (SE) pulse sequences were used for qualitative characterization of the lesions. T/sub 1/ calculations were also performed for brain and pituitary. Tumor histology and endocrine status were correlated with NMR data. All tumors were large with suprasellar extension (6 with prolactin secretion, 6 without). Pituitary T/sub 1/'s ranged from .2 to .64, the mean T/sub 1/ being longer than that of brain (Brain = .4 +- .04; Pit = .48 +- .14). 3 patients with histological evidence of homogeneous adenomas had long T/sub 1/'s (0.58 +- .05). 3 patients with evidence of recent or old hemorhage into the pituitary had much shorter T/sub 1/'s (0.29 +- .12). There was no relationship between prolactin secretion and T/sub 1/. Qualitative T/sub 1/ and T/sub 2/ information can be obtained by using a combination of SR, IR, and SE images. Using this method in the patients, homogeneous adenomas had similar T/sub 1/'s and longer T/sub 2/'s compared to the brain, while patients with bleeds had shorter T/sub 1/'s and T/sub 2/'s. Image T/sub 1/ characteristics correlated well with the calculated T/sub 1/ values. The range of T/sub 1/ (and potentially T/sub 2/) values which occur in apparently similar lesions are most likely due to anatomical and pathophysiological variations in these lesions. It may be ultimately possible to separate different types of pathological processes based on NMR image T/sub 1/ and T/sub 2/ characteristics after careful comparative studies of NMR and histological data are completed. The combination of calculated T/sub 1/ and T/sub 2/ with image T/sub 1/ and T/sub 2/ information may also be useful in further characterization of lesions

  9. Short recovery time NMR probe

    International Nuclear Information System (INIS)

    Ramia, M.E.; Martin, C.A.; Jeandrevin, S.

    2011-01-01

    A NMR probe for low frequency and short recovery time is presented in this work. The probe contains the tuning circuit, diode expanders and quarter wavelength networks to protect the receiver from both the amplifier noise and the coil ringing following the transmitter power pulse. It also possesses a coil damper which is activated by of non active components. The probe performance shows a recovery time of about of 15μs a sensitive Q factor reduction and an increase of the signal to noise ratio of about 68% during the reception at a work frequency of 2 MHz. (author)

  10. X-ray diffraction and NMR data for the study of the location of idebenone and idebenol in model membranes

    Directory of Open Access Journals (Sweden)

    Victoria Gómez-Murcia

    2016-06-01

    Full Text Available Here we present some of our data about the interaction of idebenone and idebenol with dipalmitoyl-phosphatidylcholine (DPPC. In particular, we include data of small angle X-ray diffraction (SAXD and wide angle X-ray diffraction experiments, obtention of electronic profiles of the membranes, 2H-NMR and 31P-NMR, as part of the research article: “Both idebenone and idebenol are localized near the lipid-water interface of the membrane and increase its fluidity” (Gomez-Murcia et al., 2016 [1]. These data were obtained from model membranes that included different proportions of idebenone and idebenol, at temperatures both above and below of the gel to fluid phase. The X-ray experiments were carried out by using a modified Kratky compact camera (MBraun-Graz-Optical Systems, Graz Austria, incorporating two coupled linear position sensitive detectors. The NMR data were collected from a a Bruker Avance 600 instrument.

  11. Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

    NARCIS (Netherlands)

    Van Der Schot, Gijs; Bonvin, Alexandre M J J

    We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on

  12. 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

  13. The double Brewster angle effect

    Science.gov (United States)

    Thirion-Lefevre, Laetitia; Guinvarc'h, Régis

    2018-01-01

    The Double Brewster angle effect (DBE) is an extension of the Brewster angle to double reflection on two orthogonal dielectric surfaces. It results from the combination of two pseudo-Brewster angles occurring in complementary incidence angles domains. It can be observed for a large range of incidence angles provided that double bounces mechanism is present. As a consequence of this effect, we show that the reflection coefficient at VV polarization can be at least 10 dB lower than the reflection coefficient at HH polarization over a wide range of incidence angle - typically from 20 to 70∘. It is experimentally demonstrated using a Synthetic Aperture Radar (SAR) image that this effect can be seen on buildings and forests. For large buildings, the difference can reach more than 20 dB. xml:lang="fr"

  14. Highly efficient F-19 heteronuclear decoupling in solid-state NMR spectroscopy using supercycled refocused-CW irradiation

    DEFF Research Database (Denmark)

    Equbal, Asif; Basse, Kristoffer; Nielsen, Niels Christian

    2016-01-01

    We present heteronuclear F-19 refocused CW (rCW) decoupling pulse sequences for solid-state magic-angle- spinning NMR applications. The decoupling sequences have been designed specifically to ensure suppression of the pertinent C-13-F-19 dipolar coupling interactions while simultaneously suppress...

  15. Dynamic-angle spinning and double rotation of quadrupolar nuclei

    International Nuclear Information System (INIS)

    Mueller, K.T.; California Univ., Berkeley, CA

    1991-07-01

    Nuclear magnetic resonance (NMR) spectroscopy of quadrupolar nuclei is complicated by the coupling of the electric quadrupole moment of the nucleus to local variations in the electric field. The quadrupolar interaction is a useful source of information about local molecular structure in solids, but it tends to broaden resonance lines causing crowding and overlap in NMR spectra. Magic- angle spinning, which is routinely used to produce high resolution spectra of spin-1/2 nuclei like carbon-13 and silicon-29, is incapable of fully narrowing resonances from quadrupolar nuclei when anisotropic second-order quadrupolar interactions are present. Two new sample-spinning techniques are introduced here that completely average the second-order quadrupolar coupling. Narrow resonance lines are obtained and individual resonances from distinct nuclear sites are identified. In dynamic-angle spinning (DAS) a rotor containing a powdered sample is reoriented between discrete angles with respect to high magnetic field. Evolution under anisotropic interactions at the different angles cancels, leaving only the isotropic evolution of the spin system. In the second technique, double rotation (DOR), a small rotor spins within a larger rotor so that the sample traces out a complicated trajectory in space. The relative orientation of the rotors and the orientation of the larger rotor within the magnetic field are selected to average both first- and second-order anisotropic broadening. The theory of quadrupolar interactions, coherent averaging theory, and motional narrowing by sample reorientation are reviewed with emphasis on the chemical shift anisotropy and second-order quadrupolar interactions experienced by half-odd integer spin quadrupolar nuclei. The DAS and DOR techniques are introduced and illustrated with application to common quadrupolar systems such as sodium-23 and oxygen-17 nuclei in solids

  16. Dynamic-angle spinning and double rotation of quadrupolar nuclei

    Energy Technology Data Exchange (ETDEWEB)

    Mueller, K.T. (Lawrence Berkeley Lab., CA (United States) California Univ., Berkeley, CA (United States). Dept. of Chemistry)

    1991-07-01

    Nuclear magnetic resonance (NMR) spectroscopy of quadrupolar nuclei is complicated by the coupling of the electric quadrupole moment of the nucleus to local variations in the electric field. The quadrupolar interaction is a useful source of information about local molecular structure in solids, but it tends to broaden resonance lines causing crowding and overlap in NMR spectra. Magic- angle spinning, which is routinely used to produce high resolution spectra of spin-{1/2} nuclei like carbon-13 and silicon-29, is incapable of fully narrowing resonances from quadrupolar nuclei when anisotropic second-order quadrupolar interactions are present. Two new sample-spinning techniques are introduced here that completely average the second-order quadrupolar coupling. Narrow resonance lines are obtained and individual resonances from distinct nuclear sites are identified. In dynamic-angle spinning (DAS) a rotor containing a powdered sample is reoriented between discrete angles with respect to high magnetic field. Evolution under anisotropic interactions at the different angles cancels, leaving only the isotropic evolution of the spin system. In the second technique, double rotation (DOR), a small rotor spins within a larger rotor so that the sample traces out a complicated trajectory in space. The relative orientation of the rotors and the orientation of the larger rotor within the magnetic field are selected to average both first- and second-order anisotropic broadening. The theory of quadrupolar interactions, coherent averaging theory, and motional narrowing by sample reorientation are reviewed with emphasis on the chemical shift anisotropy and second-order quadrupolar interactions experienced by half-odd integer spin quadrupolar nuclei. The DAS and DOR techniques are introduced and illustrated with application to common quadrupolar systems such as sodium-23 and oxygen-17 nuclei in solids.

  17. Angle Performance on Optima XE

    International Nuclear Information System (INIS)

    David, Jonathan; Satoh, Shu

    2011-01-01

    Angle control on high energy implanters is important due to shrinking device dimensions, and sensitivity to channeling at high beam energies. On Optima XE, beam-to-wafer angles are controlled in both the horizontal and vertical directions. In the horizontal direction, the beam angle is measured through a series of narrow slits, and any angle adjustment is made by steering the beam with the corrector magnet. In the vertical direction, the beam angle is measured through a high aspect ratio mask, and any angle adjustment is made by slightly tilting the wafer platen during implant.Using a sensitive channeling condition, we were able to quantify the angle repeatability of Optima XE. By quantifying the sheet resistance sensitivity to both horizontal and vertical angle variation, the total angle variation was calculated as 0.04 deg. (1σ). Implants were run over a five week period, with all of the wafers selected from a single boule, in order to control for any crystal cut variation.

  18. Small angle neutron scattering

    Directory of Open Access Journals (Sweden)

    Cousin Fabrice

    2015-01-01

    Full Text Available Small Angle Neutron Scattering (SANS is a technique that enables to probe the 3-D structure of materials on a typical size range lying from ∼ 1 nm up to ∼ a few 100 nm, the obtained information being statistically averaged on a sample whose volume is ∼ 1 cm3. This very rich technique enables to make a full structural characterization of a given object of nanometric dimensions (radius of gyration, shape, volume or mass, fractal dimension, specific area… through the determination of the form factor as well as the determination of the way objects are organized within in a continuous media, and therefore to describe interactions between them, through the determination of the structure factor. The specific properties of neutrons (possibility of tuning the scattering intensity by using the isotopic substitution, sensitivity to magnetism, negligible absorption, low energy of the incident neutrons make it particularly interesting in the fields of soft matter, biophysics, magnetic materials and metallurgy. In particular, the contrast variation methods allow to extract some informations that cannot be obtained by any other experimental techniques. This course is divided in two parts. The first one is devoted to the description of the principle of SANS: basics (formalism, coherent scattering/incoherent scattering, notion of elementary scatterer, form factor analysis (I(q→0, Guinier regime, intermediate regime, Porod regime, polydisperse system, structure factor analysis (2nd Virial coefficient, integral equations, characterization of aggregates, and contrast variation methods (how to create contrast in an homogeneous system, matching in ternary systems, extrapolation to zero concentration, Zero Averaged Contrast. It is illustrated by some representative examples. The second one describes the experimental aspects of SANS to guide user in its future experiments: description of SANS spectrometer, resolution of the spectrometer, optimization of

  19. 1H-NMR urinalysis

    International Nuclear Information System (INIS)

    Yamamoto, Hideaki; Yamaguchi, Shuichi

    1988-01-01

    In an effort to examine the usefulness of 1 H-nuclear magnetic resonance (NMR) urinalysis in the diagnosis of congenital metabolic disorders, 70 kinds of urinary metabolites were analysed in relation to the diagnosis of inborn errors of amino acid and organic acid disorders. Homogated decoupling (HMG) method failed to analyze six metabolites within the undetectable range. When non-decoupling method (NON), in which the materials are dissolved in dimethyl sulfoxide, was used, the identification of signals became possible. The combination of HMG and NON methods was, therefore, considered to identify all of the metabolites. When the urine samples, which were obtained from patients with hyperglycerolemia, hyperornithinemia, glutaric acidemia type II, or glycerol kinase deficiency, were analysed by using both HMG and NON methods, abnormally increased urinary metabolites were detected. 1 H-NMR urinalysis, if used in the combination of HMG and NON methods, may allow simultanenous screening of inborn errors of metabolism of amino acid and organic acid disorders. (Namekawa, K.)

  20. Structure determination of cyclo pentane terpene derivatives by crossed NMR and MS techniques

    Energy Technology Data Exchange (ETDEWEB)

    Pianet, I.; Bourgeois, G. [Bordeaux-1 Univ., 33 - Talence (France); Dolatkhani, M.; Cramail, H.; Deffieux, A. [Centre National de la Recherche Scientifique (CNRS), 33 - Talence (France)

    1995-10-01

    3 of the 4 stereoisomers of the 1-isopropenyl 2,3-dimethylcyclopentane, obtained from the cracking of 3,7-dimethylocta-1,6-diene, were purified and characterized. Dihedral angles, between the protons of the substituted carbons, have been determined by molecular modelling. Analysis of the NMR and mass spectra allowed us to access to the structure of the different isomers. (authors). 6 refs., 2 tabs.

  1. Automated analysis of angle closure from anterior chamber angle images.

    Science.gov (United States)

    Baskaran, Mani; Cheng, Jun; Perera, Shamira A; Tun, Tin A; Liu, Jiang; Aung, Tin

    2014-10-21

    To evaluate a novel software capable of automatically grading angle closure on EyeCam angle images in comparison with manual grading of images, with gonioscopy as the reference standard. In this hospital-based, prospective study, subjects underwent gonioscopy by a single observer, and EyeCam imaging by a different operator. The anterior chamber angle in a quadrant was classified as closed if the posterior trabecular meshwork could not be seen. An eye was classified as having angle closure if there were two or more quadrants of closure. Automated grading of the angle images was performed using customized software. Agreement between the methods was ascertained by κ statistic and comparison of area under receiver operating characteristic curves (AUC). One hundred forty subjects (140 eyes) were included, most of whom were Chinese (102/140, 72.9%) and women (72/140, 51.5%). Angle closure was detected in 61 eyes (43.6%) with gonioscopy in comparison with 59 eyes (42.1%, P = 0.73) using manual grading, and 67 eyes (47.9%, P = 0.24) with automated grading of EyeCam images. The agreement for angle closure diagnosis between gonioscopy and both manual (κ = 0.88; 95% confidence interval [CI), 0.81-0.96) and automated grading of EyeCam images was good (κ = 0.74; 95% CI, 0.63-0.85). The AUC for detecting eyes with gonioscopic angle closure was comparable for manual and automated grading (AUC 0.974 vs. 0.954, P = 0.31) of EyeCam images. Customized software for automated grading of EyeCam angle images was found to have good agreement with gonioscopy. Human observation of the EyeCam images may still be needed to avoid gross misclassification, especially in eyes with extensive angle closure. Copyright 2014 The Association for Research in Vision and Ophthalmology, Inc.

  2. 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.

  3. NMR Evidence for the Topologically Nontrivial Nature in a Family of Half-Heusler Compounds

    KAUST Repository

    Zhang, Xiaoming

    2016-03-16

    Spin-orbit coupling (SOC) is expected to partly determine the topologically nontrivial electronic structure of heavy half-Heusler ternary compounds. However, to date, attempts to experimentally observe either the strength of SOC or how it modifies the bulk band structure have been unsuccessful. By using bulk-sensitive nuclear magnetic resonance (NMR) spectroscopy combined with first-principles calculations, we reveal that 209Bi NMR isotropic shifts scale with relativity in terms of the strength of SOC and average atomic numbers, indicating strong relativistic effects on NMR parameters. According to first-principles calculations, we further claim that nuclear magnetic shieldings from relativistic p1/2 states and paramagnetic contributions from low-lying unoccupied p3/2 states are both sensitive to the details of band structures tuned by relativity, which explains why the hidden relativistic effects on band structure can be revealed by 209Bi NMR isotropic shifts in topologically nontrivial half-Heusler compounds. Used in complement to surface-sensitive methods, such as angle resolved photon electron spectroscopy and scanning tunneling spectroscopy, NMR can provide valuable information on bulk electronic states.

  4. NMR Evidence for the Topologically Nontrivial Nature in a Family of Half-Heusler Compounds

    KAUST Repository

    Zhang, Xiaoming; Hou, Zhipeng; Wang, Yue; Xu, Guizhou; Shi, Chenglong; Liu, EnKe; Xi, Xuekui; Wang, Wenhong; Wu, Guangheng; Zhang, Xixiang

    2016-01-01

    Spin-orbit coupling (SOC) is expected to partly determine the topologically nontrivial electronic structure of heavy half-Heusler ternary compounds. However, to date, attempts to experimentally observe either the strength of SOC or how it modifies the bulk band structure have been unsuccessful. By using bulk-sensitive nuclear magnetic resonance (NMR) spectroscopy combined with first-principles calculations, we reveal that 209Bi NMR isotropic shifts scale with relativity in terms of the strength of SOC and average atomic numbers, indicating strong relativistic effects on NMR parameters. According to first-principles calculations, we further claim that nuclear magnetic shieldings from relativistic p1/2 states and paramagnetic contributions from low-lying unoccupied p3/2 states are both sensitive to the details of band structures tuned by relativity, which explains why the hidden relativistic effects on band structure can be revealed by 209Bi NMR isotropic shifts in topologically nontrivial half-Heusler compounds. Used in complement to surface-sensitive methods, such as angle resolved photon electron spectroscopy and scanning tunneling spectroscopy, NMR can provide valuable information on bulk electronic states.

  5. Early history of NMR at Los Alamos

    International Nuclear Information System (INIS)

    Jackson, J.A.

    1985-11-01

    Nuclear magnetic resonance (NMR) spectroscopy has developed into an important research tool in chemistry. More recently, NMR imaging and in vivo spectroscopy promise to produce a revolution in medicine and biochemistry. Early experiments at Los Alamos led to DOE programs involving stable isotopes of importance to biology and to medicine. These events are briefly recounted. 2 refs

  6. Characterization of natural bentonite by NMR

    International Nuclear Information System (INIS)

    Leite, Sidnei Q.M.; Dieguez, Lidia C.; Menezes, Sonia M.C.; San Gil, Rosane A.S.

    1993-01-01

    Solid state NMR as well as several other instrumental chemical analysis techniques were used in order to characterize two natural occurring bentonite. The methodology is described. The NMR spectra, together with the other used techniques suggest that the observed differences are due to iron inclusions in tetrahedral and octahedral sites

  7. Using Cloud Storage for NMR Data Distribution

    Science.gov (United States)

    Soulsby, David

    2012-01-01

    An approach using Google Groups as method for distributing student-acquired NMR data has been implemented. We describe how to configure NMR spectrometer software so that data is uploaded to a laboratory section specific Google Group, thereby removing bottlenecks associated with printing and processing at the spectrometer workstation. Outside of…

  8. NMR studies of the structure of glasses

    International Nuclear Information System (INIS)

    Bray, P.J.; Gravina, S.J.; Stallworth, P.E.; Szu, S.P.; Jianhui Zhong

    1988-01-01

    Earlier continuous wave (CW) NMR studies of chemical bonding and structure in glasses are summarized. Examples are given of this use of the quadrupolar interaction and chemical shift to obtain structural information. New NMR data and analyses are presented for alkali borate and gallate glasses. Extensions to other elements (e.g. molybdenum, lanthanum) are suggested. 44 refs. (author)

  9. An Inversion Recovery NMR Kinetics Experiment

    Science.gov (United States)

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this…

  10. Selective sensitivity enhancement in FT-NMR

    International Nuclear Information System (INIS)

    Farrar, T.C.

    1987-01-01

    In this article the basic two-spin nuclear magnetic resonance (NMR) experiment and the new sensitivity enhancement experiments are reviewed. In part two of this two-part series an overview of two-dimensional NMR experiments will be presented. Part two will appear in the June 1 issue of Analytical Chemistry

  11. 2D NMR studies of biomolecules

    International Nuclear Information System (INIS)

    Lamerichs, R.M.J.N.

    1989-01-01

    The work described in this thesis comprises two related subjects. The first part describes methods to derive high-resolution structures of proteins in solution using two-dimensional (2-D) NMR. The second part describes 2-D NMR studies on the interaction between proteins and DNA. (author). 261 refs.; 52 figs.; 23 tabs

  12. Synthesis and NMR Elucidation of Novel Pentacycloundecane ...

    African Journals Online (AJOL)

    Herein we report the synthesis and NMR elucidation of five novel pentacycloundecane (PCU)-derived short peptides as potential HIV protease inhibitors. 1H and 13C spectral analysis show major overlapping of methine resonance of the PCU 'cage' thereby making it extremely difficult to assign the NMR signals. Attachment ...

  13. Development and applications of quantitative NMR spectroscopy

    International Nuclear Information System (INIS)

    Yamazaki, Taichi

    2016-01-01

    Recently, quantitative NMR spectroscopy has attracted attention as an analytical method which can easily secure traceability to SI unit system, and discussions about its accuracy and inaccuracy are also started. This paper focuses on the literatures on the advancement of quantitative NMR spectroscopy reported between 2009 and 2016, and introduces both NMR measurement conditions and actual analysis cases in quantitative NMR. The quantitative NMR spectroscopy using an internal reference method enables accurate quantitative analysis with a quick and versatile way in general, and it is possible to obtain the precision sufficiently applicable to the evaluation of pure substances and standard solutions. Since the external reference method can easily prevent contamination to samples and the collection of samples, there are many reported cases related to the quantitative analysis of biologically related samples and highly scarce natural products in which NMR spectra are complicated. In the precision of quantitative NMR spectroscopy, the internal reference method is superior. As the quantitative NMR spectroscopy widely spreads, discussions are also progressing on how to utilize this analytical method as the official methods in various countries around the world. In Japan, this method is listed in the Pharmacopoeia and Japanese Standard of Food Additives, and it is also used as the official method for purity evaluation. In the future, this method will be expected to spread as the general-purpose analysis method that can ensure traceability to SI unit system. (A.O.)

  14. NMR imaging of soft tissue tumors

    International Nuclear Information System (INIS)

    Laval-Jeantet, M.; Tobolsk, F.; Delepine, N.; Delepine, G.; Roger, B.; Cabanis, E.A.

    1986-01-01

    Preliminary findings on NMR imaging of 30 soft tissue tumors demonstrated the indispensable value of this examination (particularly when a surface antenna is used) for preoperative investigation and diagnosis of tumoral recurrence when compared with other radiologic techniques. The possible potential of NMR imaging for characterization of tissues, apart from lipoma or liposarcoma, cannot be evaluated at the present time [fr

  15. Carbon-13 NMR spectroscopy of biological systems

    CERN Document Server

    Beckmann, Nicolau

    1995-01-01

    This book is intended to provide an in-depth understanding of 13C NMR as a tool in biological research. 13C NMR has provided unique information concerning complex biological systems, from proteins and nucleic acids to animals and humans. The subjects addressed include multidimensional heteronuclear techniques for structural studies of molecules in the liquid and solid states, the investigation of interactions in model membranes, the elucidation of metabolic pathwaysin vitro and in vivo on animals, and noninvasive metabolic studies performed on humans. The book is a unique mix of NMR methods and biological applications which makes it a convenient reference for those interested in research in this interdisciplinary area of physics, chemistry, biology, and medicine.Key Features* An interdisciplinary text with emphasis on both 13C NMR methodology and the relevant biological and biomedical issues* State-of-the-art 13C NMR techniques are described; Whenever possible, their advantages over other approaches are empha...

  16. Measurement of the angle gamma

    International Nuclear Information System (INIS)

    Aleksan, R.; Sphicas, P.; Massachusetts Inst. of Tech., Cambridge, MA

    1993-12-01

    The angle γ as defined in the Wolfenstein approximation is not completely out of reach of current or proposed dedicated B experiments. This work represents but a first step in the direction of extracting the third angle of the unitarity triangle by study the feasibility of using new decay modes in a hadronic machine. (A.B.). 11 refs., 1 fig., 7 tabs

  17. Nucleation of small angle boundaries

    CSIR Research Space (South Africa)

    Nabarro, FRN

    1996-12-01

    Full Text Available The internal stresses induced by the strain gradients in an array of lattice cells delineated by low-angle dislocation boundaries are partially relieved by the creation of new low-angle boundaries. This is shown to be a first-order transition...

  18. Acquisition of Infrared Variable Angle Spectroscopic Ellipsometer (IR-VASE)

    Science.gov (United States)

    2016-04-22

    biomaterials , and nanocomposites. Based on this base user group it is estimated that...Engineering; and Barbara Calcagno, Department of General Engineering) 5. The Role of Mechanical Stimulus on Collagen Expression During Bone Repair (Paul...Polymeric Biomaterials Laboratory Principal Investigator: Jorge Almodóvar, PhD - The IR spectra

  19. 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.

  20. Solid-state {sup 2}H NMR investigations in guest-host systems and plastic crystals

    Energy Technology Data Exchange (ETDEWEB)

    Garibay, J.A.V.

    2004-07-01

    Variable temperature {sup 2}H NMR investigations have been carried out to study the molecular behavior of perdeuterated benzene and pyridine in the inclusion compound with tris-(1,2-dioxyphenyl)-cyclotriphosphazene. Here, a comprehensive variable temperature {sup 2}H NMR study is presented comprising line shape studies and relaxation experiments. The experimental data clearly indicate the presence of highly mobile guest species. Sample cooling gives rise to characteristic line shape effects that can be attributed to a slow-down of the rotational motion. Additional {sup 2}H NMR measurements were performed on the plastic crystal 1,4-diazabicyclo[2,2,2]octane where highly mobile species were observed. A quantitative analysis of the experimental data is achieved by appropriate computer simulations taking into account various molecular motions for each studied system. The analysis of these theoretical data give rise to the kinetic parameters that are in the order of related systems. (orig.)

  1. Systematic comparison of crystal and NMR protein structures deposited in the protein data bank.

    Science.gov (United States)

    Sikic, Kresimir; Tomic, Sanja; Carugo, Oliviero

    2010-09-03

    Nearly all the macromolecular three-dimensional structures deposited in Protein Data Bank were determined by either crystallographic (X-ray) or Nuclear Magnetic Resonance (NMR) spectroscopic methods. This paper reports a systematic comparison of the crystallographic and NMR results deposited in the files of the Protein Data Bank, in order to find out to which extent these information can be aggregated in bioinformatics. A non-redundant data set containing 109 NMR - X-ray structure pairs of nearly identical proteins was derived from the Protein Data Bank. A series of comparisons were performed by focusing the attention towards both global features and local details. It was observed that: (1) the RMDS values between NMR and crystal structures range from about 1.5 Å to about 2.5 Å; (2) the correlation between conformational deviations and residue type reveals that hydrophobic amino acids are more similar in crystal and NMR structures than hydrophilic amino acids; (3) the correlation between solvent accessibility of the residues and their conformational variability in solid state and in solution is relatively modest (correlation coefficient = 0.462); (4) beta strands on average match better between NMR and crystal structures than helices and loops; (5) conformational differences between loops are independent of crystal packing interactions in the solid state; (6) very seldom, side chains buried in the protein interior are observed to adopt different orientations in the solid state and in solution.

  2. Proton Environments in Biomimetic Calcium Phosphates Formed from Mesoporous Bioactive CaO-SiO2-P2O5 Glasses in Vitro: Insights from Solid-State NMR.

    Science.gov (United States)

    Mathew, Renny; Turdean-Ionescu, Claudia; Yu, Yang; Stevensson, Baltzar; Izquierdo-Barba, Isabel; García, Ana; Arcos, Daniel; Vallet-Regí, María; Edén, Mattias

    2017-06-22

    When exposed to body fluids, mesoporous bioactive glasses (MBGs) of the CaO-SiO 2 -P 2 O 5 system develop a bone-bonding surface layer that initially consists of amorphous calcium phosphate (ACP), which transforms into hydroxy-carbonate apatite (HCA) with a very similar composition as bone/dentin mineral. Information from various 1 H-based solid-state nuclear magnetic resonance (NMR) experiments was combined to elucidate the evolution of the proton speciations both at the MBG surface and within each ACP/HCA constituent of the biomimetic phosphate layer formed when each of three MBGs with distinct Ca, Si, and P contents was immersed in a simulated body fluid (SBF) for variable periods between 15 min and 30 days. Directly excited magic-angle-spinning (MAS) 1 H NMR spectra mainly reflect the MBG component, whose surface is rich in water and silanol (SiOH) moieties. Double-quantum-single-quantum correlation 1 H NMR experimentation at fast MAS revealed their interatomic proximities. The comparatively minor H species of each ACP and HCA component were probed selectively by heteronuclear 1 H- 31 P NMR experimentation. The initially prevailing ACP phase comprises H 2 O and "nonapatitic" HPO 4 2- /PO 4 3- groups, whereas for prolonged MBG soaking over days, a well-progressed ACP → HCA transformation was evidenced by a dominating O 1 H resonance from HCA. We show that 1 H-detected 1 H → 31 P cross-polarization NMR is markedly more sensitive than utilizing powder X-ray diffraction or 31 P NMR for detecting the onset of HCA formation, notably so for P-bearing (M)BGs. In relation to the long-standing controversy as to whether bone mineral comprises ACP and/or forms via an ACP precursor, we discuss a recently accepted structural core-shell picture of both synthetic and biological HCA, highlighting the close relationship between the disordered surface layer and ACP.

  3. Relationship between the Angle of Repose and Angle of Internal ...

    African Journals Online (AJOL)

    ). The angle of internal friction ... compression chambers. Lorenzen, 1957 (quoted by Mohsenin,. 1986), reported that the design of deep ... tiongiven for lateral pressure in deep bins as presented by Mohsenin. (1986). The presence of moisture ...

  4. The 1H NMR profile of healthy dog cerebrospinal fluid.

    Directory of Open Access Journals (Sweden)

    Mihai Musteata

    Full Text Available The availability of data for reference values in cerebrospinal fluid for healthy humans is limited due to obvious practical and ethical issues. The variability of reported values for metabolites in human cerebrospinal fluid is quite large. Dogs present great similarities with humans, including in cases of central nervous system pathologies. The paper presents the first study on healthy dog cerebrospinal fluid metabolomic profile using (1H NMR spectroscopy. A number of 13 metabolites have been identified and quantified from cerebrospinal fluid collected from a group of 10 mix breed healthy dogs. The biological variability as resulting from the relative standard deviation of the physiological concentrations of the identified metabolites had a mean of 18.20% (range between 9.3% and 44.8%. The reported concentrations for metabolites may be used as normal reference values. The homogeneity of the obtained results and the low biologic variability show that the (1H NMR analysis of the dog's cerebrospinal fluid is reliable in designing and interpreting clinical and therapeutic trials in dogs with central nervous system pathologies.

  5. 13C CPMAS NMR Studies of Anthocyanidins and their Glucosides

    International Nuclear Information System (INIS)

    Wolniak, M.; Wawer, I.

    2005-01-01

    Anthocyanins are responsible for red, purple or blue colours of flower petals and can be found in red or black fruits and berries. Many foods, especially red grapes and wines, aronia or blueberries contain large amounts of anthocyanins. Their health beneficial effects are related to antioxidant and radical scavenging properties. Structural analysis of anthocyanins by NMR are few, owing to the difficulty in obtaining analysable spectra for unstable, interconverting compounds, available in small amounts. Compounds studied by us were isolated from fruits and berries. 13 C CPMAS NMR spectra were recorded on a Bruker DSX-400 spectrometer for solid chlorides of: cyanidin, cyanidin 3-O-glucoside, cyanidin 3,5-O-diglucoside, pelargonidin and pelargonidin 3-O-glucoside. Dipolar dephased and short contact pulse sequences were used as an aid in the assignment of resonances in CPMAS spectra of solids. Inspection of the spectra indicates that anthocyanidins are in the form of flavylium (cationic) and not in form of the chalcone.: the resonance of C2 appears at ca. 160 ppm and C3 at ca. 135 ppm, whereas C ring opening produces C2 = O, for which chemical shift of ca. 180 ppm can be expected. A comparison of experimental (CPMAS) and predicted (GIAO DFT) shielding constants for cyanidin provided information about the orientation of OH groups, twist angle of aromatic ring B and the localization of the chloride anion.(author)

  6. 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

  7. Mapping protein–protein interactions by double-REDOR-filtered magic angle spinning NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Changmiao; Hou, Guangjin, E-mail: hou@udel.edu; Lu, Xingyu; Polenova, Tatyana, E-mail: tpolenov@udel.edu [University of Delaware, Department of Chemistry and Biochemistry (United States)

    2017-02-15

    REDOR-based experiments with simultaneous {sup 1}H–{sup 13}C and {sup 1}H−{sup 15}N dipolar dephasing are explored for investigating intermolecular protein–protein interfaces in complexes formed by a U–{sup 13}C,{sup 15}N-labeled protein and its natural abundance binding partner. The application of a double-REDOR filter (dREDOR) results in a complete dephasing of proton magnetization in the U–{sup 13}C,{sup 15}N-enriched molecule while the proton magnetization of the unlabeled binding partner is not dephased. This retained proton magnetization is then transferred across the intermolecular interface by {sup 1}H–{sup 13}C or {sup 1}H–{sup 15}N cross polarization, permitting to establish the residues of the U–{sup 13}C,{sup 15}N-labeled protein, which constitute the binding interface. To assign the interface residues, this dREDOR-CPMAS element is incorporated as a building block into {sup 13}C–{sup 13}C correlation experiments. We established the validity of this approach on U–{sup 13}C,{sup 15}N-histidine and on a structurally characterized complex of dynactin’s U–{sup 13}C,{sup 15}N-CAP-Gly domain with end-binding protein 1 (EB1). The approach introduced here is broadly applicable to the analysis of intermolecular interfaces when one of the binding partners in a complex cannot be isotopically labeled.

  8. Pf1 bacteriophage hydration by magic angle spinning solid-state NMR

    Energy Technology Data Exchange (ETDEWEB)

    Sergeyev, Ivan V.; Bahri, Salima; McDermott, Ann E., E-mail: aem5@columbia.edu [Department of Chemistry, Columbia University, 3000 Broadway, New York, New York 10027 (United States); Day, Loren A. [Public Health Research Institute, Rutgers University, 225 Warren St., Newark, New Jersey 07103 (United States)

    2014-12-14

    High resolution two- and three-dimensional heteronuclear correlation spectroscopy ({sup 1}H–{sup 13}C, {sup 1}H–{sup 15}N, and {sup 1}H–{sup 13}C–{sup 13}C HETCOR) has provided a detailed characterization of the internal and external hydration water of the Pf1 virion. This long and slender virion (2000 nm × 7 nm) contains highly stretched DNA within a capsid of small protein subunits, each only 46 amino acid residues. HETCOR cross-peaks have been unambiguously assigned to 25 amino acids, including most external residues 1–21 as well as residues 39–40 and 43–46 deep inside the virion. In addition, the deoxyribose rings of the DNA near the virion axis are in contact with water. The sets of cross-peaks to the DNA and to all 25 amino acid residues were from the same hydration water {sup 1}H resonance; some of the assigned residues do not have exchangeable side-chain protons. A mapping of the contacts onto structural models indicates the presence of water “tunnels” through a highly hydrophobic region of the capsid. The present results significantly extend and modify results from a lower resolution study, and yield a comprehensive hydration surface map of Pf1. In addition, the internal water could be distinguished from external hydration water by means of paramagnetic relaxation enhancement. The internal water population may serve as a conveniently localized magnetization reservoir for structural studies.

  9. Ring magnet firing angle control

    International Nuclear Information System (INIS)

    Knott, M.J.; Lewis, L.G.; Rabe, H.H.

    1975-01-01

    A device is provided for controlling the firing angles of thyratrons (rectifiers) in a ring magnet power supply. A phase lock loop develops a smooth ac signal of frequency equal to and in phase with the frequency of the voltage wave developed by the main generator of the power supply. A counter that counts from zero to a particular number each cycle of the main generator voltage wave is synchronized with the smooth AC signal of the phase lock loop. Gates compare the number in the counter with predetermined desired firing angles for each thyratron and with coincidence the proper thyratron is fired at the predetermined firing angle

  10. NMR imaging of the brain: initial impressions

    International Nuclear Information System (INIS)

    Spencer, D.H.; Bydder, G.M.

    1983-01-01

    An NMR imaging system designed and built by Thorn-EMI Ltd was installed at Hammersmith Hospital in March 1981. In the first year of operation 180 patients and 40 volunteers have had cranial examinations and initial impressions bases on this experience are presented. Patients with a wide variety of neurological diseases have been studied to provide a basis for diagnostic interpretation, to define distinctive features, and to evaluate different types of scanning sequences. NMR imaging appears to be of considerable value in neurological diagnosis and has a number of advantages over CT. The detailed evaluation of NMR imaging will require much more work but the initial results are very promising

  11. Oriented solid-state NMR spectrosocpy

    DEFF Research Database (Denmark)

    Bertelsen, Kresten

    This thesis is concerned with driving forward oriented solid-state NMR spectroscopy as a viable technique for studying peptides in membrane bilayers. I will show that structural heterogeneity is an intrinsic part of the peptide/lipid system and that NMR can be used to characterize static...... and dynamic structural features of the peptides and its local surroundings. In fact one need to take into account the dynamical features of the system in order to correctly predict the structure from oriented solid-state NMR spectra.      ...

  12. NMR reaction monitoring in flow synthesis

    Directory of Open Access Journals (Sweden)

    M. Victoria Gomez

    2017-02-01

    Full Text Available Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed.

  13. NMR reaction monitoring in flow synthesis.

    Science.gov (United States)

    Gomez, M Victoria; de la Hoz, Antonio

    2017-01-01

    Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed.

  14. 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

  15. 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.))

  16. Graphical programming for pulse automated NMR experiments

    International Nuclear Information System (INIS)

    Belmonte, S.B.; Oliveira, I.S.; Guimaraes, A.P.

    1999-01-01

    We describe a software program designed to control a broadband pulse Nuclear Magnetic Resonance (NMR) spectrometer used in zero-field NMR studies of magnetic metals. The software is written in the graphical language LabVIEW. This type of programming allows modifications and the inclusion of new routines to be easily made by the non-specialist, without changing the basic structure of the program. The program corrects for differences in the gain of the two acquisition channels [U (phase) and V (quadrature)], and automatic baseline subtraction. We present examples of measurements of NMR spectra, spin-echo decay (T 2 ), and quadrupolar oscillations, performed in magnetic intermetallic compounds. (author)

  17. The characterisation of polymers using pulsed NMR

    International Nuclear Information System (INIS)

    Charlesby, A.

    1983-01-01

    Broad line pulsed NMR is applied to obtain information on radiation-induced polymer changes and other aspects of polymer science based on the interpretation of spin-spin relaxation curves. Calculations are made to determine the molecular weight, the crosslink density of simple, low molecular weight, flexible polymers. For higher molecular weight polymers, a conclusion can be drawn on the concentrations of entangled and crosslinked units by means of pulsed NMR. Some typical applications of the technique are illustrated by the examples of polyethylenes, rubbers, filled polymeric systems and aqueous polyethylene oxide solutions. The morphology of polymers can be followed by pulsed NMR. (V.N.)

  18. Solid state NMR, basic theory and recent progress for quadrupole nuclei with half-integer spin

    International Nuclear Information System (INIS)

    Dieter, F.

    1998-01-01

    This review describes the basic theory and some recently developed techniques for the study of quadrupole nuclei with half integer spins in powder materials. The latter is connected to the introduction of the double rotation (DOR) by A. Samoson et al. (1) and to the introduction of the multiple quantum magic-angle spinning (MQ MAS) technique by L. Frydman et. al. (2). For integer spins, especially the solid-state deuterium magnetic resonance, we refer to the review of G.L. Hoatson and R.L. Vold: '' 2 H-NMR Spectroscopy of Solids and Liquid Crystals'' (3). For single crystals we refer to O. Kanert and M. Mehring: ''Static quadrupole effects in disordered cubic solids''(4) and we would like also to mention the ''classic'' review of M.H. Cohen and F. Reif: ''Quadrupole effects in NMR studies of solids'' (5). Some more recent reviews in the field under study are D. Freude and J. Haase ''Quadrupole effects in solid-state NMR'' (6). Ch. Jager: ''Satellite Transition Spectroscopy of Quadrupolar Nuclei'' (7) and B.F. Chmelka and J.W. Zwanziger: ''Solid State NMR Line Narrowing Methods for Quadrupolar Nuclei - Double Rotation and Dynamic-Angle Spinning'' (8). A survey of nuclear quadrupole frequency data published before the end of 1982 is given by H. Chihara and N. Nakamura in Landolt-Bornstein, Vol. 20 (9). Values of the chemical shift of quadrupole nuclei in solids can be found in books such as ''Multinuclear NMR'' edited by J. Mason (10). In section 9 of ref (6) some electric field gradient and chemical shift data published from 1983 to 1992 for the most studied quadrupole nuclei sup 27 Al, sup 23 Na, and sup 17 O are given

  19. NMR measurement of dynamic nuclear polarization: a technique to test the quality of its volume average obtained with different NMR coil configurations

    International Nuclear Information System (INIS)

    Zhao, W.H.; Cox, S.F.J.

    1980-07-01

    In the NMR measurement of dynamic nuclear polarization, a volume average is obtained where the contribution from different parts of the sample is weighted according to the local intensity of the RF field component perpendicular to the large static field. A method of mapping this quantity is described. A small metallic object whose geometry is chosen to perturb the appropriate RF component is scanned through the region to be occupied by the sample. The response of the phase angle of the impedance of a tuned circuit comprising the NMR coil gives a direct measurement of the local weighting factor. The correlation between theory and experiment was obtained by using a circular coil. The measuring method, checked in this way, was then used to investigate the field profiles of practical coils which are required to be rectangular for a proposed experimental neutron polarizing filter. This method can be used to evaluate other practical RF coils. (author)

  20. Two Comments on Bond Angles

    Science.gov (United States)

    Glaister, P.

    1997-09-01

    Tetrahedral Bond Angle from Elementary Trigonometry The alternative approach of using the scalar (or dot) product of vectors enables the determination of the bond angle in a tetrahedral molecule in a simple way. There is, of course, an even more straightforward derivation suitable for students who are unfamiliar with vectors, or products thereof, but who do know some elementary trigonometry. The starting point is the figure showing triangle OAB. The point O is the center of a cube, and A and B are at opposite corners of a face of that cube in which fits a regular tetrahedron. The required bond angle alpha = AÔB; and using Pythagoras' theorem, AB = 2(square root 2) is the diagonal of a face of the cube. Hence from right-angled triangle OEB, tan(alpha/2) = (square root 2) and therefore alpha = 2tan-1(square root 2) is approx. 109° 28' (see Fig. 1).

  1. NMR Determination of Hydrogen Bond Thermodynamics in a Simple Diamide: A Physical Chemistry Experiment

    Science.gov (United States)

    Morton, Janine G.; Joe, Candice L.; Stolla, Massiel C.; Koshland, Sophia R.; Londergan, Casey H.; Schofield, Mark H.

    2015-01-01

    Variable temperature NMR spectroscopy is used to determine the ?H° and ?S° of hydrogen bond formation in a simple diamide. In this two- or three-day experiment, students synthesize N,N'-dimethylmalonamide, dimethylsuccinamide, dimethylglutaramide, or dimethyladipamide from methylamine and the corresponding diester (typically in 50% recrystallized…

  2. NMR data-driven structure determination using NMR-I-TASSER in the CASD-NMR experiment

    Energy Technology Data Exchange (ETDEWEB)

    Jang, Richard [Huazhong University of Science and Technology, School of Software Engineering (China); Wang, Yan [Huazhong University of Science and Technology, School of Life Science and Technology (China); Xue, Zhidong, E-mail: zdxue@hust.edu.cn [Huazhong University of Science and Technology, School of Software Engineering (China); Zhang, Yang, E-mail: zhng@umich.edu [University of Michigan, Department of Computational Medicine and Bioinformatics (United States)

    2015-08-15

    NMR-I-TASSER, an adaption of the I-TASSER algorithm combining NMR data for protein structure determination, recently joined the second round of the CASD-NMR experiment. Unlike many molecular dynamics-based methods, NMR-I-TASSER takes a molecular replacement-like approach to the problem by first threading the target through the PDB to identify structural templates which are then used for iterative NOE assignments and fragment structure assembly refinements. The employment of multiple templates allows NMR-I-TASSER to sample different topologies while convergence to a single structure is not required. Retroactive and blind tests of the CASD-NMR targets from Rounds 1 and 2 demonstrate that even without using NOE peak lists I-TASSER can generate correct structure topology with 15 of 20 targets having a TM-score above 0.5. With the addition of NOE-based distance restraints, NMR-I-TASSER significantly improved the I-TASSER models with all models having the TM-score above 0.5. The average RMSD was reduced from 5.29 to 2.14 Å in Round 1 and 3.18 to 1.71 Å in Round 2. There is no obvious difference in the modeling results with using raw and refined peak lists, indicating robustness of the pipeline to the NOE assignment errors. Overall, despite the low-resolution modeling the current NMR-I-TASSER pipeline provides a coarse-grained structure folding approach complementary to traditional molecular dynamics simulations, which can produce fast near-native frameworks for atomic-level structural refinement.

  3. NMR mechanisms in gel dosimetry

    International Nuclear Information System (INIS)

    Schreiner, L J

    2009-01-01

    Nuclear magnetic resonance was critical to the development of gel dosimetry, as it established the potential for three dimensional dosimetry with chemical dosimeter systems through magnetic resonance imaging [1]. In the last two decades MRI has served as the gold standard for imaging, while NMR relaxometry has played an important role in the development and understanding of the behaviour of new gel dosimetry systems. Therefore, an appreciation of the relaxation mechanisms determining the NMR behaviour of irradiated gel dosimeters is important for a full comprehension of a considerable component of the literature on gel dosimetry. A number of excellent papers have presented this important theory, this brief review will highlight some of the salient points made previously [1-5]. The spin relaxation of gel dosimeters (which determines the dose dependence in most conventional MR imaging) is determined principally by the protons on water molecules in the system. These water protons exist in different environments, or groups (see Figure 1): on bulk water, on water hydrating the chemical species that are being modified under irradiation, and on water hydrating the gel matrix used to spatially stabilize the dosimeter (e.g., gelatin, agarose, etc). The spin relaxation depends on the inherent relaxation rate of each spin group, that is, on the relaxation rate which would be observed for the specific group if it were isolated. Also, the different water environments are not isolated from each other, and the observed relaxation rate also depends on the rate of exchange of magnetization between the groups, and on the fraction of protons in each group. In fact, the water exchanges quickly between the environments, so that relaxation is in what is usually termed the fast exchange regime. In the limit of fast exchange, the relaxation of the water protons is well characterized by a single exponential and hence by a single apparent relaxation rate. In irradiated gel dosimeters this

  4. Structural investigations of substituted indolizine derivatives by NMR studies

    International Nuclear Information System (INIS)

    Furdui, Bianca; Dinica, Rodica; Demeunynck, Martine; Druta, Ioan

    2008-01-01

    Owing to the increasing importance of indolizine heterocycles in the field of biology and pharmacology we have synthesized and investigated the obtained heterocycles by NMR techniques. In order to investigate the substituent effects on the spectroscopic properties, a series of indolizine derivatives were studied by 1 H-NMR, 13 C-NMR and 2D NMR (GCOSY, GHMBC and GHMQC spectra). (authors)

  5. NMR in the SPINE Structural Proteomics project.

    Science.gov (United States)

    Ab, E; Atkinson, A R; Banci, L; Bertini, I; Ciofi-Baffoni, S; Brunner, K; Diercks, T; Dötsch, V; Engelke, F; Folkers, G E; Griesinger, C; Gronwald, W; Günther, U; Habeck, M; de Jong, R N; Kalbitzer, H R; Kieffer, B; Leeflang, B R; Loss, S; Luchinat, C; Marquardsen, T; Moskau, D; Neidig, K P; Nilges, M; Piccioli, M; Pierattelli, R; Rieping, W; Schippmann, T; Schwalbe, H; Travé, G; Trenner, J; Wöhnert, J; Zweckstetter, M; Kaptein, R

    2006-10-01

    This paper describes the developments, role and contributions of the NMR spectroscopy groups in the Structural Proteomics In Europe (SPINE) consortium. Focusing on the development of high-throughput (HTP) pipelines for NMR structure determinations of proteins, all aspects from sample preparation, data acquisition, data processing, data analysis to structure determination have been improved with respect to sensitivity, automation, speed, robustness and validation. Specific highlights are protonless (13)C-direct detection methods and inferential structure determinations (ISD). In addition to technological improvements, these methods have been applied to deliver over 60 NMR structures of proteins, among which are five that failed to crystallize. The inclusion of NMR spectroscopy in structural proteomics pipelines improves the success rate for protein structure determinations.

  6. NMR study of Albemoschus esculentus characterization

    International Nuclear Information System (INIS)

    Bathista, A.L.B.S; Silva, E.O.; Nogueira, Jose de S.; Tavares, M.I.B.

    2001-01-01

    The investigation of the main compounds presented in the Albemoschus esculentus has been carried out employing nuclear magnetic resonance spectroscopy (NMR), using solution and solid state NMR when it one was necessary. The evaluation of NMR data allowed us to characterize the main type of components presented in this kind of sample. It was necessary to use a total information from solid state NMR and also the solution response. From these information we could get that four main components were presented in this sample. One in the shell, that is cellulose, another one between the shell and seeds that is a polysaccharide and in the seed two components were found one is a starch and the second one is an oil, a triacylglycerol. These components are responsible by its physical chemistry properties. (author)

  7. NMR and optical studies of piezoelectric polymers

    International Nuclear Information System (INIS)

    Schmidt, V.H.; Tuthill, G.F.

    1993-01-01

    Progress is reported in several areas dealing with piezoelectric (electroactive) polymers (mostly vinylidene fluoride, trifluoroethylene, copolymers, PVF 2 ) and liquid crystals. Optical studies, neutron scattering, NMR, thermal, theory and modeling were done

  8. High resolution NMR theory and chemical applications

    CERN Document Server

    Becker, Edwin D

    2012-01-01

    High Resolution NMR: Theory and Chemical Applications discusses the principles and theory of nuclear magnetic resonance and how this concept is used in the chemical sciences. This book is written at an intermediate level, with mathematics used to augment verbal descriptions of the phenomena. This text pays attention to developing and interrelating four approaches - the steady state energy levels, the rotating vector picture, the density matrix, and the product operator formalism. The style of this book is based on the assumption that the reader has an acquaintance with the general principles of quantum mechanics, but no extensive background in quantum theory or proficiency in mathematics is required. This book begins with a description of the basic physics, together with a brief account of the historical development of the field. It looks at the study of NMR in liquids, including high resolution NMR in the solid state and the principles of NMR imaging and localized spectroscopy. This book is intended to assis...

  9. NMR studies of cerebral metabolism in vivo

    International Nuclear Information System (INIS)

    Prichard, J.W.

    1986-01-01

    The nature and extent of the potential synergism between PET and NMR methods is not yet well appreciated in the biomedical community. The long-range interest of medical neurobiology will be well served by efforts of PET and NMR scientists to follow each others' work so that opportunities for productive interchange can be efficiently exploited. Appreciation of the synergism by the rest of the biomedical community will follow naturally. PET is said by the people doing it to be still in its infancy, for they are more concerned with advancing their discipline than with admiring its already impressive achievements. On the scale of the same developmental metaphor, many NMR methods for studying the living human brain are still in utero. The best way to provide the reader a sense of the current status and future course of NMR research in medical neurobiology is by discussion of published in vivo studies. Such a discussion, adapted from another article is what follows

  10. Development of Two-Dimensional NMR

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 20; Issue 11. Development of Two-Dimensional NMR: Strucure Determination of Biomolecules in Solution. Anil Kumar. General Article Volume 20 Issue 11 November 2015 pp 995-1002 ...

  11. NMR spectroscopy of coal pyrolysis products

    Energy Technology Data Exchange (ETDEWEB)

    Polonov, V.M.; Kalabin, G.A.; Kushnarev, D.F.; Shevchenko, G.G.

    1985-12-01

    The authors consider the scope for using H 1 and C 13 NMR spectroscopy to describe the products from coal pyrolysis and hydrogenization. The accuracy of the structural information provided by the best NMR methods is also considered. The stuctural parameters derived from H 1 and C 13 NMR spectra are presented. Results demonstrate the high accuracy and sensitivity of the structural information provided by H 1 AND C 13 NMR spectra for coal products. There are substantial structural differences between the soluble products from medium-temperature coking of Cheremkhov coal and high-speed pyrolysis of Kan-Acha coal, and also differences in behavior during hydrogenation. These differences are related to the structure of the organic matter in the initial coal and to differences in the pyrolysis mechanisms.

  12. NMR study of hydride systems

    International Nuclear Information System (INIS)

    Peretz, M.

    1980-02-01

    The hydrides of thorium (ThH 2 , Th 4 H 15 and Th 4 D 15 ) and the intermetallic compound system (Zr(Vsub(1-x)Cosub(x)) 2 and its hydrides were investigated using the nuclear magnetic resonance (NMR) technique. From the results for the thorium hydride samples it was concluded that the density of states at the Fermi level n(Esub(f)) is higher in Th 4 H 15 than in ThH 2 ; there is an indirect reaction between the protons and the d electrons belonging to the Th atoms in Th 4 H 15 ; n(E) has a sharp structure near Esub(f). It was also found that the hydrogen diffusion mechanism changes with temperature. From the results for the intermetallic compound system conclusions were drawn concerning variations in the electronic structure, which explain the behavior of the system. In hydrogen diffusion studies in several samples it was found that Co atoms slow the diffusion rate. Quadrupole spectra obtained at low temperatures show that the H atoms preferably occupy tetrahedral sites formed by three V atoms and one Z atom. (H.K.)

  13. Frontiers of NMR in Molecular Biology

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-08-25

    NMR spectroscopy is expanding the horizons of structural biology by determining the structures and describing the dynamics of blobular proteins in aqueous solution, as well as other classes of proteins including membrane proteins and the polypeptides that form the aggregates diagnostic of prion and amyloid diseases. Significant results are also emerging on DNA and RNA oligomers and their complexes with proteins. This meeting focused attention on key structural questions emanating from molecular biology and how NMR spectroscopy can be used to answer them.

  14. NMR studies of multiphase flows II

    Energy Technology Data Exchange (ETDEWEB)

    Altobelli, S.A.; Caprihan, A.; Fukushima, E. [Lovelace Institutes, Albuquerque, NM (United States)] [and others

    1995-12-31

    NMR techniques for measurements of spatial distribution of material phase, velocity and velocity fluctuation are being developed and refined. Versions of these techniques which provide time average liquid fraction and fluid phase velocity have been applied to several concentrated suspension systems which will not be discussed extensively here. Technical developments required to further extend the use of NMR to the multi-phase flow arena and to provide measurements of previously unobtainable parameters are the focus of this report.

  15. observed by high pressure NMR and NQR

    Indian Academy of Sciences (India)

    Akogun, Hyogo 678-1297, Japan. ∗. Email: kohara@sci.himeji tech.ac.jp. Abstract. NMR and NQR studies on two interesting systems (URu2Si2, CeTIn5) were performed under high pressure. (1) URu2Si2: In the pressure range 3.0 to 8.3 kbar, we have observed new 29Si. NMR signals arising from the antiferromagnetic ...

  16. Contact angle control of sessile drops on a tensioned web

    Science.gov (United States)

    Park, Janghoon; Kim, Dongguk; Lee, Changwoo

    2018-04-01

    In this study, the influence of the change of tension applied to flexible and thin web substrate on the contact angle of sessile drop in roll-to-roll system was investigated. Graphene oxide and deionized water solutions were used in the experiments. Tension was changed to 29, 49, and 69 N, and the casting distance of the micropipette and the material was set to 10, 20, and 40 mm, and the droplet volume was set to 10, 20, and 30 μL, respectively. Statistical analysis of three variables and analysis of the variance methodology showed that the casting distance was most significant for the contact angle change, and the most interesting tension variable was also affected. The change in tension caused the maximum contact angle to change by 5.5°. The tension was not uniform in the width direction. When the droplet was applied in the same direction in the width direction, it was confirmed that the tension unevenness had great influence on the contact angle up to 11°. Finally, the casting distance, which has a large effect on the contact angle, was calibrated in the width direction to reduce the width direction contact angle deviation to 1%. This study can be applied to fine patterning research using continuous inkjet printing and aerosol jet printing, which are roll-to-roll processes based on droplet handling.

  17. NMRbox: A Resource for Biomolecular NMR Computation.

    Science.gov (United States)

    Maciejewski, Mark W; Schuyler, Adam D; Gryk, Michael R; Moraru, Ion I; Romero, Pedro R; Ulrich, Eldon L; Eghbalnia, Hamid R; Livny, Miron; Delaglio, Frank; Hoch, Jeffrey C

    2017-04-25

    Advances in computation have been enabling many recent advances in biomolecular applications of NMR. Due to the wide diversity of applications of NMR, the number and variety of software packages for processing and analyzing NMR data is quite large, with labs relying on dozens, if not hundreds of software packages. Discovery, acquisition, installation, and maintenance of all these packages is a burdensome task. Because the majority of software packages originate in academic labs, persistence of the software is compromised when developers graduate, funding ceases, or investigators turn to other projects. To simplify access to and use of biomolecular NMR software, foster persistence, and enhance reproducibility of computational workflows, we have developed NMRbox, a shared resource for NMR software and computation. NMRbox employs virtualization to provide a comprehensive software environment preconfigured with hundreds of software packages, available as a downloadable virtual machine or as a Platform-as-a-Service supported by a dedicated compute cloud. Ongoing development includes a metadata harvester to regularize, annotate, and preserve workflows and facilitate and enhance data depositions to BioMagResBank, and tools for Bayesian inference to enhance the robustness and extensibility of computational analyses. In addition to facilitating use and preservation of the rich and dynamic software environment for biomolecular NMR, NMRbox fosters the development and deployment of a new class of metasoftware packages. NMRbox is freely available to not-for-profit users. Copyright © 2017 Biophysical Society. All rights reserved.

  18. A microscale protein NMR sample screening pipeline

    Energy Technology Data Exchange (ETDEWEB)

    Rossi, Paolo; Swapna, G. V. T.; Huang, Yuanpeng J.; Aramini, James M. [State University of New Jersey, Center for Advanced Biotechnology and Medicine, Department of Molecular Biology and Biochemistry, Rutgers (United States); Anklin, Clemens [Bruker Biospin Corporation (United States); Conover, Kenith; Hamilton, Keith; Xiao, Rong; Acton, Thomas B.; Ertekin, Asli; Everett, John K.; Montelione, Gaetano T., E-mail: guy@cabm.rutgers.ed [State University of New Jersey, Center for Advanced Biotechnology and Medicine, Department of Molecular Biology and Biochemistry, Rutgers (United States)

    2010-01-15

    As part of efforts to develop improved methods for NMR protein sample preparation and structure determination, the Northeast Structural Genomics Consortium (NESG) has implemented an NMR screening pipeline for protein target selection, construct optimization, and buffer optimization, incorporating efficient microscale NMR screening of proteins using a micro-cryoprobe. The process is feasible because the newest generation probe requires only small amounts of protein, typically 30-200 {mu}g in 8-35 {mu}l volume. Extensive automation has been made possible by the combination of database tools, mechanization of key process steps, and the use of a micro-cryoprobe that gives excellent data while requiring little optimization and manual setup. In this perspective, we describe the overall process used by the NESG for screening NMR samples as part of a sample optimization process, assessing optimal construct design and solution conditions, as well as for determining protein rotational correlation times in order to assess protein oligomerization states. Database infrastructure has been developed to allow for flexible implementation of new screening protocols and harvesting of the resulting output. The NESG micro NMR screening pipeline has also been used for detergent screening of membrane proteins. Descriptions of the individual steps in the NESG NMR sample design, production, and screening pipeline are presented in the format of a standard operating procedure.

  19. O-17 NMR measurement of water

    International Nuclear Information System (INIS)

    Fukazawa, Nobuyuki

    1990-01-01

    Recently, attention has been paid to the various treatment of water and the utilization of water by magnetic treatment, electric field treatment and so on. It has been said that by these treatments, the change in the properties of water arises. The state of this treated water cannot be explained by the properties of water from conventional physical and chemical standpoints. In addition, the method of measurement of whether the change arose or not is not yet determined. It is necessary to establish the method of measurement for the basic state of water. In this study, O-17 NMR which observes the state of water directly at molecular or atomic level was investigated as the method of measuring water. The measurement of O-17 NMR was carried out with a JNR 90Q FT NMR of Fourier transformation type of JEOL Ltd. The experimental method and the results are reported. The result of measurement of the O-17 NMR spectrum for distilled ion exchange water is shown. It is know that it has very wide line width as compared with the NMR spectra of protons and C-13. The relative sensitivity of O-17 observation is about 1/100,000 of that of protons. As to the information on the state of water obtained by O-17 NMR, there are chemical shift and line width. As temperature rose, the line width showed decrease, which seemed to be related to the decrease of hydrogen combination. (K.I.)

  20. Basics of spectroscopic instruments. Hardware of NMR spectrometer

    International Nuclear Information System (INIS)

    Sato, Hajime

    2009-01-01

    NMR is a powerful tool for structure analysis of small molecules, natural products, biological macromolecules, synthesized polymers, samples from material science and so on. Magnetic Resonance Imaging (MRI) is applicable to plants and animals Because most of NMR experiments can be done by an automation mode, one can forget hardware of NMR spectrometers. It would be good to understand features and performance of NMR spectrometers. Here I present hardware of a modern NMR spectrometer which is fully equipped with digital technology. (author)

  1. 33S NMR cryogenic probe for taurine detection

    Science.gov (United States)

    Hobo, Fumio; Takahashi, Masato; Maeda, Hideaki

    2009-03-01

    With the goal of a S33 nuclear magnetic resonance (NMR) probe applicable to in vivo NMR on taurine-biological samples, we have developed the S33 NMR cryogenic probe, which is applicable to taurine solutions. The NMR sensitivity gain relative to a conventional broadband probe is as large as 3.5. This work suggests that improvements in the preamplifier could allow NMR measurements on 100 μM taurine solutions, which is the level of sensitivity necessary for biological samples.

  2. Petrophysical properties of greensand as predicted from NMR measurements

    DEFF Research Database (Denmark)

    Hossain, Zakir; Grattoni, Carlos A.; Solymar, Mikael

    2011-01-01

    ABSTRACT: Nuclear magnetic resonance (NMR) is a useful tool in reservoir evaluation. The objective of this study is to predict petrophysical properties from NMR T2 distributions. A series of laboratory experiments including core analysis, capillary pressure measurements, NMR T2 measurements...... with macro-pores. Permeability may be predicted from NMR by using Kozeny's equation when surface relaxivity is known. Capillary pressure drainage curves may be predicted from NMR T2 distribution when pore size distribution within a sample is homogeneous....

  3. 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

  4. Analytical solution to the coupled evolution of multidimensional NMR data

    International Nuclear Information System (INIS)

    Mueller, Geoffrey A.

    2009-01-01

    A substantial time savings in the collection of multidimensional NMR data can be achieved by coupling the evolution of nuclei in the indirect dimensions. In order to save time, the sampling of the indirect dimensions is inherently incomplete. Therefore, many algorithms and samplings schemes have been developed aimed at separating the coevolved frequencies into analyzable data with limited artifacts. This paper extends the use of circulant matrices to describe coupled evolution with convolutions. By understanding the data in terms of convolutions, there is an exact solution to the inversion problem of extracting the orthogonal vectors from the coupled dimensions. Previously, this inversion problem has been solved using peak coordinates extracted from spectra. In contrast, the method described here uses spectra directly. This solution suggests a simple sampling scheme of collecting N orthogonal spectra, and N + 1 projections at specific projection angles, however, the theory developed can be extended generally to arbitrary projection angles. The circulant matrix methodology is demonstrated for simulated and real data. Further, an algorithm for separating overlapped signals in the detected dimension is presented. The algorithm involves the forward calculation of the coupled spectra from the orthogonal spectra, followed by back calculation of the orthogonal spectra from the coupled spectra, thus permitting rigorous cross-validation. This algorithm is shown to be robust in that erroneous solutions give rise to large artifacts

  5. A study of images of Projective Angles of pulmonary veins

    Energy Technology Data Exchange (ETDEWEB)

    Wang Jue [Beijing Anzhen Hospital, Beijing (China); Zhaoqi, Zhang [Beijing Anzhen Hospital, Beijing (China)], E-mail: zhaoqi5000@vip.sohu.com; Yu Wei; Miao Cuilian; Yan Zixu; Zhao Yike [Beijing Anzhen Hospital, Beijing (China)

    2009-09-15

    Aims: In images of magnetic resonance and computed tomography (CT) there are visible angles between pulmonary veins and the coronary, transversal or sagittal section of body. In this study these angles are measured and defined as Projective Angles of pulmonary veins. Several possible influential factors and characters of distribution are studied and analyzed for a better understanding of this imaging anatomic character of pulmonary veins. And it could be the anatomic base of adjusting correctly the angle of the central X-ray of the angiography of pulmonary veins undergoing the catheter ablation of atrial fibrillation (AF). Method: Images of contrast enhanced magnetic resonance angiography (CEMRA) and contrast enhanced computer tomography (CECT) of the left atrium and pulmonary veins of 137 health objects and patients with atrial fibrillation (AF) are processed with the technique of post-processing, and Projective Angles to the coronary and transversal sections are measured and analyzed statistically. Result: Project Angles of pulmonary veins are one of real and steady imaging anatomic characteristics of pulmonary veins. The statistical distribution of variables is relatively concentrated, with a fairly good representation of average value. It is possible to improve the angle of the central X-ray according to the average value in the selective angiography of pulmonary veins undergoing the catheter ablation of AF.

  6. Study of conformation and dynamic of surfactant molecules in graphite oxide via NMR

    Energy Technology Data Exchange (ETDEWEB)

    Ai, X.Q. [Jiangsu Second Normal University, College of Physics and Electronic Engineering, Nanjing (China); Ma, L.G. [Nanjing Xiaozhuang University, School of Electronic Engineering, Nanjing (China)

    2016-08-15

    The conformation and dynamic of surfactant in graphite oxide (GO) was investigated by solid-state {sup 13}C magic-angle-spinning NMR and {sup 1}H-{sup 13}C cross-polarization/magic-angle-spinning NMR spectra. The conformation ordering of the alkyl chains in the confined system shows strong dependence on its orientation. While the alkyl chains parallel to the GO layer in lateral monolayer arrangement are in gauche conformation in addition to a small amount of all-trans conformation, those with orientation radiating away from the GO in paraffin bilayer arrangement is in all-trans conformation in addition to some gauche conformation even though high-order diffraction peaks appears. NMR results suggest that the least mobile segment is located at the GO-surfactant interface corresponding to the N-methylene group. Further from it, the mobility of the alkyl chain increases. The terminal methyl and N-methyl carbon groups have the highest mobile. The chains in all-trans conformational state are characterized as more rigid than chains with gauche conformation; each segment of the confined alkyl chains with the lateral monolayer arrangement exhibits less mobility as compared to that with the paraffin bilayer arrangement. (orig.)

  7. The war of tools: how can NMR spectroscopists detect errors in their structures?

    Energy Technology Data Exchange (ETDEWEB)

    Saccenti, Edoardo; Rosato, Antonio [University of Florence, Magnetic Resonance Center (Italy)], E-mail: rosato@cerm.unifi.it

    2008-04-15

    Protein structure determination by NMR methods has started in the mid-eighties and has been growing steadily since then. Ca. 14% of the protein structures deposited in the PDB have been solved by NMR. The evaluation of the quality of NMR structures however is still lacking a well-established practice. In this work, we examined various tools for the assessment of structural quality to ascertain the extent to which these tools could be applied to detect flaws in NMR structures. In particular, we investigated the variation in the scores assigned by these programs as a function of the deviation of the structures induced by errors in assignments or in the upper distance limits used. These perturbations did not distort radically the protein fold, but resulted in backbone RMS deviations up to 3 A, which is in line with errors highlighted in the available literature. We found that it is quite difficult to discriminate the structures perturbed because of misassignments from the original ones, also because the spread in score over the conformers of the original bundle is relatively large. {phi}-{psi} distributions and normality scores related to the backbone conformation and to the distribution of side-chain dihedral angles are the most sensitive indicators of flaws.

  8. Computational characterization of 13C NMR lineshapes of carbon dioxide in structure 1 clathrate hydrates

    Energy Technology Data Exchange (ETDEWEB)

    Dornan, P.; Woo, T.K. [Ottawa Univ., ON (Canada). Dept. of Chemistry

    2008-07-01

    Nonspherical large cages in structure one clathrates impose non-uniform motion of nonspherical guest molecules and anisotropic lineshapes in nuclear magnetic resonance (NMR) spectra of the guest. This paper presented a general method for calculating the chemical shift lineshape anisotropy of guest molecules in clathrate hydrate compounds from molecular dynamics simulations for the case of weak host, guest dipolar coupling. In order to calculate the cage chemical shielding tensors and the NMR lineshape produced by each guest molecule, the study involved the use of orientational distributions from molecular dynamics simulation along with time and powder angle averaging. The total predicted lineshape anisotropy was calculated from the superposition of the lineshapes of all guests. The approach was applied to calculate the temperature dependent 13C NMR lineshape anisotropy of carbon dioxide in structure 1 clathrates. The paper presented the computational methodology and results and discussion. It was concluded that the resulting lineshapes were in good agreement with the experimental 13C NMR spectrum at each temperature. The method provided a uniform procedure to calculate the lineshapes at different temperatures and no prior assumptions about the nature of the motion of the guest in cages was required. 37 refs., 2 tabs., 3 figs.

  9. High-resolution NMR characterization of low abundance oligomers of amyloid-β without purification.

    Science.gov (United States)

    Kotler, Samuel A; Brender, Jeffrey R; Vivekanandan, Subramanian; Suzuki, Yuta; Yamamoto, Kazutoshi; Monette, Martine; Krishnamoorthy, Janarthanan; Walsh, Patrick; Cauble, Meagan; Holl, Mark M Banaszak; Marsh, E Neil G; Ramamoorthy, Ayyalusamy

    2015-07-03

    Alzheimer's disease is characterized by the misfolding and self-assembly of the amyloidogenic protein amyloid-β (Aβ). The aggregation of Aβ leads to diverse oligomeric states, each of which may be potential targets for intervention. Obtaining insight into Aβ oligomers at the atomic level has been a major challenge to most techniques. Here, we use magic angle spinning recoupling (1)H-(1)H NMR experiments to overcome many of these limitations. Using (1)H-(1)H dipolar couplings as a NMR spectral filter to remove both high and low molecular weight species, we provide atomic-level characterization of a non-fibrillar aggregation product of the Aβ1-40 peptide using non-frozen samples without isotopic labeling. Importantly, this spectral filter allows the detection of the specific oligomer signal without a separate purification procedure. In comparison to other solid-state NMR techniques, the experiment is extraordinarily selective and sensitive. A resolved 2D spectra could be acquired of a small population of oligomers (6 micrograms, 7% of the total) amongst a much larger population of monomers and fibers (93% of the total). By coupling real-time (1)H-(1)H NMR experiments with other biophysical measurements, we show that a stable, primarily disordered Aβ1-40 oligomer 5-15 nm in diameter can form and coexist in parallel with the well-known cross-β-sheet fibrils.

  10. Frequency scaling for angle gathers

    KAUST Repository

    Zuberi, M. A H; Alkhalifah, Tariq Ali

    2014-01-01

    Angle gathers provide an extra dimension to analyze the velocity after migration. Space-shift and time shift-imaging conditions are two methods used to obtain angle gathers, but both are reasonably expensive. By scaling the time-lag axis of the time-shifted images, the computational cost of the time shift imaging condition can be considerably reduced. In imaging and more so Full waveform inversion, frequencydomain Helmholtz solvers are used more often to solve for the wavefields than conventional time domain extrapolators. In such cases, we do not need to extend the image, instead we scale the frequency axis of the frequency domain image to obtain the angle gathers more efficiently. Application on synthetic data demonstrate such features.

  11. Angle imaging: Advances and challenges

    Science.gov (United States)

    Quek, Desmond T L; Nongpiur, Monisha E; Perera, Shamira A; Aung, Tin

    2011-01-01

    Primary angle closure glaucoma (PACG) is a major form of glaucoma in large populous countries in East and South Asia. The high visual morbidity from PACG is related to the destructive nature of the asymptomatic form of the disease. Early detection of anatomically narrow angles is important and the subsequent prevention of visual loss from PACG depends on an accurate assessment of the anterior chamber angle (ACA). This review paper discusses the advantages and limitations of newer ACA imaging technologies, namely ultrasound biomicroscopy, Scheimpflug photography, anterior segment optical coherence tomography and EyeCam, highlighting the current clinical evidence comparing these devices with each other and with clinical dynamic indentation gonioscopy, the current reference standard. PMID:21150037

  12. Towards automatic metabolomic profiling of high-resolution one-dimensional proton NMR spectra

    Energy Technology Data Exchange (ETDEWEB)

    Mercier, Pascal; Lewis, Michael J.; Chang, David, E-mail: dchang@chenomx.com [Chenomx Inc (Canada); Baker, David [Pfizer Inc (United States); Wishart, David S. [University of Alberta, Department of Computing Science and Biological Sciences (Canada)

    2011-04-15

    Nuclear magnetic resonance (NMR) and Mass Spectroscopy (MS) are the two most common spectroscopic analytical techniques employed in metabolomics. The large spectral datasets generated by NMR and MS are often analyzed using data reduction techniques like Principal Component Analysis (PCA). Although rapid, these methods are susceptible to solvent and matrix effects, high rates of false positives, lack of reproducibility and limited data transferability from one platform to the next. Given these limitations, a growing trend in both NMR and MS-based metabolomics is towards targeted profiling or 'quantitative' metabolomics, wherein compounds are identified and quantified via spectral fitting prior to any statistical analysis. Despite the obvious advantages of this method, targeted profiling is hindered by the time required to perform manual or computer-assisted spectral fitting. In an effort to increase data analysis throughput for NMR-based metabolomics, we have developed an automatic method for identifying and quantifying metabolites in one-dimensional (1D) proton NMR spectra. This new algorithm is capable of using carefully constructed reference spectra and optimizing thousands of variables to reconstruct experimental NMR spectra of biofluids using rules and concepts derived from physical chemistry and NMR theory. The automated profiling program has been tested against spectra of synthetic mixtures as well as biological spectra of urine, serum and cerebral spinal fluid (CSF). Our results indicate that the algorithm can correctly identify compounds with high fidelity in each biofluid sample (except for urine). Furthermore, the metabolite concentrations exhibit a very high correlation with both simulated and manually-detected values.

  13. Towards automatic metabolomic profiling of high-resolution one-dimensional proton NMR spectra

    International Nuclear Information System (INIS)

    Mercier, Pascal; Lewis, Michael J.; Chang, David; Baker, David; Wishart, David S.

    2011-01-01

    Nuclear magnetic resonance (NMR) and Mass Spectroscopy (MS) are the two most common spectroscopic analytical techniques employed in metabolomics. The large spectral datasets generated by NMR and MS are often analyzed using data reduction techniques like Principal Component Analysis (PCA). Although rapid, these methods are susceptible to solvent and matrix effects, high rates of false positives, lack of reproducibility and limited data transferability from one platform to the next. Given these limitations, a growing trend in both NMR and MS-based metabolomics is towards targeted profiling or “quantitative” metabolomics, wherein compounds are identified and quantified via spectral fitting prior to any statistical analysis. Despite the obvious advantages of this method, targeted profiling is hindered by the time required to perform manual or computer-assisted spectral fitting. In an effort to increase data analysis throughput for NMR-based metabolomics, we have developed an automatic method for identifying and quantifying metabolites in one-dimensional (1D) proton NMR spectra. This new algorithm is capable of using carefully constructed reference spectra and optimizing thousands of variables to reconstruct experimental NMR spectra of biofluids using rules and concepts derived from physical chemistry and NMR theory. The automated profiling program has been tested against spectra of synthetic mixtures as well as biological spectra of urine, serum and cerebral spinal fluid (CSF). Our results indicate that the algorithm can correctly identify compounds with high fidelity in each biofluid sample (except for urine). Furthermore, the metabolite concentrations exhibit a very high correlation with both simulated and manually-detected values.

  14. Angle independent velocity spectrum determination

    DEFF Research Database (Denmark)

    2014-01-01

    An ultrasound imaging system (100) includes a transducer array (102) that emits an ultrasound beam and produces at least one transverse pulse-echo field that oscillates in a direction transverse to the emitted ultrasound beam and that receive echoes produced in response thereto and a spectral vel...... velocity estimator (110) that determines a velocity spectrum for flowing structure, which flows at an angle of 90 degrees and flows at angles less than 90 degrees with respect to the emitted ultrasound beam, based on the received echoes....

  15. Temperature dependence of Brewster's angle.

    Science.gov (United States)

    Guo, Wei

    2018-01-01

    In this work, a dielectric at a finite temperature is modeled as an ensemble of identical atoms moving randomly around where they are trapped. Light reflection from the dielectric is then discussed in terms of atomic radiation. Specific calculation demonstrates that because of the atoms' thermal motion, Brewster's angle is, in principle, temperature-dependent, and the dependence is weak in the low-temperature limit. What is also found is that the Brewster's angle is nothing but a result of destructive superposition of electromagnetic radiation from the atoms.

  16. Continuous Flow 1H and 13C NMR Spectroscopy in Microfluidic Stripline NMR Chips

    NARCIS (Netherlands)

    Oosthoek-de Vries, Anna Jo; Bart, Jacob; Tiggelaar, Roald M.; Janssen, Johannes W.G.; van Bentum, Jan (P.J.M.); Gardeniers, Han J.G.E.; Kentgens, Arno P.M.

    2017-01-01

    Microfluidic stripline NMR technology not only allows for NMR experiments to be performed on small sample volumes in the submicroliter range, but also experiments can easily be performed in continuous flow because of the stripline's favorable geometry. In this study we demonstrate the possibility of

  17. Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR.

    Science.gov (United States)

    van der Schot, Gijs; Bonvin, Alexandre M J J

    2015-08-01

    We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665-1674, 2005b, doi: 10.1021/ja047109h). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27-35, 2013, doi: 10.1007/s10858-013-9762-6), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution.

  18. Use of NMR and NMR Prediction Software to Identify Components in Red Bull Energy Drinks

    Science.gov (United States)

    Simpson, Andre J.; Shirzadi, Azadeh; Burrow, Timothy E.; Dicks, Andrew P.; Lefebvre, Brent; Corrin, Tricia

    2009-01-01

    A laboratory experiment designed as part of an upper-level undergraduate analytical chemistry course is described. Students investigate two popular soft drinks (Red Bull Energy Drink and sugar-free Red Bull Energy Drink) by NMR spectroscopy. With assistance of modern NMR prediction software they identify and quantify major components in each…

  19. New methods for the correction of 31P NMR spectra in in vivo NMR spectroscopy

    International Nuclear Information System (INIS)

    Starcuk, Z.; Bartusek, K.; Starcuk, Z. jr.

    1994-01-01

    The new methods for the correction of 31 P NMR spectra in vivo NMR spectroscopy have been performed. A method for the baseline correction of the spectra which represents a combination of time-domain and frequency-domain has been discussed.The method is very fast and efficient for minimization of base line artifacts of biological tissues impact

  20. Design of a self-calibration high precision micro-angle deformation optical monitoring scheme

    Science.gov (United States)

    Gu, Yingying; Wang, Li; Guo, Shaogang; Wu, Yun; Liu, Da

    2018-03-01

    In order to meet the requirement of high precision and micro-angle measurement on orbit, a self-calibrated optical non-contact real-time monitoring device is designed. Within three meters, the micro-angle variable of target relative to measuring basis can be measured in real-time. The range of angle measurement is +/-50'', the angle measurement accuracy is less than 2''. The equipment can realize high precision real-time monitoring the micro-angle deformation, which caused by high strength vibration and shock of rock launching, sun radiation and heat conduction on orbit and so on.

  1. Optimisation of underwater visual census and controlled angling ...

    African Journals Online (AJOL)

    Whereas UVC provided less variable estimates of relative density, controlled angling provided greater sampling efficiency. It is thus recommended that the two methods be used in conjunction. The optimal sampling protocols identified are suitable for rapid assessments or long-term monitoring of subtidal, temperate reef fish ...

  2. HPLC-NMR revisited: Using time-slice HPLC-SPE-NMR with database assisted dereplication

    DEFF Research Database (Denmark)

    Johansen, Kenneth; Wubshet, Sileshi Gizachew; Nyberg, Nils

    2013-01-01

    Time based trapping of chromatographically separated compounds on to solid-phase extraction cartridges (SPE) and subsequent elution to NMR-tubes was done to emulate the function of HPLC–NMR for dereplication purposes. Sufficient mass sensitivity was obtained by the use of a state-of-the-art HPLC......–SPE–NMR-system with a cryogenically cooled probe head, designed for 1.7 mm NMR-tubes. The resulting 1H NMR spectra (600 MHz) were evaluated against a database of previously acquired and prepared spectra. The in-house developed matching algorithm, based on partitioning of the spectra and allowing for changes in the chemical shifts......, is described and the code included as Supplementary Information. Two mixtures of natural products was used to test the approach; one extract of Carthamus oxyacantha (wild safflower) containing an array of spiro compounds and one extract of the endophytic fungus Penicillum namyslowski containing griseofulvin...

  3. 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...

  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. 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.

  6. NMR techniques in the study of cardiovascular structure and functions

    International Nuclear Information System (INIS)

    Osbakken, M.; Haselgrove, J.

    1987-01-01

    The chapter titles of this book are: Introduction to NMR Techniques;Theory of NMR Probe Design;Overview of Magnetic Resonance Imaging to Study the Cardiovascular System;Vascular Anatomy and Physiology Studied with NMR Techniques;Assessment of Myocardial Ischemia and Infarction by Nuclear Magnetic Resonance Imaging;The Use of MRI in Congenital Heart Disease;Cardiomyopathies and Myocarditis Studied with NMR Techniques;Determination of Myocardial Mechanical Function with Magnetic Resonance Imaging Techniques;Determination of Flow Using NMR Techniques;The Use of Contrast Agents in Cardiac MRI;Can Cardiovascular Disease Be Effectively Evaluated with NMR Spectroscopy? NMR Studies of ATP Synthesis Reactions in the Isolated Heart;Studies of Intermediary Metabolism in the Heart by 13C NMR Spectroscopy;23Na and 39K NMR Spectroscopic Studies of the Intact Beating Heart;and Evaluation of Skeletal Muscle Metabolism in Patients with Congestive Heart Failure Using Phosphorus Nuclear Magnetic Resonance

  7. High resolution NMR spectroscopy of synthetic polymers in bulk

    International Nuclear Information System (INIS)

    Komorski, R.A.

    1986-01-01

    The contents of this book are: Overview of high-resolution NMR of solid polymers; High-resolution NMR of glassy amorphous polymers; Carbon-13 solid-state NMR of semicrystalline polymers; Conformational analysis of polymers of solid-state NMR; High-resolution NMR studies of oriented polymers; High-resolution solid-state NMR of protons in polymers; and Deuterium NMR of solid polymers. This work brings together the various approaches for high-resolution NMR studies of bulk polymers into one volume. Heavy emphasis is, of course, given to 13C NMR studies both above and below Tg. Standard high-power pulse and wide-line techniques are not covered

  8. 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....

  9. Prostate Cancer Diagnosis: experimental and Clinical Studies With HRMAS NMR Spectroscopy

    International Nuclear Information System (INIS)

    Stenman, Katarina

    2011-01-01

    and 2D high-resolution magic angle spinning (HRMAS) NMR spectroscopy combined with histopathology on intact prostatectomy specimens was evaluated in this research project. The non-destructive nature of HRMAS NMR enables spectroscopic analysis of intact tissue samples with consecutive histological examinations under light microscope. Metabolomics aids in the unraveling and the discovery of organ-specific endogenous metabolites that have the potential to be reliable indicators of organ function and viability, extrinsic and intrinsic perturbations, as well as valuable markers for treatment response. The results may, therefore, be applied clinically to characterize an organ by utilizing bio-markers that have the capacity to distinguish between disease and health. The aim was to characterize the human and the rat prostate in terms of its intermediary metabolism, which is shown here to differ between species and anatomical regions. Furthermore, the aim is to seek the verification of HRMAS NMR derived metabolites which are known to be a part of the prostate metabolome such as, citrate, choline, and the polyamines which were performed, but also the identification of metabolites not previously identified as part of the local prostate metabolism, such as Omega-6, which was detected in tumors. The extended aim was to elucidate novel bio-markers with clinical potential. In this study, the common phyto-nutrient, inositol, which appears to possess protective properties, was identified as being a potentially important PCa bio-marker for the distinction between the more indolent Gleason score 6 and the more aggressive Gleason score 7 in non-malignant prostate tissues with tumors elsewhere in the organ. Further studies in this area of PCa research are therefore warranted

  10. Prostate Cancer Diagnosis: experimental and Clinical Studies With HRMAS NMR Spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stenman, Katarina

    2011-07-01

    approach using 1D and 2D high-resolution magic angle spinning (HRMAS) NMR spectroscopy combined with histopathology on intact prostatectomy specimens was evaluated in this research project. The non-destructive nature of HRMAS NMR enables spectroscopic analysis of intact tissue samples with consecutive histological examinations under light microscope. Metabolomics aids in the unraveling and the discovery of organ-specific endogenous metabolites that have the potential to be reliable indicators of organ function and viability, extrinsic and intrinsic perturbations, as well as valuable markers for treatment response. The results may, therefore, be applied clinically to characterize an organ by utilizing bio-markers that have the capacity to distinguish between disease and health. The aim was to characterize the human and the rat prostate in terms of its intermediary metabolism, which is shown here to differ between species and anatomical regions. Furthermore, the aim is to seek the verification of HRMAS NMR derived metabolites which are known to be a part of the prostate metabolome such as, citrate, choline, and the polyamines which were performed, but also the identification of metabolites not previously identified as part of the local prostate metabolism, such as Omega-6, which was detected in tumors. The extended aim was to elucidate novel bio-markers with clinical potential. In this study, the common phyto-nutrient, inositol, which appears to possess protective properties, was identified as being a potentially important PCa bio-marker for the distinction between the more indolent Gleason score 6 and the more aggressive Gleason score 7 in non-malignant prostate tissues with tumors elsewhere in the organ. Further studies in this area of PCa research are therefore warranted

  11. Multi-angle compound imaging

    DEFF Research Database (Denmark)

    Jespersen, Søren Kragh; Wilhjelm, Jens Erik; Sillesen, Henrik

    1998-01-01

    This paper reports on a scanning technique, denoted multi-angle compound imaging (MACI), using spatial compounding. The MACI method also contains elements of frequency compounding, as the transmit frequency is lowered for the highest beam angles in order to reduce grating lobes. Compared to conve......This paper reports on a scanning technique, denoted multi-angle compound imaging (MACI), using spatial compounding. The MACI method also contains elements of frequency compounding, as the transmit frequency is lowered for the highest beam angles in order to reduce grating lobes. Compared...... to conventional B-mode imaging MACI offers better defined tissue boundaries and lower variance of the speckle pattern, resulting in an image with reduced random variations. Design and implementation of a compound imaging system is described, images of rubber tubes and porcine aorta are shown and effects...... on visualization are discussed. The speckle reduction is analyzed numerically and the results are found to be in excellent agreement with existing theory. An investigation of detectability of low-contrast lesions shows significant improvements compared to conventional imaging. Finally, possibilities for improving...

  12. Femoral varus: what's the angle

    DEFF Research Database (Denmark)

    Miles, James Edward; Svalastoga, Eiliv Lars; Eriksen, Thomas

    angles were calculated using Microsoft Excel for the three previously reported techniques and a novel method, which we believed would be more reliable. Reliability between readings was assessed using the within-subject standard deviation and repeatability coefficient, and the effect of angulation...

  13. High-pressure, high-temperature magic angle spinning nuclear magnetic resonance devices and processes for making and using same

    Science.gov (United States)

    Hu, Jian Zhi; Hu, Mary Y.; Townsend, Mark R.; Lercher, Johannes A.; Peden, Charles H. F.

    2015-10-06

    Re-usable ceramic magic angle spinning (MAS) NMR rotors constructed of high-mechanic strength ceramics are detailed that include a sample compartment that maintains high pressures up to at least about 200 atmospheres (atm) and high temperatures up to about least about 300.degree. C. during operation. The rotor designs minimize pressure losses stemming from penetration over an extended period of time. The present invention makes possible a variety of in-situ high pressure, high temperature MAS NMR experiments not previously achieved in the prior art.

  14. Nuclear magnetic resonance (NMR): principles and applications

    International Nuclear Information System (INIS)

    Quibilan, E.I.

    The basis for the phenomenon of nuclear magnetic resonance (NMR) is the ability of certain nuclei possessing both intrinsic angular momentum or ''spin'' I and magnetic moment to absorb electromagnetic energy in the radio frequency range. In principle, there are approximately 200 nuclei which may be investigated using the NMR technique. The NMR spectrum consists of intensity peaks along an axis calibrated in terms of the steady magnetic field or the frequency of the radiofrequency electromagnetic radiation. Analysis of the number, spacing, position and intensity of the lines in an NMR spectrum consists of intensity peaks along an axis calibrated in terms of the steady magnetic field or the frequency of the radiofrequency electromagnetic radiation. Analysis of the number, spacing, position and intensity of the lines in an NMR spectrum provides a variety of qualitative and quantitative analytical applications. The most obvious applications consist of the measurements of nuclear properties, such as spin number and nuclear magnetic moment. In liquids, the fine structure of resonance spectra provides a tool for chemical identification and molecular structure analysis. Other applications include the measurements of self-diffusion coefficients, magnetic fields and field homogeneity, inter-nuclear distances, and, in some cases, the water content of biological materials. (author)

  15. NMR studies on magnetic properties of intermetallic compounds Er1-xYxCo3

    International Nuclear Information System (INIS)

    Niki, H.; Kinjo, T.; Yogi, M.; Pieper, M.W.; Gratz, E.; Markosyan, A.S.

    2007-01-01

    Field dependence of 59 Co NMR in ferrimagnetic Er 1-x Y x Co 3 was measured up to 8T at 4.2K using aligned powdered samples. For pure ErCo 3 in fields perpendicular to the c axis the resonance frequencies change discontinuously between 2 and 3T due to a field induced metamagnetic transition. The easy axis is found to be along the c axis for x=0 and 0.1. An average angle for the Co moments of 45+/-5 o from the c axis is obtained from field dependence of 59 Co NMR at x=0.3. Directions of Co moments are also found to be inclined from the c axis for x=0.5

  16. 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.

  17. 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)

  18. NMR-based Enantiodifferentiation of Chiral trans-2-Phenylcyclopropane Derivatives Using a Chiral Lanthanide Shift Reagent

    International Nuclear Information System (INIS)

    Cho, Nam Sook; Kim, Hyun Sook; Song, Mi Sook

    2011-01-01

    In contrast with optical methods, there is no need to characterize the pure enantiomers. Instead, the NMR method makes use of chiral reagents that convert a mixture of enantiomers into a mixture of diastereomeric complexes. Integration of the resulting NMR spectra yields a direct measurement of enantiomeric purity as long as there is a sufficiently large difference between the chemical shifts of the two diastereoisomeric complexes to produce baseline-resolved peaks. Absolute enantiomeric configurations can also be determined using this method. Chiral lanthanide shift reagents have been used since the 1970s to form addition complexes with various compounds through interactions with electron donor sites. Lanthanide-induced, pseudo-contact shifts (LIS) are a function of the distance, r, between the nuclei under observation and the lanthanide center, and the angle, θ, between the line connecting the metal ion with the observed nucleus and the line representing the CLSR magnetic axis

  19. 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

  20. 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...

  1. NMR Phase Noise in Bitter Magnets

    Science.gov (United States)

    Sigmund, E. E.; Calder, E. S.; Thomas, G. W.; Mitrović, V. F.; Bachman, H. N.; Halperin, W. P.; Kuhns, P. L.; Reyes, A. P.

    2001-02-01

    We have studied the temporal instability of a high field resistive Bitter magnet through nuclear magnetic resonance (NMR). This instability leads to transverse spin decoherence in repeated and accumulated NMR experiments as is normally performed during signal averaging. We demonstrate this effect via Hahn echo and Carr-Purcell-Meiboom-Gill (CPMG) transverse relaxation experiments in a 23-T resistive magnet. Quantitative analysis was found to be consistent with separate measurements of the magnetic field frequency fluctuation spectrum, as well as with independent NMR experiments performed in a magnetic field with a controlled instability. Finally, the CPMG sequence with short pulse delays is shown to be successful in recovering the intrinsic spin-spin relaxation even in the presence of magnetic field temporal instability.

  2. Remote tuning of NMR probe circuits.

    Science.gov (United States)

    Kodibagkar, V D; Conradi, M S

    2000-05-01

    There are many circumstances in which the probe tuning adjustments cannot be located near the rf NMR coil. These may occur in high-temperature NMR, low-temperature NMR, and in the use of magnets with small diameter access bores. We address here circuitry for connecting a fixed-tuned probe circuit by a transmission line to a remotely located tuning network. In particular, the bandwidth over which the probe may be remotely tuned while keeping the losses in the transmission line acceptably low is considered. The results show that for all resonant circuit geometries (series, parallel, series-parallel), overcoupling of the line to the tuned circuit is key to obtaining a large tuning bandwidth. At equivalent extents of overcoupling, all resonant circuit geometries have nearly equal remote tuning bandwidths. Particularly for the case of low-loss transmission line, the tuning bandwidth can be many times the tuned circuit's bandwidth, f(o)/Q. Copyright 2000 Academic Press.

  3. Deuterium NMR, induced and intrinsic cholesteric lyomesophases

    International Nuclear Information System (INIS)

    Alcantara, M.R.

    1982-01-01

    Induced and intrinsic cholesteric lyotropic mesophases were studied. Induced cholesteric lyomesophases based on potassium laurate (KL) system, with small amounts of cholesterol added, were studied by deuterium NMR and by polarizing microscopy. Order profiles obtained from deuterium NMR of KL perdenderated chains in both induced cholesteric and normal mesophases were compared. The intrinsic cholesteric lyotropic mesophases were based on the amphiphile potassium N-lauroyl serinate (KLNS) in the resolved levo form. The study of the type I intrinsic cholesteric mesophase was made by optical microscopy under polarized light and the type II intrinsic cholesteric lyomesophase was characterized by deuterium NMR. The new texture was explained by the use of the theory of disclinations developed for thermotropic liquid crystals, specially for cholesteric type. (M.J.C.) [pt

  4. Determination of solid fat content by NMR

    International Nuclear Information System (INIS)

    Kawada, Tsukasa; Kato, Chihiro; Suzuki, Kazuaki

    1984-01-01

    To establish a standard method for determing solid fat content, the NMR method was tested at six laboratories and the results were examined for collaboration. Two types of instruments, pulse NMR and wide-line NMR were used. Standard deviation in results at six laboratories was less than 1.5 for the step wise method, but more than 1.5 for the rapid method. The standard deviation in results at a single laboratory was much less than either of these cases. No significant difference could be observed in the values obtained using both instruments. Solid fat content values measured for a mixture of fully hydrogenated rapeseed and rapeseed oil agreed well with the percentage of solid by weight. (author)

  5. Muscular pathology: echographic and NMR imaging aspects

    International Nuclear Information System (INIS)

    Pascal-Suisse, P.; Beaurain, P.; Mougniot, C.

    1995-01-01

    A comparison of echographic techniques and NMR imaging has been done for the diagnosis of muscular trauma and tumor pathologies. In traumatic pathology, the echographic analysis allows to determine the complete assessment of recent muscular injuries. NMR imaging can be used in granuloma or fibrous callosity appreciation and for the analysis of deep injury (muscles and muscles-tendon junctions) and of muscular aponeurosis. Echography must be used together with color coding Doppler technique in the diagnosis of tumor pathology and for the study of slow fluxes. The recently available energy Doppler technique seems to be powerful in the study of vascularization of small expansive formations, but their extension to adjacent bone or tissue can only be appreciated using NMR imaging. (J.S.)

  6. XRD, TEM, IR, Raman and NMR Spectroscopy of In Situ Crystallization of Lithium Disilicate Glass

    Science.gov (United States)

    Fuss, T.; Mogus-Milankovic, A.; Ray, C. S.; Lesher, C. E.; Youngman, R.; Day, D. E.

    2006-01-01

    The structure of a Li2O-2SiO2 (LS2) glass was investigated as a function of pressure and temperature up to 6 GPa and 750 C respectively, using XRD, TEM, IR, Raman and NMR spectroscopy. Glass densified at 6 GPa has an average Si-O-Si bond angle approx.7deg lower than that found in glass processed at 4.5 GPa. At 4.5 GPa, lithium disilicate crystallizes from the glass, while at 6 GPa a new high pressure form of lithium metasilicate crystallizes. The new phase, while having lithium metasilicate crystal symmetry, contains at least 4 different Si sites. NMR results for 6 GPa sample indicate the presence of Q4 species with (Q(sup 4))Si-O-Si(Q(sup 4)) bond angles of approx.157deg. This is the first reported occurrence of Q(sup 4) species with such large bond angles in alumina free alkali silicate glass. No five- or six- coordinated Si are found.

  7. REDOR NMR of stable-isotope-labeled protein binding sites

    Energy Technology Data Exchange (ETDEWEB)

    Schaefer, J. [Washington Univ., St. Louis, MO (United States)

    1994-12-01

    Rotational-echo, double resonance (REDOR) NMR, a new analytical spectroscopic technique for solids spinning at the magic angle, has been developed over the last 5 years. REDOR provides a direct measure of heteronuclear dipolar coupling between isolated pairs of labeled nuclei. In a solid with a {sup 13}C-{sup 15}N labeled pair, for example, the {sup 13}C rotational echoes that form each rotor period following a{sup 1}H-{sup 13}C cross-polarization transfer can be prevented from reaching full intensity by insertion of a {sup 15}N {pi} pulse each half rotor period. The REDOR difference (the difference between a {sup 13}C NMR spectrum obtained under these conditions and one obtained with no {sup 15}N {pi} pulses) has a strong dependence on the {sup 13}C-{sup 15}N dipolar coupling, and hence, the {sup 13}C-{sup 15}N internuclear distance. REDOR is described as double-resonance even though three radio frequencies (typically {sup 1}H, {sup 13}C, and {sup 15}N) are used because the protons are removed from the important evolution part of the experiment by resonant decoupling. The dephasing of magnetization in REDOR arises from a local dipolar {sup 13}C-{sup 15}N field gradient and involves no polarization transfer. REDOR has no dependence on {sup 13}C or {sup 15}N chemical-shift tensors and does not require resolution of a {sup 13}C-{sup 15}N coupling in the chemical-shift dimension.

  8. Contact replacement for NMR resonance assignment.

    Science.gov (United States)

    Xiong, Fei; Pandurangan, Gopal; Bailey-Kellogg, Chris

    2008-07-01

    Complementing its traditional role in structural studies of proteins, nuclear magnetic resonance (NMR) spectroscopy is playing an increasingly important role in functional studies. NMR dynamics experiments characterize motions involved in target recognition, ligand binding, etc., while NMR chemical shift perturbation experiments identify and localize protein-protein and protein-ligand interactions. The key bottleneck in these studies is to determine the backbone resonance assignment, which allows spectral peaks to be mapped to specific atoms. This article develops a novel approach to address that bottleneck, exploiting an available X-ray structure or homology model to assign the entire backbone from a set of relatively fast and cheap NMR experiments. We formulate contact replacement for resonance assignment as the problem of computing correspondences between a contact graph representing the structure and an NMR graph representing the data; the NMR graph is a significantly corrupted, ambiguous version of the contact graph. We first show that by combining connectivity and amino acid type information, and exploiting the random structure of the noise, one can provably determine unique correspondences in polynomial time with high probability, even in the presence of significant noise (a constant number of noisy edges per vertex). We then detail an efficient randomized algorithm and show that, over a variety of experimental and synthetic datasets, it is robust to typical levels of structural variation (1-2 AA), noise (250-600%) and missings (10-40%). Our algorithm achieves very good overall assignment accuracy, above 80% in alpha-helices, 70% in beta-sheets and 60% in loop regions. Our contact replacement algorithm is implemented in platform-independent Python code. The software can be freely obtained for academic use by request from the authors.

  9. Prediction of peak overlap in NMR spectra

    International Nuclear Information System (INIS)

    Hefke, Frederik; Schmucki, Roland; Güntert, Peter

    2013-01-01

    Peak overlap is one of the major factors complicating the analysis of biomolecular NMR spectra. We present a general method for predicting the extent of peak overlap in multidimensional NMR spectra and its validation using both, experimental data sets and Monte Carlo simulation. The method is based on knowledge of the magnetization transfer pathways of the NMR experiments and chemical shift statistics from the Biological Magnetic Resonance Data Bank. Assuming a normal distribution with characteristic mean value and standard deviation for the chemical shift of each observable atom, an analytic expression was derived for the expected overlap probability of the cross peaks. The analytical approach was verified to agree with the average peak overlap in a large number of individual peak lists simulated using the same chemical shift statistics. The method was applied to eight proteins, including an intrinsically disordered one, for which the prediction results could be compared with the actual overlap based on the experimentally measured chemical shifts. The extent of overlap predicted using only statistical chemical shift information was in good agreement with the overlap that was observed when the measured shifts were used in the virtual spectrum, except for the intrinsically disordered protein. Since the spectral complexity of a protein NMR spectrum is a crucial factor for protein structure determination, analytical overlap prediction can be used to identify potentially difficult proteins before conducting NMR experiments. Overlap predictions can be tailored to particular classes of proteins by preparing statistics from corresponding protein databases. The method is also suitable for optimizing recording parameters and labeling schemes for NMR experiments and improving the reliability of automated spectra analysis and protein structure determination.

  10. Synergistic effect of the simultaneous chemometric analysis of {sup 1}H NMR spectroscopic and stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data: Application to wine analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monakhova, Yulia B., E-mail: yul-monakhova@mail.ru [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, Saratov 410012 (Russian Federation); Godelmann, Rolf [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Hermann, Armin [Landesuntersuchungsamt -Institut für Lebensmittelchemie und Arzneimittelprüfung, Emy-Roeder-Straße 1, Mainz 55129 (Germany); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Cannet, Claire; Schäfer, Hartmut; Spraul, Manfred [Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Rutledge, Douglas N. [AgroParisTech, UMR 1145, Ingénierie Procédés Aliments, 16 rue Claude Bernard, Paris F-75005 (France)

    2014-06-23

    Highlights: • {sup 1}H NMR profilings of 718 wines were fused with stable isotope analysis data (SNIF-NMR, {sup 18}O, {sup 13}C). • The best improvement was obtained for prediction of the geographical origin of wine. • Certain enhancement was also obtained for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data). • Independent component analysis was used as an alternative chemometric tool for classification. - Abstract: It is known that {sup 1}H NMR spectroscopy represents a good tool for predicting the grape variety, the geographical origin, and the year of vintage of wine. In the present study we have shown that classification models can be improved when {sup 1}H NMR profiles are fused with stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data. Variable selection based on clustering of latent variables was performed on {sup 1}H NMR data. Afterwards, the combined data of 718 wine samples from Germany were analyzed using linear discriminant analysis (LDA), partial least squares-discriminant analysis (PLS-DA), factorial discriminant analysis (FDA) and independent components analysis (ICA). Moreover, several specialized multiblock methods (common components and specific weights analysis (ComDim), consensus PCA and consensus PLS-DA) were applied to the data. The best improvement in comparison with {sup 1}H NMR data was obtained for prediction of the geographical origin (up to 100% for the fused data, whereas stable isotope data resulted only in 60–70% correct prediction and {sup 1}H NMR data alone in 82–89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of {sup 1}H NMR data with stable isotope data improves efficiency of classification models for geographical origin and vintage of wine and can be potentially used for other food products as well.

  11. Applications of NMR spectroscopy to xenobiotic metabolism

    International Nuclear Information System (INIS)

    Harris, T.M.

    1989-01-01

    Recent years have seen high field NMR spectrometers become commonplace in research laboratories. At the same time, major advances in methodology for structural analysis have occurred, particularly notable among these being the development of two-dimensional spectroscopic techniques. Many applications have been made of NMR spectroscopy in the study of xenobiotic metabolic processes. This deals with two specific applications which have been made in the author's laboratory and involve mechanistic studies of the reactions of the carcinogens ethylene dibromide and aflatoxin with DNA

  12. Tritiation methods and tritium NMR spectroscopy

    International Nuclear Information System (INIS)

    Jaiswal, D.K.; Morimoto, H.; Salijoughian, M.; Williams, P.G.

    1991-09-01

    We have used a simple process for the production of highly tritiated water and characterized the product species by 1 H and 3 H NMR spectroscopy. The water is readily manipulated and used in subsequent reactions either as T 2 O, CH 3 COOT or CF 3 COOT. Development of tritiated diimide has progressed to the point where cis-hydrogenated products at 1-20 Ci/mmole S.A. are possible. Tri-n-butyl tin tritide has been produced at >95% tritium content and well characterized by multinuclear NMR techniques. 27 refs., 3 figs

  13. Applications of NMR in biological metabolic research

    International Nuclear Information System (INIS)

    Nie Jiarui; Li Xiuqin; He Chunjian

    1989-01-01

    The nuclear magnetic resonance has become a powerful means of studying biological metabolism in non-invasive and non-destructive way. Being used to study the metabolic processes of living system in normal physiological conditions as well as in molecular level, the method is better than other conventional approaches. Using important parameters such as NMR-chemical shifts, longitudinal relaxation time and transverse relaxation time, it is possible to probe the metabolic processes as well as conformation, concentration, transportation and distribution of reacting and resulting substances. The NMR spectroscopy of 1 H, 31 P and 13 C nuclei has already been widely used in metabolic researches

  14. Deuteron NMR and modelling in solid polymers

    International Nuclear Information System (INIS)

    Hirschinger, J.

    1992-01-01

    Deuteron NMR techniques are described and some recent applications to the study of rotational motions in solid polymers are reviewed. The information content and the domain of applicability of each technique are presented. Ultra-slow motions are studied in real time without any motional model consideration. For very fast motions, computer molecular dynamics simulations are shown to complement the NMR results. Experimental examples deal with the chain motion in the crystalline α-phase of poly(vinylidenefluoride) and nylon 6,6

  15. Programmable pulse series generator for NMR relaxometer

    International Nuclear Information System (INIS)

    Stolbunov, R.N.; Chichikov, S.A.; Lundin, A.G.

    2005-01-01

    Paper describes a pulse series generator for NMR relaxometer. The operation mode is set on the basis of the PC program by the PCI bus in the internal memory. The design is based on two Altera Company MAX7000S and Cyclone family microcircuits using the Qartus II 4.0 software. The basic parameters are as follows: pulse minimum length - 50 ns, time resolution - 10 ns, pulse maximum number - 1024, number of controlled output channels - 8. The designed device as a part of the NMR hardware-software system enables to record, to process and to store the experiment results in the form of electronic document [ru

  16. NMR relaxation times of natural rubber latex

    International Nuclear Information System (INIS)

    Harun, S.; Aziz, H.; Basir, Z.

    1994-01-01

    NMR relaxation times T sub 1 and T sub 2 of natural rubber latex have been measured at 25 degree C on a pulsed NMR spectrometer. The work focuses on the variation of the relaxation times with the amount of water content from 0% to 50%. The water content was adjusted by centrifuging and removing a certain amount of water from the sample. The data were analysed using a biexponential fitting procedure which yields simultaneously either T sub 1a and T sub 1b or T sub 2a and T sub 2b. The amount of solid was compared with the known amount of dry rubber content

  17. 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

  18. Solution structure of the 3'-5' cyclic dinucleotide d. A combined NMR, UV melting, and molecular mechanics study

    International Nuclear Information System (INIS)

    Blommers, M.J.J.; Haasnoot, C.A.G.; Walters, J.A.L.I.; van der Marel, G.A.; van Boom, J.H.; Hilbers, C.W.

    1988-01-01

    The 3'-5' cyclic dinucleotide d 1 H and 13 C NMR experiments, UV-melting experiments, and molecular mechanics calculations. The 1 H and 13 C NMR spectra were analyzed by means of 2-dimensional NMR experiments. J-Coupling analysis of the 1D and 2D 1 H and 13 C spectra was used to determine the conformation of the ring systems in the molecule. It appeared that at low temperature (283 K) the deoxyribose sugars adopt a N-type conformation. The geometry is best described by an intermediate between the 3 2 T and 3 E forms. In addition, the authors were able to derive all other torsion angles in the phosphate backbone ring system, i.e., α + , β/sup t/, γ + , δ (=89/degrees/), ε/sup t/ and /zeta/ + . When the molecule is subjected to an energy minimization procedure (using the program AMBER), the sugar ring system retains, practically speaking, the torsion angles found from the NMR experiments, while the torsion angles around the glycosidic bond adopt a value of 175/degrees/ in the minimum energy conformation. UV-melting experiments indicate that two molecules can form a dimer in which the adenine bases are intercalated. The feasibility of this structure is indicated by molecular mechanics calculations. At higher temperatures the dimer is converted into separate monomers. In the monomer form the sugars exhibit S-pucker 20% of the time. Concomitantly with the conversion of the N- to the S-conformation, the torsion angles α and γ change

  19. 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)

  20. A portable Halbach magnet that can be opened and closed without force: the NMR-CUFF.

    Science.gov (United States)

    Windt, Carel W; Soltner, Helmut; van Dusschoten, Dagmar; Blümler, Peter

    2011-01-01

    Portable equipment for nuclear magnetic resonance (NMR) is becoming increasingly attractive for use in a variety of applications. One of the main scientific challenges in making NMR portable is the design of light-weight magnets that possess a strong and homogeneous field. Existing NMR magnets can provide such magnetic fields, but only for small samples or in small regions, or are rather heavy. Here we show a simple yet elegant concept for a Halbach-type permanent magnet ring, which can be opened and closed with minimal mechanical force. An analytical solution for an ideal Halbach magnet shows that the magnetic forces cancel if the structure is opened at an angle of 35.3° relative to its poles. A first prototype weighed only 3.1 kg, and provided a flux density of 0.57 T with a homogeneity better than 200 ppm over a spherical volume of 5mm in diameter without shimming. The force needed to close it was found to be about 20 N. As a demonstration, intact plants were imaged and water (xylem) flow measured. Magnets of this type (NMR-CUFF = Cut-open, Uniform, Force Free) are ideal for portable use and are eminently suited to investigate small or slender objects that are part of a larger or immobile whole, such as branches on a tree, growing fruit on a plant, or non-metallic tubing in industrial installations. This new concept in permanent-magnet design enables the construction of openable, yet strong and homogeneous magnets, which aside from use in NMR or MRI could also be of interest for applications in accelerators, motors, or magnetic bearings. Copyright © 2010 Elsevier Inc. All rights reserved.

  1. Crystallinity and compositional changes in carbonated apatites: Evidence from 31P solid-state NMR, Raman, and AFM analysis

    Science.gov (United States)

    McElderry, John-David P.; Zhu, Peizhi; Mroue, Kamal H.; Xu, Jiadi; Pavan, Barbara; Fang, Ming; Zhao, Guisheng; McNerny, Erin; Kohn, David H.; Franceschi, Renny T.; Holl, Mark M. Banaszak; Tecklenburg, Mary M. J.; Ramamoorthy, Ayyalusamy; Morris, Michael D.

    2013-10-01

    Solid-state (magic-angle spinning) NMR spectroscopy is a useful tool for obtaining structural information on bone organic and mineral components and synthetic model minerals at the atomic-level. Raman and 31P NMR spectral parameters were investigated in a series of synthetic B-type carbonated apatites (CAps). Inverse 31P NMR linewidth and inverse Raman PO43-ν1 bandwidth were both correlated with powder XRD c-axis crystallinity over the 0.3-10.3 wt% CO32- range investigated. Comparison with bone powder crystallinities showed agreement with values predicted by NMR and Raman calibration curves. Carbonate content was divided into two domains by the 31P NMR chemical shift frequency and the Raman phosphate ν1 band position. These parameters remain stable except for an abrupt transition at 6.5 wt% carbonate, a composition which corresponds to an average of one carbonate per unit cell. This near-binary distribution of spectroscopic properties was also found in AFM-measured particle sizes and Ca/P molar ratios by elemental analysis. We propose that this transition differentiates between two charge-balancing ion-loss mechanisms as measured by Ca/P ratios. These results define a criterion for spectroscopic characterization of B-type carbonate substitution in apatitic minerals.

  2. Contact angles on stretched solids

    Science.gov (United States)

    Mensink, Liz; Snoeijer, Jacco

    2017-11-01

    The surface energy of solid interfaces plays a central role in wetting, as they dictate the liquid contact angle. Yet, it has been challenging to measure the solid surface energies independently, without making use of Young's law. Here we present Molecular Dynamics (MD) simulations by which we measure the surface properties for all interfaces, including the solids. We observe change in contact angles upon stretching the solid substrates, showing that the surface energy is actually strain dependent. This is clear evidence of the so-called Shuttleworth effect, making it necessary to distinguish surface energy from surface tension. We discuss how this effect gives rise to a new class of elasto-capillary phenomena. ERC Consolidator Grant No. 616918.

  3. Disorders of the cerebellopontine angle

    International Nuclear Information System (INIS)

    Block, F.

    2006-01-01

    Disorders of the cerebellopontine angle may present by symptoms like vertigo, hearing problems, affection of the trigeminal or facial nerve. Ipsilateral ataxia and contralateral hemiparesis develop in case of a rather large tumor in this region and display an involvement of the cerebellum and/or brainstem. However, some of these typical symptoms are not recognized by the patient. Thus, in case of a suspicion of a disorder of the cerebellopontine angle the relevant functions have to be tested clinically. In addition, electrophysiology can confirm dysfunction of these cranial nerves. Mainstay of the therapy should be the treatment of the underlying cause. Nevertheless, not seldom it is necessary to treat symptoms like vertigo or facial pain. (orig.) [de

  4. Measurement of the angle gamma

    International Nuclear Information System (INIS)

    Aleksan, R.; Kayser, B.; Sphicas, P.

    1993-01-01

    The angle γ at least as defined in the Wolfenstein approximation is not completely out of reach of current or proposed dedicated B experiments. This conclusion certainly depends crucially on the assumed trigger and tagging efficiencies and also on the expected backgrounds. The work summarized here represents but a first step in the direction of extracting the third angle of the unitarity triangle. The theoretical developments during the workshop have resulted in a clearer understanding of the quantities studied. On the experimental side, new decay modes (i.e. in addition to the traditional ρK s decay) have resulted in expections for observing CP violation in B s decays which are not unreasonable. It is conceivable that a dedicated B experiment can probe a fundamental aspect of the Standard Model, the CKM matrix, in multiple ways. In the process, new physics can appear anywhere along the line

  5. Inter-tetrahedra bond angle of permanently densified silicas extracted from their Raman spectra

    International Nuclear Information System (INIS)

    Hehlen, B

    2010-01-01

    Relative Raman scattering intensities are obtained in three samples of vitreous silica of increasing density. The variation of the intensity upon densification is very different for bending and stretching modes. For the former we find a Raman coupling-to-light coefficient C B ∝ω 2 . A comparative intensity and frequency dependence of the Raman spectral lines in the three glasses is performed. Provided the Raman spectra are normalized by C B , there exists a simple relation between the Si-O-Si bond angle and the frequency of all O-bending motions, including those of fourfold (n = 4) and threefold (n = 3) rings. For 20% densification we find a reduction of ∼5.7 deg. of the maximum of the network angle distribution, a value in very close agreement with previous NMR experiments. The threefold and fourfold rings are weakly perturbed by the densification, with a bond angle reduction of ∼0.5 deg. for the former.

  6. [Anatomy of fractures of the inferior scapular angle].

    Science.gov (United States)

    Bartoníček, J; Tuček, M; Malík, J

    2018-01-01

    The aim of this study is to describe the anatomy of fractures of the inferior angle and the adjacent part of the scapular body, based on 3D CT reconstructions. In a series of 375 scapular fractures, we identified a total of 20 fractures of the inferior angle of the scapular body (13 men, 7 women), with a mean patient age of 50 years (range 3373). In all fractures, 3D CT reconstructions were obtained, allowing an objective evaluation of the fracture pattern with a focus on the size and shape of the inferior angle fragment, propagation of the fracture line to the lateral and medial borders of the infraspinous part of the scapular body, fragment displacement and any additional fracture of the ipsilateral scapula and the shoulder girdle. We identified a total of 5 types of fracture involving the distal half of the infraspinous part of the scapular body. The first type, recorded in 5 cases, affected only the apex of the inferior angle, with a small part of the adjacent medial border. The second type, occurring in 4 cases, involved fractures separating the entire inferior angle. The third type, represented by 4 cases, was characterized by a fracture line starting medially close above the inferior angle and passing proximolaterally. The separated fragment had a shape of a big drop, carrying also the distal half of the lateral pillar in addition to the inferior angle. In the fourth type identified in 5 fractures, the separated fragment was formed both by the inferior angle and a variable part of the medial border. The fifth type, being by its nature a transition to the fracture of the infraspinous part of the body, was recorded in 2 cases, with the same V-shaped fragment. Fractures of the inferior angle and the adjacent part of the scapular body are groups of fractures differing from other infraspinous fractures of the scapular body. Although these fractures are highly variable in terms of shape, they have the same course of fracture line and the manner of displacement

  7. LHC Report: playing with angles

    CERN Multimedia

    Mike Lamont for the LHC team

    2016-01-01

    Ready (after a machine development period), steady (running), go (for a special run)!   The crossing angles are an essential feature of the machine set-up. They have to be big enough to reduce the long-range beam-beam effect. The LHC has recently enjoyed a period of steady running and managed to set a new record for “Maximum Stable Luminosity Delivered in 7 days” of 3.29 fb-1 between 29 August and 4 September. The number of bunches per beam remains pegged at 2220 because of the limitations imposed by the SPS beam dump. The bunch population is also somewhat reduced due to outgassing near one of the injection kickers at point 8. Both limitations will be addressed during the year-end technical stop, opening the way for increased performance in 2017. On 10 and 11 September, a two day machine development (MD) period took place. The MD programme included a look at the possibility of reducing the crossing angle at the high-luminosity interaction points. The crossing angles are an ess...

  8. Light Scattering at Various Angles

    Science.gov (United States)

    Latimer, Paul; Pyle, B. E.

    1972-01-01

    The Mie theory of scattering is used to provide new information on how changes in particle volume, with no change in dry weight, should influence light scattering for various scattering angles and particle sizes. Many biological cells (e.g., algal cells, erythrocytes) and large subcellular structures (e.g., chloroplasts, mitochondria) in suspension undergo this type of reversible volume change, a change which is related to changes in the rates of cellular processes. A previous study examined the effects of such volume changes on total scattering. In this paper scattering at 10° is found to follow total scattering closely, but scattering at 45°, 90°, 135°, and 170° behaves differently. Small volume changes can cause very large observable changes in large angle scattering if the sample particles are uniform in size; however, the natural particle size heterogeneity of most samples would mask this effect. For heterogeneous samples of most particle size ranges, particle shrink-age is found to increase large angle scattering. PMID:4556610

  9. Angle comparison using an autocollimator

    Science.gov (United States)

    Geckeler, Ralf D.; Just, Andreas; Vasilev, Valentin; Prieto, Emilio; Dvorácek, František; Zelenika, Slobodan; Przybylska, Joanna; Duta, Alexandru; Victorov, Ilya; Pisani, Marco; Saraiva, Fernanda; Salgado, Jose-Antonio; Gao, Sitian; Anusorn, Tonmueanwai; Leng Tan, Siew; Cox, Peter; Watanabe, Tsukasa; Lewis, Andrew; Chaudhary, K. P.; Thalmann, Ruedi; Banreti, Edit; Nurul, Alfiyati; Fira, Roman; Yandayan, Tanfer; Chekirda, Konstantin; Bergmans, Rob; Lassila, Antti

    2018-01-01

    Autocollimators are versatile optical devices for the contactless measurement of the tilt angles of reflecting surfaces. An international key comparison (KC) on autocollimator calibration, EURAMET.L-K3.2009, was initiated by the European Association of National Metrology Institutes (EURAMET) to provide information on the capabilities in this field. The Physikalisch-Technische Bundesanstalt (PTB) acted as the pilot laboratory, with a total of 25 international participants from EURAMET and from the Asia Pacific Metrology Programme (APMP) providing measurements. This KC was the first one to utilise a high-resolution electronic autocollimator as a standard. In contrast to KCs in angle metrology which usually involve the full plane angle, it focused on relatively small angular ranges (+/-10 arcsec and +/-1000 arcsec) and step sizes (10 arcsec and 0.1 arcsec, respectively). This document represents the approved final report on the results of the KC. Main text To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database kcdb.bipm.org/. The final report has been peer-reviewed and approved for publication by the CCL, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).

  10. Recommendations of the wwPDB NMR Validation Task Force

    Science.gov (United States)

    Montelione, Gaetano T.; Nilges, Michael; Bax, Ad; Güntert, Peter; Herrmann, Torsten; Richardson, Jane S.; Schwieters, Charles; Vranken, Wim F.; Vuister, Geerten W.; Wishart, David S.; Berman, Helen M.; Kleywegt, Gerard J.; Markley, John L.

    2013-01-01

    As methods for analysis of biomolecular structure and dynamics using nuclear magnetic resonance spectroscopy (NMR) continue to advance, the resulting 3D structures, chemical shifts, and other NMR data are broadly impacting biology, chemistry, and medicine. Structure model assessment is a critical area of NMR methods development, and is an essential component of the process of making these structures accessible and useful to the wider scientific community. For these reasons, the Worldwide Protein Data Bank (wwPDB) has convened an NMR Validation Task Force (NMR-VTF) to work with the wwPDB partners in developing metrics and policies for biomolecular NMR data harvesting, structure representation, and structure quality assessment. This paper summarizes the recommendations of the NMR-VTF, and lays the groundwork for future work in developing standards and metrics for biomolecular NMR structure quality assessment. PMID:24010715

  11. nmrML: A Community Supported Open Data Standard for the Description, Storage, and Exchange of NMR Data.

    Science.gov (United States)

    Schober, Daniel; Jacob, Daniel; Wilson, Michael; Cruz, Joseph A; Marcu, Ana; Grant, Jason R; Moing, Annick; Deborde, Catherine; de Figueiredo, Luis F; Haug, Kenneth; Rocca-Serra, Philippe; Easton, John; Ebbels, Timothy M D; Hao, Jie; Ludwig, Christian; Günther, Ulrich L; Rosato, Antonio; Klein, Matthias S; Lewis, Ian A; Luchinat, Claudio; Jones, Andrew R; Grauslys, Arturas; Larralde, Martin; Yokochi, Masashi; Kobayashi, Naohiro; Porzel, Andrea; Griffin, Julian L; Viant, Mark R; Wishart, David S; Steinbeck, Christoph; Salek, Reza M; Neumann, Steffen

    2018-01-02

    NMR is a widely used analytical technique with a growing number of repositories available. As a result, demands for a vendor-agnostic, open data format for long-term archiving of NMR data have emerged with the aim to ease and encourage sharing, comparison, and reuse of NMR data. Here we present nmrML, an open XML-based exchange and storage format for NMR spectral data. The nmrML format is intended to be fully compatible with existing NMR data for chemical, biochemical, and metabolomics experiments. nmrML can capture raw NMR data, spectral data acquisition parameters, and where available spectral metadata, such as chemical structures associated with spectral assignments. The nmrML format is compatible with pure-compound NMR data for reference spectral libraries as well as NMR data from complex biomixtures, i.e., metabolomics experiments. To facilitate format conversions, we provide nmrML converters for Bruker, JEOL and Agilent/Varian vendor formats. In addition, easy-to-use Web-based spectral viewing, processing, and spectral assignment tools that read and write nmrML have been developed. Software libraries and Web services for data validation are available for tool developers and end-users. The nmrML format has already been adopted for capturing and disseminating NMR data for small molecules by several open source data processing tools and metabolomics reference spectral libraries, e.g., serving as storage format for the MetaboLights data repository. The nmrML open access data standard has been endorsed by the Metabolomics Standards Initiative (MSI), and we here encourage user participation and feedback to increase usability and make it a successful standard.

  12. NMR chemical shifts in amino acids: Effects of environments, electric field, and amine group rotation

    International Nuclear Information System (INIS)

    Yoon, Young-Gui; Pfrommer, Bernd G.; Louie, Steven G.; Canning, Andrew

    2002-01-01

    The authors present calculations of NMR chemical shifts in crystalline phases of some representative amino acids such as glycine, alanine, and alanyl-alanine. To get an insight on how different environments affect the chemical shifts, they study the transition from the crystalline phase to completely isolated molecules of glycine. In the crystalline limit, the shifts are dominated by intermolecular hydrogen-bonds. In the molecular limit, however, dipole electric field effects dominate the behavior of the chemical shifts. They show that it is necessary to average the chemical shifts in glycine over geometries. Tensor components are analyzed to get the angle dependent proton chemical shifts, which is a more refined characterization method

  13. Poling effects on anisotropic temperature changes in NMR second moments of drawn PVDF films

    International Nuclear Information System (INIS)

    Ishii, Fumiaki; Sawatari, Takanori; Odajima, Akira

    1982-01-01

    For the drawn PVDF film, the NMR second moment vs temperature curves at 0 0 and 90 0 of the alignment angle (γ) cross over each other during the motional narrowing in the Tsub(g) region (-- -50 0 C). On poling, however, they decrease almost in parallel up to -20 0 C and show another narrowing above 30 0 C depending strongly on γ. These findings indicate that the molecular chain is oriented in the non-crystalline region and the poling more clearly separates low orientations from high orientations. The increase in the high orientation part should be attributed to polarization in the oriented non-crystalline region. (author)

  14. Effect of stifle angle on the magnitude of the tibial plateau angle measurement in dogs with intact and transected cranial cruciate ligament. A cadaveric study.

    Science.gov (United States)

    Aulakh, K S; Harper, T A M; Lanz, O I; Daniel, G B; Werre, S R

    2011-01-01

    To determine the effect of stifle angle on the magnitude of the radiographic tibial plateau angle (TPA) in normal and cranial cruciate ligament (CCL) -deficient stifles. Three pairs of canine cadaver hindlimbs from three skeletally mature dogs were positioned in a custom-made positioning device. A lateral radiograph of each specimen was obtained before and after transection of the CCL at four stifle angles (90°, 110°, 135° and 140-150° [i.e. maximum extension]), based on goniometric measurements. Four observers determined the radiographic TPA twice for each radiograph with a minimum of two days between each measurement. The radiographic TPA measurements in all specimens at different stifle angles with intact CCL and transected CCL were compared with mixed-model ANOVA. The effect of stifle angle, CCL transection, and interaction between the two on observer TPA measurement variability was also determined using the coefficient of variation. Tibial plateau angle was not statistically different in the stifle angles for either the intact or transected CCL. There was also no statistical difference for TPA between intact and transected CCL groups at each of the stifle angles. Stifle angle, CCL transection and interaction between the two did not have any significant effect for intra-observer and inter-observer variation. The angle of the stifle during radiography does not influence the magnitude of the TPA measurement as determined on true lateral radiographs of the stifle and tibia in cadaveric canine limbs.

  15. Software Library for Bruker TopSpin NMR Data Files

    Energy Technology Data Exchange (ETDEWEB)

    2016-10-14

    A software library for parsing and manipulating frequency-domain data files that have been processed using the Bruker TopSpin NMR software package. In the context of NMR, the term "processed" indicates that the end-user of the Bruker TopSpin NMR software package has (a) Fourier transformed the raw, time-domain data (the Free Induction Decay) into the frequency-domain and (b) has extracted the list of NMR peaks.

  16. NMR imaging of the cardiovascular system

    International Nuclear Information System (INIS)

    Canby, R.C.; Evanochko, W.T.; Pohost, G.M.

    1986-01-01

    Proton nuclear magnetic resonance (NMR) imaging permits high-resolution tomographic and three-dimensional images of the human body to be obtained without exposure to ionizing radiation. Such imaging not only yields anatomic resolution comparable to X-ray examinations but also provides a potential means to discriminate between healthy tissue and diseased tissue. This potential is based on certain NMR properties known as relaxation times, which determine, in part, the signal intensity in an image. These properties are related to such factors as the sizes and concentrations of proteins and mobile lipids and the compartmentalization of the protons of water. Although NMR imaging (also called magnetic resonance imaging, MRI) is becoming widely available for clinical use, application to the cardiovascular system, though promising, remains primarily a research tool. Gated proton NMR imaging can generate cardiac images with excellent morphologic detail and contrast; however, its ultimate importance as a cardiovascular diagnostic modality will depend on the development of several unique applications. These applications are discussed in this paper

  17. NMR imaging of the musculoskeletal system

    International Nuclear Information System (INIS)

    Naegele, M.; Lienemann, A.; Hahn, D.

    1988-01-01

    NMR imaging now allows in vivo imaging of soft tissue hitherto undetectable by non-invasive means. This opens up excellent perspectives with regard to the diagnosis and therapy of various diseases in the field of traumatology and oncology, of which examples are discussed in this paper. (orig.) [de

  18. Fourier transform zero field NMR and NQR

    International Nuclear Information System (INIS)

    Zax, D.B.

    1985-01-01

    In many systems the chemical shifts measured by traditional high resolution solid state NMR methods are insufficiently sensitive, or the information contained in the dipole-dipole couplings is more important. In these cases, Fourier transform zero field magnetic resonance may make an important contribution. Zero field NMR and NQR is the subject of this thesis. Chapter I presents the quantum mechanical background and notational formalism for what follows. Chapter II gives a brief review of high resolution magnetic resonance methods, with particular emphasis on techniques applicable to dipole-dipole and quadrupolar couplings. Level crossings between spin-1/2 and quadrupolar spins during demagnetization transfer polarization from high to low λ nuclei. This is the basis of very high sensitivity zero field NQR measurements by field cycling. Chapter III provides a formal presentation of the high resolution Fourier transform zero field NMR method. Theoretical signal functions are calculated for common spin systems, and examples of typical spectra are presented. Chapters IV and V review the experimental progress in zero field NMR of dipole-dipole coupled spin-1/2 nuclei and for quadrupolar spin systems. Variations of the simple experiment describe in earlier chapters that use pulsed dc fields are presented in Chapter VI

  19. NMR Analysis of Some Pentacycloundecanedione Derivatives

    African Journals Online (AJOL)

    NJD

    Although many authors have commented on the difficulty of ... coming these former difficulties. Cookson's dione 19,10 .... and 2.58 ppm) is the common factor and the positions of H-2. (2.94 ppm) .... Owing to advances in NMR technology, the.

  20. Proton NMR imaging in experimental ischemic infarction

    International Nuclear Information System (INIS)

    Buonanno, F.S.; Pykett, I.L.; Brady, T.J.; Vielma, J.; Burt, C.T.; Goldman, M.R.; Hinshaw, W.S.; Pohost, G.M.; Kistler, J.P.

    1983-01-01

    Proton nuclear magnetic resonance (NMR) images depict the distribution and concentration of mobile protons modified by the relaxation times T1 and T2. Using the steady-state-free-precession (SSFP) technique, serial coronal images were obtained sequentially over time in laboratory animals with experimental ischemic infarction. Image changes were evident as early as 2 hours after carotid artery ligation, and corresponded to areas of ischemic infarction noted pathologically. Resulting SSFP images in experimental stroke are contrasted to inversion-recovery NMR images in an illustrative patient with established cerebral infarction. Bulk T1 and T2 measurements were made in vitro in three groups of gerbils: normal, those with clinical evidence of infarction, and those clinically normal after carotid ligature. Infarcted hemispheres had significantly prolonged T1 and T2 (1.47 +/- .12 sec, 76.0 +/- 9.0 msec, respectively) when compared to the contralateral hemisphere (T1 . 1.28 +/- .05 sec, T2 . 58.7 +/- 3.9 msec) or to the other two groups. These data suggest that changes in NMR parameters occur and can be detected by NMR imaging as early as two hours after carotid artery ligation

  1. Hyperpolarized NMR Probes for Biological Assays

    Directory of Open Access Journals (Sweden)

    Sebastian Meier

    2014-01-01

    Full Text Available During the last decade, the development of nuclear spin polarization enhanced (hyperpolarized molecular probes has opened up new opportunities for studying the inner workings of living cells in real time. The hyperpolarized probes are produced ex situ, introduced into biological systems and detected with high sensitivity and contrast against background signals using high resolution NMR spectroscopy. A variety of natural, derivatized and designed hyperpolarized probes has emerged for diverse biological studies including assays of intracellular reaction progression, pathway kinetics, probe uptake and export, pH, redox state, reactive oxygen species, ion concentrations, drug efficacy or oncogenic signaling. These probes are readily used directly under natural conditions in biofluids and are often directly developed and optimized for cellular assays, thus leaving little doubt about their specificity and utility under biologically relevant conditions. Hyperpolarized molecular probes for biological NMR spectroscopy enable the unbiased detection of complex processes by virtue of the high spectral resolution, structural specificity and quantifiability of NMR signals. Here, we provide a survey of strategies used for the selection, design and use of hyperpolarized NMR probes in biological assays, and describe current limitations and developments.

  2. Structural Studies of Biological Solids Using NMR

    Science.gov (United States)

    Ramamoorthy, Ayyalusamy

    2011-03-01

    High-resolution structure and dynamics of biological molecules are important in understanding their function. While studies have been successful in solving the structures of water-soluble biomolecules, it has been proven difficult to determine the structures of membrane proteins and fibril systems. Recent studies have shown that solid-state NMR is a promising technique and could be highly valuable in studying such non-crystalline and non-soluble biosystems. I will present strategies to study the structures of such challenging systems and also about the applications of solid-state NMR to study the modes of membrane-peptide interactions for a better assessment of the prospects of antimicrobial peptides as substitutes to antibiotics in the control of human disease. Our studies on the mechanism of membrane disruption by LL-37 (a human antimicrobial peptide), analogs of the naturally occurring antimicrobial peptide magainin2 extracted from the skin of the African frog Xenopus Laevis, and pardaxin will be presented. Solid-state NMR experiments were used to determine the secondary structure, dynamics and topology of these peptides in lipid bilayers. Similarities and difference in the cell-lysing mechanism, and their dependence on the membrane composition, of these peptides will be discussed. Atomic-level resolution NMR structures of amyloidogenic proteins revealing the misfolding pathway and early intermediates that play key roles in amyloid toxicity will also be presented.

  3. Synthesis and NMR elucidation of novel pentacycloundecane ...

    African Journals Online (AJOL)

    NICO

    SYNTHESIS AND NMR ELUCIDATION OF NOVEL. PENTACYCLOUNDECANE DERIVED PEPTIDES. Rajshekhar Karpoormath, a. Oluseye K. Onajole, a. Thavendran Govender, b. Glenn E. M. Maguire, a and Hendrik G. Kruger a* a. School of Chemistry, University of KwaZulu-Natal, Durban 4001, South Africa b. School of ...

  4. The bar coil for NMR tomograph

    International Nuclear Information System (INIS)

    Bogorodzki, P.; Piatkowski, A.; Wasielewski, J.

    1995-01-01

    The bar coil (bi-planar) for the NMR tomograph, designed for medical diagnostics, has been described. The tests of coil shown that it generates good homogenous magnetic field in a big volume what results in improving of the signal-to-noise ratio

  5. NMR characterization of polymers: Review and update

    Science.gov (United States)

    NMR spectroscopy is a major technique for the characterization and analysis of polymers. A large number of methodologies have been developed in both the liquid and the solid state, and the literature has grown considerably (1-5). The field now covers a broad spectrum of activities, including polym...

  6. 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.)

  7. Structures of Biomolecules by NMR Spectroscopy

    Indian Academy of Sciences (India)

    IAS Admin

    an edge over the X-ray method as it can be used to study biomolecules ... currently as an Associate. Professor. ... Such a wealth of data is made available to the NMR ... important step towards structural characterization of a biomolecule. Box 1.

  8. NMR blood vessel imaging method and apparatus

    International Nuclear Information System (INIS)

    Riederer, S.J.

    1988-01-01

    A high speed method of forming computed images of blood vessels based on measurements of characteristics of a body is described comprising the steps of: subjecting a predetermined body area containing blood vessels of interest to, successively, applications of a short repetition time (TR) NMR pulse sequence during the period of high blood velocity and then to corresponding applications during the period of low blood velocity for successive heart beat cycles; weighting the collected imaging data from each application of the NMR pulse sequence according to whether the data was acquired during the period of high blood velocity or a period of low blood velocity of the corresponding heart beat cycle; accumulating weighted imaging data from a plurality of NMR pulse sequences corresponding to high blood velocity periods and from a plurality of NMR pulse sequences corresponding to low blood velocity periods; subtracting the weighted imaging data corresponding to each specific phase encoding acquired during the high blood velocity periods from the weighted imaging data for the same phase encoding corresponding to low blood velocity periods in order to compute blood vessel imaging data; and forming an image of the blood vessels of interest from the blood vessel imaging data

  9. 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.

  10. Recent Advances in Targeted and Untargeted Metabolomics by NMR and MS/NMR Methods

    Energy Technology Data Exchange (ETDEWEB)

    Bingol, Kerem

    2018-04-18

    Metabolomics has made significant progress in multiple fronts in the last 18 months. This minireview aimed to give an overview of these advancements in the light of their contribution to targeted and untargeted metabolomics. New computational approaches have emerged to overcome manual absolute quantitation step of metabolites in 1D 1H NMR spectra. This provides more consistency between inter-laboratory comparisons. Integration of 2D NMR metabolomics databases under a unified web server allowed very accurate identification of the metabolites that have been catalogued in these databases. For the remaining uncatalogued and unknown metabolites, new cheminformatics approaches have been developed by combining NMR and mass spectrometry. These hybrid NMR/MS approaches accelerated the identification of unknowns in untargeted studies, and now they are allowing to profile ever larger number of metabolites in application studies.

  11. Solid-state NMR spectroscopy on complex biomolecules

    NARCIS (Netherlands)

    Renault, M.A.M.; Cukkemane, A.A.; Baldus, M.

    2010-01-01

    Biomolecular applications of NMR spectroscopy are often merely associated with soluble molecules or magnetic resonance imaging. However, since the late 1970s, solid-state NMR (ssNMR) spectroscopy has demonstrated its ability to provide atomic-level insight into complex biomolecular systems ranging

  12. Polymeric proanthocyanidins 13C NMR studies of procyanidins

    Science.gov (United States)

    Lawrence J. Porter; Roger H. Newman; Lai Yeap Foo; Herbert Wong; Richard W. Hemingway

    1982-01-01

    Proanthocyanidin polymers have been shown to consist entirely of flavan-3-ol units by a combination of techniques including 13C n.m.r. spectroscopy. The 13C n.m.r. spectra of the polymers and related molecules are now considered in more detail. Prior to this study UC n.m.r. data has been published of procyanidins and...

  13. Crocus sativus Petals: Waste or Valuable Resource? The Answer of High-Resolution and High-Resolution Magic Angle Spinning Nuclear Magnetic Resonance.

    Science.gov (United States)

    Righi, Valeria; Parenti, Francesca; Tugnoli, Vitaliano; Schenetti, Luisa; Mucci, Adele

    2015-09-30

    Intact Crocus sativus petals were studied for the first time by high-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR) spectroscopy, revealing the presence of kinsenoside (2) and goodyeroside A (3), together with 3-hydroxy-γ-butyrolactone (4). These findings were confirmed by HR-NMR analysis of the ethanol extract of fresh petals and showed that, even though carried out rapidly, partial hydrolysis of glucopyranosyloxybutanolides occurs during extraction. On the other hand, kaempferol 3-O-sophoroside (1), which is "NMR-silent" in intact petals, is present in extracts. These results suggest to evaluate the utilization of saffron petals for phytopharmaceutical and nutraceutical purposes to exploit a waste product of massive production of commercial saffron and point to the application of HR-MAS NMR for monitoring bioactive compounds directly on intact petals, avoiding the extraction procedure and the consequent hydrolysis reaction.

  14. Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

    Energy Technology Data Exchange (ETDEWEB)

    Schot, Gijs van der [Uppsala University, Laboratory of Molecular Biophysics, Department of Cell and Molecular Biology (Sweden); Bonvin, Alexandre M. J. J., E-mail: a.m.j.j.bonvin@uu.nl [Utrecht University, Faculty of Science – Chemistry, Bijvoet Center for Biomolecular Research (Netherlands)

    2015-08-15

    We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665–1674, 2005b, doi: 10.1021/ja047109h 10.1021/ja047109h ). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27–35, 2013, doi: 10.1007/s10858-013-9762-6 10.1007/s10858-013-9762-6 ), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution.

  15. Performance of the WeNMR CS-Rosetta3 web server in CASD-NMR

    International Nuclear Information System (INIS)

    Schot, Gijs van der; Bonvin, Alexandre M. J. J.

    2015-01-01

    We present here the performance of the WeNMR CS-Rosetta3 web server in CASD-NMR, the critical assessment of automated structure determination by NMR. The CS-Rosetta server uses only chemical shifts for structure prediction, in combination, when available, with a post-scoring procedure based on unassigned NOE lists (Huang et al. in J Am Chem Soc 127:1665–1674, 2005b, doi: 10.1021/ja047109h 10.1021/ja047109h ). We compare the original submissions using a previous version of the server based on Rosetta version 2.6 with recalculated targets using the new R3FP fragment picker for fragment selection and implementing a new annotation of prediction reliability (van der Schot et al. in J Biomol NMR 57:27–35, 2013, doi: 10.1007/s10858-013-9762-6 10.1007/s10858-013-9762-6 ), both implemented in the CS-Rosetta3 WeNMR server. In this second round of CASD-NMR, the WeNMR CS-Rosetta server has demonstrated a much better performance than in the first round since only converged targets were submitted. Further, recalculation of all CASD-NMR targets using the new version of the server demonstrates that our new annotation of prediction quality is giving reliable results. Predictions annotated as weak are often found to provide useful models, but only for a fraction of the sequence, and should therefore only be used with caution

  16. Open angle glaucoma as a manifestation of Waardenburg′s syndrome.

    Directory of Open Access Journals (Sweden)

    Gupta Viney

    2000-01-01

    Full Text Available Waardenburg′s syndrome is a rare, autosomal dominant disorder, with several clinical signs, each with variable penetrance. We report this case of Waardenburg′s syndrome with bilateral open-angle glaucoma with unique gonioscopic findings.

  17. First NMR Experiments in the Hybrid, 40T and beyond: A challenge to traditional NMR instrumentation

    Science.gov (United States)

    Reyes, Arneil P.

    2001-03-01

    The recent commissioning of the continuous 45T hybrid magnet at NHMFL has opened new horizon for science but carried with it new challenges that forced NMR spectroscopists to reevaluate the traditional approach to NMR instrumentation. Very recently, a world record frequency at 1.5GHz has been achieved, signaling the new era of NMR probe designs that may someday blur the distinction between the classic NMR and millimeter-wave spectroscopies. No longer can we ignore stray capacitances and exposed leads in the terrain where every millimeter of cable counts. The challenge brought about by ever increasing fields and consequently, frequency, requirements has stimulated ingenuity among scientists. This is eased by accelerated growth in RF communications and computing technologies that made available advanced devices with more speed, power, bandwidth, noise immunity, flexibility, and complexity in small space at very low costs. Utilization of these devices have been paramount consideration in cutting-edge designs at NHMFL for Condensed Matter NMR and will be described in this talk. I will also discuss a number of first >33T NMR experiments to date utilizing the strength of the field to expose, as well as to induce occurrence of, new physical phenomena in condensed matter and which resulted in better understanding of the physics of materials. This work has been a result of continuing collaboration with P. L Kuhns, W. G. Moulton, W. P. Halperin (NU), and W. G. Clark (UCLA). The NHMFL is supported through the National Science Foundation and the State of Florida.

  18. Crystalline phase of sodium germanate system determined by x-ray diffraction and 23Na magic angle spinning nuclear magnetic resonance

    International Nuclear Information System (INIS)

    Hussin, R.; Holland, D.; Dupree, R.

    2000-01-01

    Crystalline products of sodium germanate glasses system with composition from 10 mol% to 50 mol% Na 2 O have been investigated using 23 Na magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy and x-ray diffraction (XRD). Fitting of the 23 Na NMR spectra of the crystalline phases concerning different crystallographically sodium atom in sodium germanate system are reasonably reproducible as observed by the spectra obtained. The line shape simulations of the 23 Na NMR spectra yielded NMR quadrupolar parameters such as nuclear quadrupole coupling constants (C Q ), asymmetry parameters (η), and isotropic chemical shifts (δ i ). 23 Na NMR isotropic chemical shift may also provide further information on the structural environment of the sodium atom. A simple correlation between structure and NMR parameters to be tested can be used to probe the structure of sodium germanate glasses. The experimental 23 Na chemical shifts correlate well with an empirical shift parameter based on the total oxygen-cation bond valence and Na-O distances of all oxygen atoms in the first coordination sphere of the sodium cation. In this study the different phases in the sodium germanate system were identified. These results show that 23 Na NMR can provide examples of the types of structural information for sodium germanate system. (Author)

  19. Small angle scattering and polymers

    International Nuclear Information System (INIS)

    Cotton, J.P.

    1996-01-01

    The determination of polymer structure is a problem of interest for both statistical physics and industrial applications. The average polymer structure is defined. Then, it is shown why small angle scattering, associated with isotopic substitution, is very well suited to the measurement of the chain conformation. The corresponding example is the old, but pedagogic, measurement of the chain form factor in the polymer melt. The powerful contrast variation method is illustrated by a recent determination of the concentration profile of a polymer interface. (author) 12 figs., 48 refs

  20. A Simple Approach for Obtaining High Resolution, High Sensitivity ¹H NMR Metabolite Spectra of Biofluids with Limited Mass Supply

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Rommereim, Donald N.; Wind, Robert A.; Minard, Kevin R.; Sears, Jesse A.

    2006-11-01

    A simple approach is reported that yields high resolution, high sensitivity ¹H NMR spectra of biofluids with limited mass supply. This is achieved by spinning a capillary sample tube containing a biofluid at the magic angle at a frequency of about 80Hz. A 2D pulse sequence called ¹H PASS is then used to produce a high-resolution ¹H NMR spectrum that is free from magnetic susceptibility induced line broadening. With this new approach a high resolution ¹H NMR spectrum of biofluids with a volume less than 1.0 µl can be easily achieved at a magnetic field strength as low as 7.05T. Furthermore, the methodology facilitates easy sample handling, i.e., the samples can be directly collected into inexpensive and disposable capillary tubes at the site of collection and subsequently used for NMR measurements. In addition, slow magic angle spinning improves magnetic field shimming and is especially suitable for high throughput investigations. In this paper first results are shown obtained in a magnetic field of 7.05T on urine samples collected from mice using a modified commercial NMR probe.