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Sample records for non-destructive magic angle

  1. 'Magic Angle Precession'

    SciTech Connect

    Binder, Bernd

    2008-01-21

    An advanced and exact geometric description of nonlinear precession dynamics modeling very accurately natural and artificial couplings showing Lorentz symmetry is derived. In the linear description it is usually ignored that the geometric phase of relativistic motion couples back to the orbital motion providing for a non-linear recursive precession dynamics. The high coupling strength in the nonlinear case is found to be a gravitomagnetic charge proportional to the precession angle and angular velocity generated by geometric phases, which are induced by high-speed relativistic rotations and are relevant to propulsion technologies but also to basic interactions. In the quantum range some magic precession angles indicating strong coupling in a phase-locked chaotic system are identified, emerging from a discrete time dynamical system known as the cosine map showing bifurcations at special precession angles relevant to heavy nuclei stability. The 'Magic Angle Precession' (MAP) dynamics can be simulated and visualized by cones rolling in or on each other, where the apex and precession angles are indexed by spin, charge or precession quantum numbers, and corresponding magic angles. The most extreme relativistic warping and twisting effect is given by the Dirac spinor half spin constellation with 'Hyperdiamond' MAP, which resembles quark confinement.

  2. Non-destructive microwave evaluation of TBC delamination induced by acute angle laser drilling

    NASA Astrophysics Data System (ADS)

    Sezer, H. K.; Li, Lin; Wu, Z.; Anderson, B.; Williams, P.

    2007-01-01

    Laser drilling has been applied to the production of cooling holes of various size and angles in the modern aerospace gas turbine components such as turbine blades, nozzle guide vanes, combustion chambers and afterburner. These parts are usually made of heat resistant nickel superalloys. The superalloy substrate is coated with yttria-stabilized zirconia thermal barrier coatings (TBCs) to protect them from reaching excessive temperatures in hot engine environments. Drilling the parts at acute angles to the surface is complicated because (i) multiple layers are being drilled through, (ii) the melt ejection and heat flow patterns around the hole are non-symmetrical and (iii) the drilling distance is greater than when drilling normal to the surface. In a previous investigation by the authors, delamination of TBC was addressed as a main problem of angled drilling and mechanisms involved were discussed. Characterization of delamination cracks was normally performed via metallographic techniques. It involves sectioning the samples using an abrasive cutting machine, grinding with successively finer silicon carbide paper up to the centre of the hole and polishing to allow optical microscopic analysis of the cracks. However, clamping and sectioning process of thermal-spray-coated workpieces can introduce cracks in brittle coatings due to the drag of the cut-off wheels. Hence, it is not possible to decide if the delamination is caused as a result of post-process sectioning or laser drilling. In this paper, a microwave non-destructive testing (NDT) technique is employed to evaluate the integrity of TBC after acute angle laser drilling. An Agilent 8510 XF network analyser operating over the frequency range of 45 MHz to 110 GHz was used to measure the amplitude and phase variations of scattered waves. The results significantly indicated the existence of delamination of 1-1.5 mm long at the TBC/substrate interface on the leading edge part of an acute-angled hole laser drilled

  3. Depth-dependent non-destructive analysis of thin overlayers using total-reflection-angle X-ray spectroscopy

    NASA Astrophysics Data System (ADS)

    Shibata, Noriyoshi; Okubo, Soichiro; Yonemitsu, Kyoko

    1996-07-01

    Electron-beam excited X-ray chemical analysis with very small angle condition has been applied to measure thin overlayers on substrates. Relations between the fluorescent X-ray intensity and the emission angle is investigated based on a model. It is demonstrated that the emission-angle dependence of the X-ray intensity is sensitively reflected by film thickness and layer structure. The calculations agreed well with experiments for thin Au and Pd multilayers on Si substrate. The results show that this method is applicable to a non-destructive depth profiling of chemical compositions.

  4. Magic Angle Spinning NMR Metabolomics

    SciTech Connect

    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.

  5. Magic-angle turning with double acquisition.

    PubMed

    Matsunaga, Tatsuya; Takegoshi, K

    2017-01-01

    The double-acquisition scheme for efficient data collection of hypercomplex data (the States method) of a two-dimensional experiment is adopted to magic-angle hopping (MAH) and magic-angle turning (MAT) experiments, which are powerful methods to measure the principal values of the chemical shift anisotropy (CSA) in a powder sample. It is shown that the double acquisition MAT (DAMAT) sequence realizes the S/N ratio comparable to or better than those of other variants of the MAH/MAT sequences. In addition, we show that DAMAT has preferable features that there are no spinning sidebands in the indirect dimension, and no spectral shearing is necessary.

  6. Magic-angle turning with double acquisition

    NASA Astrophysics Data System (ADS)

    Matsunaga, Tatsuya; Takegoshi, K.

    2017-01-01

    The double-acquisition scheme for efficient data collection of hypercomplex data (the States method) of a two-dimensional experiment is adopted to magic-angle hopping (MAH) and magic-angle turning (MAT) experiments, which are powerful methods to measure the principal values of the chemical shift anisotropy (CSA) in a powder sample. It is shown that the double acquisition MAT (DAMAT) sequence realizes the S/N ratio comparable to or better than those of other variants of the MAH/MAT sequences. In addition, we show that DAMAT has preferable features that there are no spinning sidebands in the indirect dimension, and no spectral shearing is necessary.

  7. Magic Angle Spinning NMR of Viruses

    PubMed Central

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

    2015-01-01

    Viruses, relatively simple pathogens, are able to replicate in many living organisms and to adapt to various environments. Conventional atomic-resolution structural biology techniques, X-ray crystallography and solution NMR spectroscopy provided abundant information on the structures of individual proteins and nucleic acids comprising viruses; however, viral assemblies are not amenable to analysis by these techniques because of their large size, insolubility, and inherent lack of long-range order. In this article, we review the recent advances in magic angle spinning NMR spectroscopy that enabled atomic-resolution analysis of structure and dynamics of large viral systems and give examples of several exciting case studies. PMID:25919197

  8. Magic angle spinning NMR of paramagnetic proteins.

    PubMed

    Knight, Michael J; Felli, Isabella C; Pierattelli, Roberta; Emsley, Lyndon; Pintacuda, Guido

    2013-09-17

    Metal ions are ubiquitous in biochemical and cellular processes. Since many metal ions are paramagnetic due to the presence of unpaired electrons, paramagnetic molecules are an important class of targets for research in structural biology and related fields. Today, NMR spectroscopy plays a central role in the investigation of the structure and chemical properties of paramagnetic metalloproteins, linking the observed paramagnetic phenomena directly to electronic and molecular structure. A major step forward in the study of proteins by solid-state NMR came with the advent of ultrafast magic angle spinning (MAS) and the ability to use (1)H detection. Combined, these techniques have allowed investigators to observe nuclei that previously were invisible in highly paramagnetic metalloproteins. In addition, these techniques have enabled quantitative site-specific measurement of a variety of long-range paramagnetic effects. Instead of limiting solid-state NMR studies of biological systems, paramagnetism provides an information-rich phenomenon that can be exploited in these studies. This Account emphasizes state-of-the-art methods and applications of solid-state NMR in paramagnetic systems in biological chemistry. In particular, we discuss the use of ultrafast MAS and (1)H-detection in perdeuterated paramagnetic metalloproteins. Current methodology allows us to determine the structure and dynamics of metalloenzymes, and, as an example, we describe solid-state NMR studies of microcrystalline superoxide dismutase, a 32 kDa dimer. Data were acquired with remarkably short times, and these experiments required only a few milligrams of sample.

  9. Non-destructive analysis of hydrogen-induced cracking of api steels using acoustic microscopy and small-angle neutron scattering

    NASA Astrophysics Data System (ADS)

    Oh, S. B.; Choi, Y.; Jung, H. G.; Kho, S. W.; Lee, C. S.

    2014-12-01

    Acoustic microscopy and small-angle neutron scattering were applied to non-destructively evaluate the hydrogen-induced cracking of API steels and to find the initiation time of the crack. The API steels had equiaxed grains with about 4 to 12-μm average grain size along the rolling, sample-normal, and transverse directions. For 5 days of immersion in a sodium-acetic solution with chloride ions (NaCl: CH3COOH: H2O: FeCl2 = 50: 5: 944: 1, pH = 2.7), micro-sized cracks were not formed in the as-received specimen, but they did form in the 7% deformed specimen. Nano-sized cracks were observed in the specimen after 3 days of immersion by small-angle neutron scattering.

  10. An efficient magic state approach to small angle rotations

    NASA Astrophysics Data System (ADS)

    Campbell, Earl T.; O'Gorman, Joe

    2016-12-01

    Standard error-correction techniques only provide a quantum memory and need extra gadgets to perform computation. Central to quantum algorithms are small angle rotations, which can be fault-tolerantly implemented given a supply of an unconventional species of magic state. We present a low-cost distillation routine for preparing these small angle magic states. Our protocol builds on the work of Duclos-Cianci and Poulin (2015 Phys. Rev. A 91 042315) by compressing their circuit. Additionally, we present a method of diluting magic states that reduces costs associated with very small angle rotations. We quantify performance by the expected number of noisy magic states consumed per rotation, and compare with other protocols. For modest-sized angles, our protocols offer a factor 24 improvement over the best-known gate synthesis protocols and a factor 2 over the Duclos-Cianci and Poulin protocol. For very small angle rotations, the dilution protocol dramatically reduces costs, giving several orders magnitude improvement over competitors. There also exists an intermediary regime of small, but not very small, angles where our approach gives a marginal improvement over gate synthesis. We discuss how different performance metrics may alter these conclusions.

  11. Broadband "Infinite-Speed" Magic-Angle Spinning NMR Spectroscopy

    SciTech Connect

    Hu, Yan-Yan; Levin, E.M; Schmidt-Rohr, Klaus

    2009-06-02

    High-resolution magic-angle spinning NMR of high-Z spin- 1/2 nuclei such as {sup 125}Te, {sup 207}Pb, {sup 119}Sn, {sup 113}Cd, and {sup 195}Pt is often hampered by large (>1000 ppm) chemical-shift anisotropies, which result in strong spinning sidebands that can obscure the centerbands of interest. In various tellurides with applications as thermoelectrics and as phase-change materials for data storage, even 22-kHz magic-angle spinning cannot resolve the center- and sidebands broadened by chemical-shift dispersion, which precludes peak identification or quantification. For sideband suppression over the necessary wide spectral range (up to 200 kHz), radio frequency pulse sequences with few, short pulses are required. We have identified Gan's two-dimensional magic-angle-turning (MAT) experiment with five 90{sup o} pulses as a promising broadband technique for obtaining spectra without sidebands. We have adapted it to broad spectra and fast magic-angle spinning by accounting for long pulses (comparable to the dwell time in t{sub 1}) and short rotation periods. Spectral distortions are small and residual sidebands negligible even for spectra with signals covering a range of 1.5 {gamma}B{sub 1}, due to a favorable disposition of the narrow ranges containing the signals of interest in the spectral plane. The method is demonstrated on various technologically interesting tellurides with spectra spanning up to 170 kHz, at 22 kHz MAS.

  12. Cross polarization magic-angle spinning NMR at cryogenic temperatures

    NASA Astrophysics Data System (ADS)

    Macho, V.; Kendrick, R.; Yannoni, C. S.

    A magic angle spinning (MAS) apparatus which can be used for high resolution solid state NMR at temperatures as low as 15 K is described. To demonstrate the utility of this apparatus, 13C spectra of molecules containing methyl groups have been investigated at cryogenic temperatures. The spectra, which are described in detail, provide direct evidence for the slowdown of methyl rotation.

  13. NMR in rotating magnetic fields: Magic angle field spinning

    SciTech Connect

    Sakellariou, D.; Meriles, C.; Martin, R.; Pines, A.

    2004-09-10

    Magic angle sample spinning has been one of the cornerstones in high-resolution solid state NMR. Spinning frequencies nowadays have increased by at least one order of magnitude over the ones used in the first experiments and the technique has gained tremendous popularity. It is currently a routine procedure in solid-state NMR, high-resolution liquid-state NMR and solid-state MRI. The technique enhances the spectral resolution by averaging away rank 2 anisotropic spin interactions thereby producing isotropic-like spectra with resolved chemical shifts and scalar couplings. Andrew proposed that it should be possible to induce similar effects in a static sample if the direction of the magnetic field is varied, e.g., magic-angle rotation of the B0 field (B0-MAS) and this has been recently demonstrated using electromagnetic field rotation. Here we discuss on the possibilities to perform field rotation using alternative hardware, together with spectroscopic methods to recover isotropic resolution even in cases where the field is not rotating at the magic angle. Extension to higher magnetic fields would be beneficial in situations where the physical manipulation of the sample is inconvenient or impossible. Such situations occur often in materials or biomedical samples where ''ex-situ'' NMR spectroscopy and imaging analysis is needed.

  14. Hydrogen and deuterium NMR of solids by magic angle spinning

    SciTech Connect

    Eckman, Richard Raymond

    1982-10-01

    The nuclear magnetic resonance of solids has long been characterized by very large spectral 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. For example, the homonuclear dipolar broadening, HD, for hydrogen is usually several tens of kilohertz. For deuterium, HD is relatively small; however, the quadrupole interaction causes a broadening which can be hundreds of kilohertz in polycrystalline or amorphous solids. 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, βm = Arccos(3-1/2), with respect to the direction of the external magnetic field. Two approaches have been developed for each nucleus. 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 HD was small. This often occurs naturally when the nuclei are semi-dilute or involved in

  15. Microcoil high-resolution magic angle spinning NMR spectroscopy.

    PubMed

    Janssen, Hans; Brinkmann, Andreas; van Eck, Ernst R H; van Bentum, P Jan M; Kentgens, Arno P M

    2006-07-12

    We report the construction of a dual-channel microcoil nuclear magnetic resonance probehead allowing magic-angle spinning for mass-limited samples. With coils down to 235 mum inner diameter, this allows high-resolution solid-state NMR spectra to be obtained for amounts of materials of a few nanoliters. This is demonstrated by the carbon-13 spectrum of a tripeptide and a single silk rod, prepared from the silk gland of the Bombyx mori silkworm. Furthermore, the microcoil allows for radio frequency field strengths well beyond current probe technology, aiding in getting the highest possible resolution by efficiently decoupling the observed nuclei from the abundantly present proton nuclei.

  16. Methods for magnetic resonance analysis using magic angle technique

    DOEpatents

    Hu, Jian Zhi [Richland, WA; Wind, Robert A [Kennewick, WA; Minard, Kevin R [Kennewick, WA; Majors, Paul D [Kennewick, WA

    2011-11-22

    Methods of performing a magnetic resonance analysis of a biological object are disclosed that include placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. In particular embodiments the method includes pulsing the radio frequency to provide at least two of a spatially selective read pulse, a spatially selective phase pulse, and a spatially selective storage pulse. Further disclosed methods provide pulse sequences that provide extended imaging capabilities, such as chemical shift imaging or multiple-voxel data acquisition.

  17. High-resolution NMR of anisotropic samples with spinning away from the magic angle

    SciTech Connect

    Sakellariou, Dimitris; Meriles, Carlos A.; Martin, Rachel W.; Pines, Alexander

    2003-03-31

    High-resolution NMR of samples in the solid state is typically performed under mechanical sample spinning around an axis that makes an angle, called the magic angle, of 54.7 degrees with the static magnetic field. There are many cases in which geometrical and engineering constraints prevent spinning at this specific angle. Implementations of in-situ and ex-situ magic angle field spinning might be extremely demanding because of the power requirements or an inconvenient sample size or geometry. Here we present a methodology based on switched angle spinning between two angles, none of which is the magic angle, which provide both isotropic and anisotropic information. Using this method, named Projected Magic Angle Spinning, we were able to obtain resolved isotropic chemical shifts in spinning samples where the broadening is mostly inhomogeneous.

  18. Multiple quantum magic-angle spinning using rotary resonance excitation

    NASA Astrophysics Data System (ADS)

    Vosegaard, Thomas; Florian, Pierre; Massiot, Dominique; Grandinetti, Philip J.

    2001-03-01

    We have discovered rotary resonances between rf field strength, ω1, and magic-angle spinning (MAS) frequency, ωR, which dramatically enhance the sensitivity of triple quantum preparation and mixing in the multiple-quantum MAS experiment, particularly for quadrupolar nuclei having low gyromagnetic ratios or experiencing strong quadrupole couplings. Triple quantum excitation efficiency minima occur when 2ω1=nωR, where n is an integer, with significant maxima occurring between these minima. For triple quantum mixing we observe maxima when ω1=nωR. In both preparation and mixing the pulse lengths required to reach maxima exceed one rotor period. We have combined these rotary resonance conditions into a new experiment called FASTER MQ-MAS, and have experimentally demonstrated a factor of 3 enhancement in sensitivity in comparison to conventional MQ-MAS.

  19. Magic angle effects and angular magnetoresistance oscillations as dimensional crossovers.

    PubMed

    Lebed, A G; Bagmet, N N; Naughton, M J

    2004-10-08

    Interference effects between velocity and density of states, which occur as electrons move along open orbits in the extended Brillouin zone in anisotropic conductors, result in a change of wave functions' dimensionality at magic angle (MA) directions of a magnetic field. In particular, these 1D-->2D dimensional crossovers result in the appearance of sharp minima in a resistivity component rho perpendicular (H,alpha), perpendicular to conducting layers. This explains the main qualitative features of MA and angular magnetoresistance oscillations' phenomena observed due to the existence of quasi-one-dimensional sheets of Fermi surface in (TMTSF)2X, (DMET-TSeF)2X, and kappa-(ET)2Cu(NCS)(2) conductors.

  20. Freezing of Molecular Motions Probed by Cryogenic Magic Angle Spinning NMR.

    PubMed

    Concistrè, Maria; Carignani, Elisa; Borsacchi, Silvia; Johannessen, Ole G; Mennucci, Benedetta; Yang, Yifeng; Geppi, Marco; Levitt, Malcolm H

    2014-02-06

    Cryogenic magic angle spinning makes it possible to obtain the NMR spectra of solids at temperatures low enough to freeze out most molecular motions. We have applied cryogenic magic angle spinning NMR to a crystalline small-molecule solid (ibuprofen sodium salt), which displays a variety of molecular dynamics. Magic angle (13)C NMR spectra are shown for a wide range of temperatures, including in the cryogenic regime down to 20 K. The hydrophobic and hydrophilic regions of the molecular structure display different behavior in the cryogenic regime, with the hydrophilic region remaining well-structured, while the hydrophobic region exhibits a broad frozen conformational distribution.

  1. High-pressure magic angle spinning nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Hoyt, David W.; Turcu, Romulus V. F.; Sears, Jesse A.; Rosso, Kevin M.; Burton, Sarah D.; Felmy, Andrew R.; Hu, Jian Zhi

    2011-10-01

    A high-pressure magic angle spinning (MAS) NMR capability, consisting of a reusable high-pressure MAS rotor, a high-pressure rotor loading/reaction chamber for in situ sealing and re-opening of the high-pressure MAS rotor, and a MAS probe with a localized RF coil for background signal suppression, is reported. The unusual technical challenges associated with development of a reusable high-pressure MAS rotor are addressed in part by modifying standard ceramics for the rotor sleeve by abrading the internal surface at both ends of the cylinder. In this way, not only is the advantage of ceramic cylinders for withstanding very high-pressure utilized, but also plastic bushings can be glued tightly in place so that other removable plastic sealing mechanisms/components and O-rings can be mounted to create the desired high-pressure seal. Using this strategy, sealed internal pressures exceeding 150 bars have been achieved and sustained under ambient external pressure with minimal loss of pressure for 72 h. As an application example, in situ13C MAS NMR studies of mineral carbonation reaction intermediates and final products of forsterite (Mg 2SiO 4) reacted with supercritical CO 2 and H 2O at 150 bar and 50 °C are reported, with relevance to geological sequestration of carbon dioxide.

  2. High-pressure magic angle spinning nuclear magnetic resonance.

    PubMed

    Hoyt, David W; Turcu, Romulus V F; Sears, Jesse A; Rosso, Kevin M; Burton, Sarah D; Felmy, Andrew R; Hu, Jian Zhi

    2011-10-01

    A high-pressure magic angle spinning (MAS) NMR capability, consisting of a reusable high-pressure MAS rotor, a high-pressure rotor loading/reaction chamber for in situ sealing and re-opening of the high-pressure MAS rotor, and a MAS probe with a localized RF coil for background signal suppression, is reported. The unusual technical challenges associated with development of a reusable high-pressure MAS rotor are addressed in part by modifying standard ceramics for the rotor sleeve by abrading the internal surface at both ends of the cylinder. In this way, not only is the advantage of ceramic cylinders for withstanding very high-pressure utilized, but also plastic bushings can be glued tightly in place so that other removable plastic sealing mechanisms/components and O-rings can be mounted to create the desired high-pressure seal. Using this strategy, sealed internal pressures exceeding 150 bars have been achieved and sustained under ambient external pressure with minimal loss of pressure for 72 h. As an application example, in situ(13)C MAS NMR studies of mineral carbonation reaction intermediates and final products of forsterite (Mg(2)SiO(4)) reacted with supercritical CO(2) and H(2)O at 150 bar and 50°C are reported, with relevance to geological sequestration of carbon dioxide.

  3. High-pressure magic angle spinning nuclear magnetic resonance

    SciTech Connect

    Hoyt, David W.; Turcu, Romulus V. F.; Sears, Jesse A.; Rosso, Kevin M.; Burton, Sarah D.; Felmy, Andrew R.; Hu, Jian Zhi

    2011-10-01

    A high-pressure magic angle spinning (MAS) NMR capability, consisting of a reusable high-pressure MAS rotor, a high-pressure rotor loading/reaction chamber for in situ sealing and re-opening of the high-pressure MAS rotor, and a MAS probe with a localized RF coil for background signal suppression, is reported. The unusual technical challenges associated with development of a reusable high-pressure MAS rotor are addressed in part by modifying standard ceramics for the rotor sleeve by abrading the internal surface at both ends of the cylinder. In this way, not only is the advantage of ceramic cylinders for withstanding very high-pressure utilized, but also plastic bushings can be glued tightly in place so that other removable plastic sealing mechanisms/components and O-rings can be mounted to create the desired high-pressure seal. Using this strategy, sealed internal pressures exceeding 150 bars have been achieved and sustained under ambient external pressure with minimal loss of pressure for 72 h. Finally, as an application example, in situ13C MAS NMR studies of mineral carbonation reaction intermediates and final products of forsterite (Mg2SiO4) reacted with supercritical CO2 and H2O at 150 bar and 50 °C are reported, with relevance to geological sequestration of carbon dioxide.

  4. Magic angle magnetic resonance imaging of diode laser induced and naturally occurring lesions in equine tendons.

    PubMed

    Spriet, Mathieu; Murphy, Brian; Vallance, Stuart A; Vidal, Martin A; Whitcomb, Mary Beth; Wisner, Erik R

    2012-01-01

    Magic angle magnetic resonance (MR) imaging consists of imaging tendons at 55° to the magnetic field. In people, magic angle MR imaging is valuable for detection of chronic tendon lesions and allows calculation of tendon T1 values. Increased T1 values occur in people with chronic tendinopathy. The T1 values of normal equine tendons have been reported but there are no available data for abnormal equine tendons. Twelve limbs were studied. Two limbs had diode laser tendon lesions induced postmortem, four limbs had diode laser tendon lesions induced in vivo and six limbs had naturally occurring tendon lesions. The limbs were imaged at 1.5 T using both conventional MR imaging and magic angle MR imaging. The post-mortem laser induced lesions were identified only with magic angle MR imaging. The in vivo induced lesions and naturally occurring lesions were identified with both techniques but had a different appearance with the two imaging techniques. Magic angle imaging was helpful at identifying lesions that were hypointense on conventional imaging. Increased T1 values were observed in all abnormal tendons and in several tendons with a subjectively normal MR appearance. The increased T1 value may reflect diffuse changes in the biochemical composition of tendons. Magic angle imaging has potential as a useful noninvasive tool to assess the changes of the extracellular tendon matrix using T1 values.

  5. High-resolution NMR spectroscopy of biological tissues usingprojected Magic Angle Spinning

    SciTech Connect

    Martin, Rachel W.; Jachmann, Rebecca C.; Sakellariou, Dimitris; Nielsen, Ulla Gro; Pines, Alexander

    2005-01-27

    High-resolution NMR spectra of materials subject toanisotropic broadening are usually obtained by rotating the sample aboutthe magic angle, which is 54.7 degrees to the static magnetic field. Inprojected Magic Angle Spinning (p-MAS), the sample is spun about twoangles, neither of which is the magic angle. This provides a method ofobtaining isotropic spectra while spinning at shallow angles. The p-MASexperiment may be used in situations where spinning the sample at themagic angle is not possible due to geometric or other constraints,allowing the choice of spinning angle to be determined by factors such asthe shape of the sample, rather than by the spin physics. The applicationof this technique to bovine tissue samples is demonstrated as a proof ofprinciple for future biological or medical applications.

  6. Atlantis Non-destructive Testing

    NASA Image and Video Library

    2003-10-29

    In the Orbiter Processing Facility, the nose cap (foreground) removed from Atlantis (behind) waits to be shipped to the original manufacturing company, Vought in Ft. Worth, Texas, a subsidiary of Lockheed Martin, to undergo non-destructive testing such as CAT scan and thermography.

  7. Solid effect in magic angle spinning dynamic nuclear polarization.

    PubMed

    Corzilius, Björn; Smith, Albert A; Griffin, Robert G

    2012-08-07

    For over five decades, the solid effect (SE) has been heavily utilized as a mechanism for performing dynamic nuclear polarization (DNP). Nevertheless, it has not found widespread application in contemporary, high magnetic field DNP experiments because SE enhancements display an ω(0)(-2) field dependence. In particular, for nominally forbidden zero and double quantum SE transitions to be partially allowed, it is necessary for mixing of adjacent nuclear spin states to occur, and this leads to the observed field dependence. However, recently we have improved our instrumentation and report here an enhancement of ε = 91 obtained with the organic radical trityl (OX063) in magic angle spinning experiments performed at 5 T and 80 K. This is a factor of 6-7 higher than previous values in the literature under similar conditions. Because the solid effect depends strongly on the microwave field strength, we attribute this large enhancement to larger microwave field strengths inside the sample volume, achieved with more efficient coupling of the gyrotron to the sample chamber. In addition, we develop a theoretical model to explain the dependence of the buildup rate of enhanced nuclear polarization and the steady-state enhancement on the microwave power. Buildup times and enhancements were measured as a function of (1)H concentration for both trityl and Gd-DOTA. Comparison of the results indicates that for trityl the initial polarization step is the slower, rate-determining step. However, for Gd-DOTA the spread of nuclear polarization via homonuclear (1)H spin diffusion is rate-limiting. Finally, we discuss the applicability of the solid effect at fields > 5 T and the requirements to address the unfavorable field dependence of the solid effect.

  8. Solid effect in magic angle spinning dynamic nuclear polarization

    PubMed Central

    Corzilius, Björn; Smith, Albert A.; Griffin, Robert G.

    2012-01-01

    For over five decades, the solid effect (SE) has been heavily utilized as a mechanism for performing dynamic nuclear polarization (DNP). Nevertheless, it has not found widespread application in contemporary, high magnetic field DNP experiments because SE enhancements display an \\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{upgreek} \\usepackage{mathrsfs} \\setlength{\\oddsidemargin}{-69pt} \\begin{document} \\begin{equation*}\\omega _0 ^{ - 2}\\end{equation*} \\end{document}ω0−2 field dependence. In particular, for nominally forbidden zero and double quantum SE transitions to be partially allowed, it is necessary for mixing of adjacent nuclear spin states to occur, and this leads to the observed field dependence. However, recently we have improved our instrumentation and report here an enhancement of ɛ = 91 obtained with the organic radical trityl (OX063) in magic angle spinning experiments performed at 5 T and 80 K. This is a factor of 6-7 higher than previous values in the literature under similar conditions. Because the solid effect depends strongly on the microwave field strength, we attribute this large enhancement to larger microwave field strengths inside the sample volume, achieved with more efficient coupling of the gyrotron to the sample chamber. In addition, we develop a theoretical model to explain the dependence of the buildup rate of enhanced nuclear polarization and the steady-state enhancement on the microwave power. Buildup times and enhancements were measured as a function of 1H concentration for both trityl and Gd-DOTA. Comparison of the results indicates that for trityl the initial polarization step is the slower, rate-determining step. However, for Gd-DOTA the spread of nuclear polarization via homonuclear 1H spin diffusion is rate-limiting. Finally, we discuss the applicability of the solid effect at fields > 5 T and the requirements

  9. Hall Plateaus at magic angles in ultraquantum Bismuth

    NASA Astrophysics Data System (ADS)

    Benoît, Fauqué.

    2009-03-01

    The behaviour of a three-dimensional electron gas in the presence of a magnetic field strong enough to put all carriers in the first Landau level (i.e. beyond the quantum limit) is a longstanding question of theoretical condensed matter physics [1]. This issue has been recently explored by two high-field experiments on elemental semi-metal Bismuth. In a first study of transport coefficients (which are dominated by hole-like carriers), the Nernst coefficient presented three unexpected maxima that are concomitant with quasi-plateaux in the Hall coefficient [2]. In a second series of experiments, torque magnetometry (which mainly probes the three Dirac valley electron pockets) detected a field-induced phase transition [3]. The full understanding of the electron and hole behaviours above the quantum limit of pure Bi is therefore still under debate. In this talk, we will present our measurement of the Hall resistivity and torque magnetometry with magnetic field up to 31 T and rotating in the trigonal-bisectrix plane [4]. The Hall response is dominated by the hole pockets according to its sign as well as the period and the angular dependence of its quantum oscillations. In the vicinity of the quantum limit, it presents additional anomalies which are the fingerprints of the electron pockets. We found that for particular orientations of the magnetic field (namely ``magic angles''), the Hall response becomes field-independent within the experimental resolution around 20T. This drastic dependence of the plateaux on the field orientation provides strong constraints for theoretical scenarios. [4pt] [1] Bertrand I. Halperin, Japanese Journal of Applied Physics, 26, Supplement 26-3 (1987).[0pt] [2] Kamran Behnia, Luis Balicas, Yakov Kopelevich, Science, 317, 1729 (2008).[0pt] [3] Lu Li, J. G. Checkelsky, Y. S. Hor, C. Uher, A. F. Hebard, R. J. Cava, and N. P. Ong , Science, 321, 5888 (2008).[0pt] [4] Benoît Fauqu'e, Luis Balicas, Ilya Sheikin, Jean Paul Issi and Kamran Behnia

  10. Theoretical aspects of Magic Angle Spinning - Dynamic Nuclear Polarization.

    PubMed

    Mentink-Vigier, Frederic; Akbey, Ümit; Oschkinat, Hartmut; Vega, Shimon; Feintuch, Akiva

    2015-09-01

    Magic Angle Spinning (MAS) combined with Dynamic Nuclear Polarization (DNP) has been proven in recent years to be a very powerful method for increasing solid-state NMR signals. Since the advent of biradicals such as TOTAPOL to increase the nuclear polarization new classes of radicals, with larger molecular weight and/or different spin properties have been developed. These have led to unprecedented signal gain, with varying results for different experimental parameters, in particular the microwave irradiation strength, the static field, and the spinning frequency. Recently it has been demonstrated that sample spinning imposes DNP enhancement processes that differ from the active DNP mechanism in static samples as upon sample spinning the DNP enhancements are the results of energy level anticrossings occurring periodically during each rotor cycle. In this work we present experimental results with regards to the MAS frequency dependence of the DNP enhancement profiles of four nitroxide-based radicals at two different sets of temperature, 110 and 160K. In fact, different magnitudes of reduction in enhancement are observed with increasing spinning frequency. Our simulation code for calculating MAS-DNP powder enhancements of small model spin systems has been improved to extend our studies of the influence of the interaction and relaxation parameters on powder enhancements. To achieve a better understanding we simulated the spin dynamics of a single three-spin system {ea-eb-n} during its steady state rotor periods and used the Landau-Zener formula to characterize the influence of the different anti-crossings on the polarizations of the system and their necessary action for reaching steady state conditions together with spin relaxation processes. Based on these model calculations we demonstrate that the maximum steady state nuclear polarization cannot become larger than the maximum polarization difference between the two electrons during the steady state rotor cycle. This

  11. Slow Magic Angle Sample Spinning: A Non- or Minimally Invasive Method for High- Resolution 1H Nuclear Magnetic Resonance (NMR) Metabolic Profiling

    SciTech Connect

    Hu, Jian Z.

    2011-05-01

    High resolution 1H magic angle spinning nuclear magnetic resonance (NMR), using a sample spinning rate of several kHz or more (i.e., high resolution-magic angle spinning (hr-MAS)), is a well established method for metabolic profiling in intact tissues without the need for sample extraction. The only shortcoming with hr-MAS is that it is invasive and is thus unusable for non-destructive detections. Recently, a method called slow-MAS, using the concept of two dimensional NMR spectroscopy, has emerged as an alternative method for non- or minimal invasive metabolomics in intact tissues, including live animals, due to the slow or ultra-slow-sample spinning used. Although slow-MAS is a powerful method, its applications are hindered by experimental challenges. Correctly designing the experiment and choosing the appropriate slow-MAS method both require a fundamental understanding of the operation principles, in particular the details of line narrowing due to the presence of molecular diffusion. However, these fundamental principles have not yet been fully disclosed in previous publications. The goal of this chapter is to provide an in depth evaluation of the principles associated with slow-MAS techniques by emphasizing the challenges associated with a phantom sample consisting of glass beads and H2O, where an unusually large magnetic susceptibility field gradient is obtained.

  12. Slow magic angle sample spinning: a non- or minimally invasive method for high-resolution 1H nuclear magnetic resonance (NMR) metabolic profiling.

    PubMed

    Hu, Jian Zhi

    2011-01-01

    High-resolution (1)H magic angle spinning nuclear magnetic resonance (NMR), using a sample spinning rate of several kilohertz or more (i.e., high-resolution magic angle spinning (hr-MAS)), is a well-established method for metabolic profiling in intact tissues without the need for sample extraction. The only shortcoming with hr-MAS is that it is invasive and is thus unusable for non-destructive detections. Recently, a method called slow MAS, using the concept of two-dimensional NMR spectroscopy, has emerged as an alternative method for non- or minimally invasive metabolomics in intact tissues, including live animals, due to the slow or ultra-slow sample spinning used. Although slow MAS is a powerful method, its applications are hindered by experimental challenges. Correctly designing the experiment and choosing the appropriate slow MAS method both require a fundamental understanding of the operation principles, in particular the details of line narrowing due to the presence of molecular diffusion. However, these fundamental principles have not yet been fully disclosed in previous publications. The goal of this chapter is to provide an in-depth evaluation of the principles associated with slow MAS techniques by emphasizing the challenges associated with a phantom sample consisting of glass beads and H(2)O, where an unusually large magnetic susceptibility field gradient is obtained.

  13. The magic angle effect: a source of artifact, determinant of image contrast, and technique for imaging.

    PubMed

    Bydder, Mark; Rahal, Andres; Fullerton, Gary D; Bydder, Graeme M

    2007-02-01

    This review provides a formalism for understanding magic angle effects in clinical studies. It involves consideration of the fiber-to-field angle for linear structures such as tendons, ligaments, and peripheral nerves, disc-like and circular structures such as menisci and labra, as well as complex three-dimensional structures. There may be one or more fiber types with different orientations within each of these tissues. The orientation of these fibers to B(0) is crucial in determining their magic angle effect. Tissues may show a variety of appearances depending on their baseline T2, as well as the increase in T2 produced by the magic angle effect. The appearances are affected by TE, which affects both the general tissue signal level and the change in signal produced by the magic angle effect, fiber-to-slice orientation, and partial volume effects. Deliberate positioning of structures and tissues at particular orientations to B(0) can be used to increase the signal from tissues such as tendons and ligaments and so allow them to be imaged with conventional sequences. The technique can also be used to produce contrast between tissues with fibers that have different orientations to B(0). (c) 2007 Wiley-Liss, Inc.

  14. Non-Destructive Testing Scanner

    NASA Technical Reports Server (NTRS)

    1990-01-01

    Bio-Imaging Research's technology that originated in an aerospace program has come full circle with a new aerospace adaptation called the Advanced Computed Tomography Inspection System, or ACTIS. The medical version of CT scans the human body for tumors or other abnormalities, the ACTIS system finds imperfections in aerospace structures and components, such as castings, assemblies, rocket motors and nozzles. ACTIS is described by its developer as the most versatile CT scanner available for non-destructive testing applications. ACTIS is a variable geometry system. ACTIS source and detectors can be moved closer together or farther apart to optimize the geometry for different sizes of test objects. The combination of variable geometry, three sources, and focusing detectors makes ACTIS cost effective for a broad range of applications. System can scan anything from very small turbine blades to large rocket assemblies.

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

    SciTech Connect

    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.

  16. A Theoretical Design Approach for Passive Shimming of a Magic-Angle-Spinning NMR Magnet.

    PubMed

    Li, Frank X; Voccio, John P; Sammartino, Michael; Ahn, Minchul; Hahn, Seungyong; Bascuñán, Juan; Iwasa, Yukikazu

    2016-06-01

    This paper presents a passive shimming design approach for a magic-angle-spinning (MAS) NMR magnet. In order to achieve a 1.5-T magic-angle field in NMR samples, we created two independent orthogonal magnetic vector fields by two separate coils: the dipole and solenoid. These two coils create a combined 1.5-T magnetic field vector directed at the magic angle (54.74° from the spinning axis). Additionally, the stringent magnetic field homogeneity requirement of the MAS magnet is the same as that of a solenoidal NMR magnet. The challenge for the magic-angle passive shimming design is to correct both the dipole and solenoid magnetic field spherical harmonics with one set of iron pieces, the so-called ferromagnetic shimming. Furthermore, the magnetization of the iron pieces is produced by both the dipole and solenoid coils. In our design approach, a matrix of 2 mm by 5 mm iron pieces with different thicknesses was attached to a thin-walled tube, 90-mm diameter and 40-mm high. Two sets of spherical harmonic coefficients were calculated for both the dipole and solenoid coil windings. By using the multiple-objective linear programming optimization technique and coordinate transformations, we have designed a passive shimming set that can theoretically reduce 22 lower-order spherical harmonics and improve the homogeneity of our MAS NMR magnet.

  17. Devices and process for high-pressure magic angle spinning nuclear magnetic resonance

    DOEpatents

    Hoyt, David W; Sears, Jr., Jesse A; Turcu, Romulus V.F.; Rosso, Kevin M; Hu, Jian Zhi

    2014-04-08

    A high-pressure magic angle spinning (MAS) rotor is detailed that includes a high-pressure sample cell that maintains high pressures exceeding 150 bar. The sample cell design minimizes pressure losses due to penetration over an extended period of time.

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

    SciTech Connect

    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, ..beta../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 ..beta... 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 /sup 1/H with /sup 2/H combined with magic angle rotation. The resolution obtained represents the practical limit for proton NMR of solids.

  19. Towards monomaterial p-n junctions: Single-step fabrication of tin oxide films and their non-destructive characterisation by angle-dependent X-ray photoelectron spectroscopy

    SciTech Connect

    Krzywiecki, Maciej; Sarfraz, Adnan; Erbe, Andreas

    2015-12-07

    The application of a non-destructive method for characterization of electronic structure of an ultra-thin SnO{sub 1angle dependent XPS, we quantified stoichiometry changes inside the SnO{sub 1

  20. Complete protocol for slow-spinning high-resolution magic-angle spinning NMR analysis of fragile tissues.

    PubMed

    André, Marion; Dumez, Jean-Nicolas; Rezig, Lamya; Shintu, Laetitia; Piotto, Martial; Caldarelli, Stefano

    2014-11-04

    High-resolution magic-angle spinning (HR-MAS) nuclear magnetic resonance (NMR) is an essential tool to characterize a variety of semisolid systems, including biological tissues, with virtually no sample preparation. The "non-destructive" nature of NMR is typically compromised, however, by the extreme centrifugal forces experienced under conventional HR-MAS frequencies of several kilohertz. These features limit the usefulness of current HR-MAS approaches for fragile samples. Here, we introduce a full protocol for acquiring high-quality HR-MAS NMR spectra of biological tissues at low spinning rates (down to a few hundred hertz). The protocol first consists of a carefully designed sample preparation, which yields spectra without significant spinning sidebands at low spinning frequency for several types of sample holders, including the standard disposable inserts classically used in HR-MAS NMR-based metabolomics. Suppression of broad spectral features is then achieved using a modified version of the recently introduced PROJECT experiment with added water suppression and rotor synchronization, which deposits limited power in the sample and which can be suitably rotor-synchronized at low spinning rates. The performance of the slow HR-MAS NMR procedure is demonstrated on conventional (liver tissue) and very delicate (fish eggs) samples, for which the slow-spinning conditions are shown to preserve the structural integrity and to minimize intercompartmental leaks of metabolites. Taken together, these results expand the applicability and reliability of HR-MAS NMR spectroscopy. These results have been obtained at 400 and 600 MHz and suggest that high-quality slow HR-MAS spectra can be expected at higher magnetic fields using the described protocol.

  1. V-shaped nematogens with the "magic bent angle".

    PubMed

    Seltmann, Jens; Müller, Kathrin; Klein, Susanne; Lehmann, Matthias

    2011-06-21

    V-shaped nematogens 1a-c and 2a-b with benzodithiophene bending units have been synthesised. The derivatives 1a-c comprise a flat core with a bending angle of 109°, which is almost the tetrahedral angle proposed to be optimal in the realization of mesogens forming a biaxial nematic thermotropic mesophase.

  2. Method for high resolution magnetic resonance analysis using magic angle technique

    DOEpatents

    Wind, Robert A.; Hu, Jian Zhi

    2004-12-28

    A method of performing a magnetic resonance analysis of a biological object that includes placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. The object may be reoriented about the magic angle axis between three predetermined positions that are related to each other by 120.degree.. The main magnetic field may be rotated mechanically or electronically. Methods for magnetic resonance imaging of the object are also described.

  3. Method for high resolution magnetic resonance analysis using magic angle technique

    DOEpatents

    Wind, Robert A.; Hu, Jian Zhi

    2003-12-30

    A method of performing a magnetic resonance analysis of a biological object that includes placing the object in a main magnetic field (that has a static field direction) and in a radio frequency field; rotating the object at a frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a phase-corrected magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. The object may be reoriented about the magic angle axis between three predetermined positions that are related to each other by 120.degree.. The main magnetic field may be rotated mechanically or electronically. Methods for magnetic resonance imaging of the object are also described.

  4. Discrete magic angle turning system, apparatus, and process for in situ magnetic resonance spectroscopy and imaging

    DOEpatents

    Hu, Jian Zhi; Sears, Jr., Jesse A.; Hoyt, David W.; Wind, Robert A.

    2009-05-19

    Described are a "Discrete Magic Angle Turning" (DMAT) system, devices, and processes that combine advantages of both magic angle turning (MAT) and magic angle hopping (MAH) suitable, e.g., for in situ magnetic resonance spectroscopy and/or imaging. In an exemplary system, device, and process, samples are rotated in a clockwise direction followed by an anticlockwise direction of exactly the same amount. Rotation proceeds through an angle that is typically greater than about 240 degrees but less than or equal to about 360 degrees at constant speed for a time applicable to the evolution dimension. Back and forth rotation can be synchronized and repeated with a special radio frequency (RF) pulse sequence to produce an isotropic-anisotropic shift 2D correlation spectrum. The design permits tubes to be inserted into the sample container without introducing plumbing interferences, further allowing control over such conditions as temperature, pressure, flow conditions, and feed compositions, thus permitting true in-situ investigations to be carried out.

  5. Restoring Resolution in Biological Solid-State NMR under Conditions of Off-Magic-Angle Spinning.

    PubMed

    Sarkar, Riddhiman; Rodriguez Camargo, Diana C; Pintacuda, Guido; Reif, Bernd

    2015-12-17

    Spin-state-selective excitation (S3E) experiments allow the selection of individual transitions in a coupled two spin system. We show that in the solid state, the dipole-dipole interaction (DD) between (15)N and (1)H in a (1)H-(15)N bond and the chemical shift anisotropy (CSA) of (15)N in an amide moiety mutually cancel each other for a particular multiplet component at high field, when the sample is spun off the magic angle (Arctan [√2] = 54.74°). The accuracy of the adjustment of the spinning angle is crucial in conventional experiments. We demonstrate that for S3E experiments, the requirement to spin the sample exactly at the magic angle is not mandatory. Applications of solid state NMR in narrow bore magnets will be facilitated where the adjustment of the magic angle is often difficult. The method opens new perspectives for the development of schemes to determine distances and to quantify dynamics in the solid state.

  6. A sensitive, high resolution magic angle turning experiment for measuring chemical shift tensor principal values

    NASA Astrophysics Data System (ADS)

    Alderman, D. W.

    1998-12-01

    A sensitive, high-resolution 'FIREMAT' two-dimensional (2D) magic-angle-turning experiment is described that measures chemical shift tensor principal values in powdered solids. The spectra display spinning-sideband patterns separated by their isotropic shifts. The new method's sensitivity and high resolution in the isotropic-shift dimension result from combining the 5pi magic-angle-turning pulse sequence, an extension of the pseudo-2D sideband-suppression data rearrangement, and the TIGER protocol for processing 2D data. TPPM decoupling is used to enhance resolution. The method requires precise synchronization of the pulses and sampling to the rotor position. It is shown that the technique obtains 35 natural-abundance 13C tensors from erythromycin in 19 hours, and high quality naturalabundance 15N tensors from eight sites in potassium penicillin V in three days on a 400MHz spectrometer.

  7. Correlation of fast and slow chemical shift spinning sideband patterns under fast magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Eléna, Bénédicte; Hediger, Sabine; Emsley, Lyndon

    2003-01-01

    A new two-dimensional solid-state NMR experiment, which correlates slow and fast chemical shift anisotropy sideband patterns is proposed. The experiment, dubbed ROSES, is performed under fast magic-angle spinning and leads to an isotropic spectrum in the directly detected ω2 dimension. In the evolution dimension ω1, the isotropic chemical shift is reduced by a factor S, and spinning sidebands are observed spaced by a scaled effective spinning speed ωR/ S. These spinning sidebands patterns are not identical to those observed with standard slow magic-angle spinning experiments. Chemical shift anisotropy parameters can be accurately extracted with standard methods from these spinning sideband patterns. The experiment is demonstrated with carbon-13 experiments on powdered samples of a dipeptide and a cyclic undecapeptide, cyclosporin-A.

  8. Microfabricated inserts for magic angle coil spinning (MACS) wireless NMR spectroscopy.

    PubMed

    Badilita, Vlad; Fassbender, Birgit; Kratt, Kai; Wong, Alan; Bonhomme, Christian; Sakellariou, Dimitris; Korvink, Jan G; Wallrabe, Ulrike

    2012-01-01

    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.

  9. Spin-locking and cross-polarization under magic-angle spinning of uniformly labeled solids.

    PubMed

    Hung, Ivan; Gan, Zhehong

    2015-07-01

    Spin-locking and cross-polarization under magic-angle spinning are investigated for uniformly (13)C and (15)N labeled solids. In particular, the interferences from chemical shift anisotropy, and (1)H heteronuclear and (13)C homonuclear dipolar couplings are identified. The physical origin of these interferences provides guidelines for selecting the best (13)C and (15)N polarization transfer rf fields. Optimal settings for both the zero- and double-quantum cross-polarization transfer mechanisms are recommended.

  10. NMR high-resolution magic angle spinning rotor design for quantification of metabolic concentrations

    NASA Astrophysics Data System (ADS)

    Holly, R.; Damyanovich, A.; Peemoeller, H.

    2006-05-01

    A new high-resolution magic angle spinning nuclear magnetic resonance technique is presented to obtain absolute metabolite concentrations of solutions. The magnetic resonance spectrum of the sample under investigation and an internal reference are acquired simultaneously, ensuring both spectra are obtained under the same experimental conditions. The robustness of the technique is demonstrated using a solution of creatine, and it is shown that the technique can obtain solution concentrations to within 7% or better.

  11. Determination of T1 relaxation time of normal equine tendons using magic angle magnetic resonance imaging.

    PubMed

    Spriet, Mathieu; Wisner, Erik R; Anthenill, Lucy A; Buonocore, Michael H

    2011-01-01

    Seven isolated equine front limbs were used to establish the normal T1 relaxation time of equine superficial digital flexor tendon (SDFT), deep digital flexor tendon (DDFT), and suspensory ligament (SL) using magic angle magnetic resonance (MR) imaging. MR imaging of the metacarpi was performed with the limbs positioned at 55° (the magic angle) relative to the main magnetic field. Transverse spin-echo proton density and inversion recovery images were acquired. T1 relaxation time was calculated based on ratios of signal intensity determined from the different pulse sequences. T1 relaxation times for SDFT, DDFT, and SL were 288 (± 17), 244 (± 14), and 349 (± 16) ms, respectively. The difference in T1 values between SDFT, DDFT, and SL was statistically significant. T1 values of equine tendons can be determined with magic angle imaging on a clinical MR system using < 10 min total scan time. The knowledge of the normal range of T1 values may be useful to identify horses with chronic tendinopathy, where based on the human literature, an increased T1 value may be expected. © 2010 Veterinary Radiology & Ultrasound.

  12. An isotropic chemical shift-chemical shift anisotropic correlation experiment using discrete magic angle turning.

    PubMed

    Hu, Jian Zhi; Sears, Jesse A; Kwak, Ja Hun; Hoyt, David W; Wang, Yong; Peden, Charles H F

    2009-05-01

    An isotropic-anisotropic shift 2D correlation spectroscopy is introduced that combines the advantages of both magic angle turning (MAT) and magic angle hopping (MAH) technologies. In this new approach, denoted DMAT for "discrete magic angle turning", the sample rotates clockwise followed by an anticlockwise rotation of exactly the same amount with each rotation less or equal than 360 degrees but greater than 240 degrees , with the rotation speed being constant only for times related to the evolution dimension. This back and forth rotation is repeated and synchronized with a special radio frequency (RF) pulse sequence to produce an isotropic-anisotropic shift 2D correlation spectrum. For any spin-interaction of rank-2 such as chemical shift anisotropy, isotropic magnetic susceptibility interaction, and residual homo-nuclear dipolar interaction in biological fluid samples, the projection along the isotropic dimension is a high resolution spectrum. Since a less than 360 degrees sample rotation is involved, the design potentially allows for in situ control over physical parameters such as pressure, flow conditions, feed compositions, and temperature so that true in situ NMR investigations can be carried out.

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

    PubMed Central

    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

  14. An X0 shim coil for precise magic-angle adjustment.

    PubMed

    Matsunaga, Tatsuya; Mizuno, Takashi; Takegoshi, K

    2015-07-01

    A new method for precise setting of the spinning angle to the magic angle by using a saddle coil is described. The coil, which is referred to as an X0 shim coil, is wound to produce a uniform static magnetic field Bx perpendicular to the main magnetic field B0. The magnetic field felt by a sample is a vector sum of the main field B0 and the transverse field Bx produced by the X0 shim coil. Hence the angle between the spinner axis and the effective magnetic field can be controlled by current I supplied to the X0 shim coil, leading to precise angle adjustment without backlash accompanied with a mechanical system conventionally used. It is shown that the angle range achieved is ±0.05° for I=±5A at B0=7T. Copyright © 2015 Elsevier Inc. All rights reserved.

  15. Microfabricated Inserts for Magic Angle Coil Spinning (MACS) Wireless NMR Spectroscopy

    PubMed Central

    Badilita, Vlad; Fassbender, Birgit; Kratt, Kai; Wong, Alan; Bonhomme, Christian; Sakellariou, Dimitris; Korvink, Jan G.; Wallrabe, Ulrike

    2012-01-01

    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. PMID:22936994

  16. Magic angle and height quantization in nanofacets on SiC(0001) surfaces

    SciTech Connect

    Sawada, Keisuke; Iwata, Jun-Ichi; Oshiyama, Atsushi

    2014-02-03

    We report on the density-functional calculations that provide microscopic mechanism of the facet formation on the SiC (0001) surface. We first identify atom-scale structures of single-, double-, and quad-bilayer steps and find that the single-bilayer (SB) step has the lowest formation energy. We then find that the SB steps are bunched to form a nanofacet with a particular angle relative to the (0001) plane (magic facet angle) and with a discretized height along the (0001) direction (height quantization). We also clarify a microscopic reason for the self-organization of the nanofacet observed experimentally.

  17. Non-destructive identification of twisted light.

    PubMed

    Li, Pengyun; Wang, Bo; Song, Xinbing; Zhang, Xiangdong

    2016-04-01

    The non-destructive identification of the orbital angular momentum (OAM) is essential to various applications in the optical information processing. Here, we propose and demonstrate experimentally an efficient method to identify non-destructively the OAM by using a modified Mach-Zehnder interferometer. Our schemes are applicable not only to the case with integer charges, but also to optical vortices with noninteger charges. Our Letter presents the first experimental demonstration of the non-destructive identification of twisted light with integer or noninteger topological charges, which has potential applications in the OAM-based data transmission for optical communications.

  18. Experiments Optimized for Magic Angle Spinning and Oriented Sample Solid-State NMR of Proteins

    PubMed Central

    Das, Bibhuti B.; Lin, Eugene C.; Opella, Stanley J.

    2013-01-01

    Structure determination by solid-state NMR of proteins is rapidly advancing as result of recent developments of samples, experimental methods, and calculations. There are a number of different solid-state NMR approaches that utilize stationary, aligned samples or magic angle spinning of unoriented ‘powder’ samples, and depending on the sample and the experimental method can emphasize the measurement of distances or angles, ideally both, as sources of structural constraints. Multi-dimensional correlation spectroscopy of low-gamma nuclei such as 15N and 13C is an important step for making resonance assignments and measurements of angular restraints in membrane proteins. However, the efficiency of coherence transfer predominantly depends upon the strength of dipole-dipole interaction, and this can vary from site to site and between sample alignments, for example, during the mixing of 13C and 15N magnetization in stationary aligned and in magic angle spinning samples. Here, we demonstrate that the efficiency of polarization transfer can be improved by using adiabatic demagnetization and remagnetization techniques on stationary aligned samples; and proton assisted insensitive nuclei cross-polarization in magic angle sample spinning samples. Adiabatic cross-polarization technique provides an alternative mechanism for spin-diffusion experiments correlating 15N/15N and 15N/13C chemical shifts over large distances. Improved efficiency in cross-polarization with 40% – 100% sensitivity enhancements are observed in proteins and single crystals, respectively. We describe solid-state NMR experimental techniques that are optimal for membrane proteins in liquid crystalline phospholipid bilayers under physiological conditions. The techniques are illustrated with data from both single crystals of peptides and of membrane proteins in phospholipid bilayers. PMID:24044695

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

    PubMed

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

    2017-03-29

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

  20. Magic

    NASA Astrophysics Data System (ADS)

    Willetts, Andrew; Gagliardi, Laura; Ioannou, Andrew G.; Skylaris, Chris-Kriton; Spencer, Steven; Handy, Nicholas C.; Simper, Adrian M.

    The nuclear industry has enormous challenges to address in understanding its waste products and their safe disposal. It is extremely expensive and difficult to work with such waste products. As computational chemistry has made so many advances in the last 30 years, the question arises as to whether it can start to answer some of the basic questions. It was in this context that British Nuclear Fuels plc approached the quantum chemistry group at the University of Cambridge. After initial considerations, it was decided to write an entirely new quantum chemistry package to address these fundamental problems. The MAGIC program has been written to model as accurately as possible the properties of heavy-atom (in particular, actinide) complexes in realistic environments. Major requirements were the need to include relativistic effects for which several investigations have been carried out by quantum chemists in recent years. A severe difficulty is the high angular momentum of the occupied orbitals in the actinides. It was also believed that it was very important to include the effects of electron correlation. Again much progress has been made by quantum chemists with this problem. Therefore this code was written to take into account all these advances in a simple enough way that calculations on realistic systems are possible. The program is the result of a collaboration between British Nuclear Fuels plc and the University of Cambridge. The program has been developed with a view to making the implementation of new ideas as straightforward as possible. Hence, the code has a simple modular structure. Individual modules may of course be combined in a script to run more complicated procedures, such as a self-consistent field (SCF) procedure. The aim of such an approach is to maximize the time spent in the science compared with that spent interfacing with the computer code. For the end user a simple graphical user interface through Cerius# is provided. Standard features of the

  1. 14N overtone NMR spectra under magic angle spinning: Experiments and numerically exact simulations

    NASA Astrophysics Data System (ADS)

    O'Dell, Luke A.; Brinkmann, Andreas

    2013-02-01

    It was recently shown that high resolution 14N overtone NMR spectra can be obtained directly under magic angle spinning (MAS) conditions [L. A. O'Dell and C. I. Ratcliffe, Chem. Phys. Lett. 514, 168 (2011)], 10.1016/j.cplett.2011.08.030. Preliminary experimental results showed narrowed powder pattern widths, a frequency shift that is dependent on the MAS rate, and an apparent absence of spinning sidebands, observations which appeared to be inconsistent with previous theoretical treatments. Herein, we reproduce these effects using numerically exact simulations that take into account the full nuclear spin Hamiltonian. Under sample spinning, the 14N overtone signal is split into five (0, ±1, ±2) overtone sidebands separated by the spinning frequency. For a powder sample spinning at the magic angle, the +2ωr sideband is dominant while the others show significantly lower signal intensities. The resultant MAS powder patterns show characteristic quadrupolar lineshapes from which the 14N quadrupolar parameters and isotropic chemical shift can be determined. Spinning the sample at other angles is shown to alter both the shapes and relative intensities of the five overtone sidebands, with MAS providing the benefit of averaging dipolar couplings and shielding anisotropy. To demonstrate the advantages of this experimental approach, we present the 14N overtone MAS spectrum obtained from L-histidine, in which powder patterns from all three nitrogen sites are clearly resolved.

  2. 14N overtone NMR spectra under magic angle spinning: experiments and numerically exact simulations.

    PubMed

    O'Dell, Luke A; Brinkmann, Andreas

    2013-02-14

    It was recently shown that high resolution (14)N overtone NMR spectra can be obtained directly under magic angle spinning (MAS) conditions [L. A. O'Dell and C. I. Ratcliffe, Chem. Phys. Lett. 514, 168 (2011)]. Preliminary experimental results showed narrowed powder pattern widths, a frequency shift that is dependent on the MAS rate, and an apparent absence of spinning sidebands, observations which appeared to be inconsistent with previous theoretical treatments. Herein, we reproduce these effects using numerically exact simulations that take into account the full nuclear spin Hamiltonian. Under sample spinning, the (14)N overtone signal is split into five (0, ±1, ±2) overtone sidebands separated by the spinning frequency. For a powder sample spinning at the magic angle, the +2ω(r) sideband is dominant while the others show significantly lower signal intensities. The resultant MAS powder patterns show characteristic quadrupolar lineshapes from which the (14)N quadrupolar parameters and isotropic chemical shift can be determined. Spinning the sample at other angles is shown to alter both the shapes and relative intensities of the five overtone sidebands, with MAS providing the benefit of averaging dipolar couplings and shielding anisotropy. To demonstrate the advantages of this experimental approach, we present the (14)N overtone MAS spectrum obtained from L-histidine, in which powder patterns from all three nitrogen sites are clearly resolved.

  3. Magic angle spinning nuclear magnetic resonance apparatus and process for high-resolution in situ investigations

    SciTech Connect

    Hu, Jian Zhi; Sears, Jr., Jesse A.; Hoyt, David W.; Mehta, Hardeep S.; Peden, Charles H. F.

    2015-11-24

    A continuous-flow (CF) magic angle sample spinning (CF-MAS) NMR rotor and probe are described for investigating reaction dynamics, stable intermediates/transition states, and mechanisms of catalytic reactions in situ. The rotor includes a sample chamber of a flow-through design with a large sample volume that delivers a flow of reactants through a catalyst bed contained within the sample cell allowing in-situ investigations of reactants and products. Flow through the sample chamber improves diffusion of reactants and products through the catalyst. The large volume of the sample chamber enhances sensitivity permitting in situ .sup.13C CF-MAS studies at natural abundance.

  4. High resolution 11B NMR of magnesium diboride using cryogenic magic angle spinning

    NASA Astrophysics Data System (ADS)

    Beckett, Peter; Denning, Mark S.; Heinmaa, Ivo; Dimri, Mukesh C.; Young, Edward A.; Stern, Raivo; Carravetta, Marina

    2012-09-01

    Static and magic-angle spinning 11B nuclear magnetic resonance (NMR) data at 4.7 T and 8.5 T have been obtained under cryogenic conditions on a diluted sample of magnesium diboride powder in the normal and superconducting state. The data provide accurate information on the magnetic shift and longitudinal relaxation time down to a temperature of 8 K, with a resolution improvement over the entire temperature range. The onset of superconductivity is unaffected by the sample rotation, as revealed by a steep variation of the magnetic shift just below the critical temperature.

  5. The use of variable temperature and magic-angle sample spinning in studies of fulvic acids

    USGS Publications Warehouse

    Earl, W.L.; Wershaw, R. L.; Thorn, K.A.

    1987-01-01

    Intensity distortions and poor signal to noise in the cross-polarization magic-angle sample spinning NMR of fulvic acids were investigated and attributed to molecular mobility in these ostensibly "solid" materials. We have shown that inefficiencies in cross polarization can be overcome by lowering the sample temperature to about -60??C. These difficulties can be generalized to many other synthetic and natural products. The use of variable temperature and cross-polarization intensity as a function of contact time can yield valuable qualitative information which can aid in the characterization of many materials. ?? 1987.

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

    NASA Astrophysics Data System (ADS)

    Rosay, Melanie; Blank, Monica; Engelke, Frank

    2016-03-01

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

  7. In vivo high-resolution magic angle spinning magnetic resonance spectroscopy of Drosophila melanogaster at 14.1 T shows trauma in aging and in innate immune-deficiency is linked to reduced insulin signaling

    PubMed Central

    RIGHI, VALERIA; APIDIANAKIS, YIORGOS; MINTZOPOULOS, DIONYSSIOS; ASTRAKAS, LOUKAS; RAHME, LAURENCE G.; TZIKA, A. ARIA

    2010-01-01

    In vivo magnetic resonance spectroscopy (MRS), a non-destructive biochemical tool for investigating live organisms, has yet to be used in the fruit fly Drosophila melanogaster, a useful model organism for investigating genetics and physiology. We developed and implemented a high-resolution magic-angle-spinning (HRMAS) MRS method to investigate live Drosophila at 14.1 T. We demonstrated, for the first time, the feasibility of using HRMAS MRS for molecular characterization of Drosophila with a conventional MR spectrometer equipped with an HRMAS probe. We showed that the metabolic HRMAS MRS profiles of injured, aged wild-type (wt) flies and of immune deficient (imd) flies were more similar to chico flies mutated at the chico gene in the insulin signaling pathway, which is analogous to insulin receptor substrate 1–4 (IRS1–4) in mammals and less to those of adipokinetic hormone receptor (akhr) mutant flies, which have an obese phenotype. We thus provide evidence for the hypothesis that trauma in aging and in innate immune-deficiency is linked to insulin signaling. This link may explain the mitochondrial dysfunction that accompanies insulin resistance and muscle wasting that occurs in trauma, aging and immune system deficiencies, leading to higher susceptibility to infection. Our approach advances the development of novel in vivo non-destructive research approaches in Drosophila, suggests biomarkers for investigation of biomedical paradigms, and thus may contribute to novel therapeutic development. PMID:20596596

  8. Cryocoil magic-angle-spinning solid-state nuclear magnetic resonance probe system utilized for sensitivity enhancement in multiple-quantum magic-angle-spinning spectroscopy for a low-γ quadrupolar nucleus of 85Rb

    NASA Astrophysics Data System (ADS)

    Nakai, Toshihito; Toda, Mitsuru; Ashida, Jun; Hobo, Fumio; Endo, Yuki; Utsumi, Hiroaki; Nemoto, Takahiro; Mizuno, Takashi

    2017-06-01

    Sensitivity enhancement in solid-state nuclear magnetic resonance using a cryocoil magic-angle-spinning system was investigated, by comparing, at room temperature and at cryogenic temperature, the signal-to-noise ratios of the multiple-quantum magic-angle-spinning spectra as well as the conventional spectra for a low-γ nucleus 85Rb in RbNO3. The increase of the sample-coil quality-factor and the thermal noise reduction were found to enhance the sensitivities by approximately 4.5 times; the former yielded the further doubled signal increase in the multiple-quantum spectroscopy via the increase of the radio-frequency field strengths. Eventually, 20-30 times of the sensitivity enhancement were realized in the two-dimensional multiple-quantum magic-angle-spinning spectra.

  9. Advanced slow-magic angle spinning probe for magnetic resonance imaging and spectroscopy

    DOEpatents

    Wind, Robert A.; Hu, Jian Zhi; Minard, Kevin R.; Rommereim, Donald N.

    2006-01-24

    The present invention relates to a probe and processes useful for magnetic resonance imaging and spectroscopy instruments. More particularly, the invention relates to a MR probe and processes for obtaining resolution enhancements of fluid objects, including live specimens, using an ultra-slow (magic angle) spinning (MAS) of the specimen combined with a modified phase-corrected magic angle turning (PHORMAT) pulse sequence. Proton NMR spectra were measured of the torso and the top part of the belly of a female BALBc mouse in a 2T field, while spinning the animal at a speed of 1.5 Hz. Results show that even in this relatively low field with PHORMAT, an isotropic spectrum is obtained with line widths that are a factor 4.6 smaller than those obtained in a stationary mouse. Resolution of 1H NMR metabolite spectra are thus significantly enhanced. Results indicate that PHORMAT has the potential to significantly increase the utility of 1H NMR spectroscopy for in vivo biochemical, biomedical and/or medical applications involving large-sized biological objects such as mice, rats and even humans within a hospital setting. For small-sized objects, including biological objects, such as excised tissues, organs, live bacterial cells, and biofilms, use of PASS at a spinning rate of 30 Hz and above is preferred.

  10. Magnetic resonance imaging of DNP enhancements in a rotor spinning at the magic angle

    DOE PAGES

    Perras, Frederic A.; Kobayashi, Takeshi; Pruski, Marek

    2016-02-23

    Simulations performed on model, static, samples have shown that the microwave power is non-uniformly distributed in the magic angle spinning (MAS) rotor when using conventional dynamic nuclear polarization (DNP) instrumentation. Here, we applied the stray-field magic angle spinning imaging (STRAFI–MAS) experiment to generate a spatial map of the DNP enhancements in a full rotor, which is spun at a low rate in a commercial DNP–MAS NMR system. Notably, we observed that the enhancement factors produced in the center of the rotor can be twice as large as those produced at the top of the rotor. Surprisingly, we observed that themore » largest enhancement factors are observed along the axis of the rotor as opposed to against its walls, which are most directly irradiated by the microwave beam. We lastly observed that the distribution of enhancement factors can be moderately improved by degassing the sample and increasing the microwave power. The inclusion of dielectric particles greatly amplifies the enhancement factors throughout the rotor. Furthermore, the STRAFI–MAS approach can provide useful guidance for optimizing the access of microwave power to the sample, and thereby lead to further increases in sensitivity of DNP–MAS NMR.« less

  11. MATPASS/CPMG: a sensitivity enhanced magic-angle spinning sideband separation experiment for disordered solids.

    PubMed

    Hung, Ivan; Edwards, Trenton; Sen, Sabyasachi; Gan, Zhehong

    2012-08-01

    A Carr-Purcell Meiboom-Gill (CPMG) sensitivity-enhanced spinning sideband separation experiment is presented. The experiment combines the idea of magic-angle turning and phase-adjusted sideband separation (MATPASS), allowing for isotropic/anisotropic chemical shift separation of disordered solids with line widths far greater than the magic-angle spinning frequency. The use of CPMG enhances the sensitivity of the wide-line spectra by an order of magnitude via multiple-echo acquisition. The MATPASS/CPMG protocol involves acquisition of time-domain data using a MAT/CPMG pulse sequence followed by f(1) shearing during data processing to arrive at the PASS representation. Such a protocol has √2 higher sensitivity than the conventional PASS method because all CPMG echo signals are used for the final PASS spectrum. Application of this method is demonstrated using a GeSe₄ glass sample with both ⁷⁷Se isotropic line widths and chemical shift anisotropy that far exceed the spinning frequency. The sideband separation allows for the measurement of chemical shift anisotropy of the disordered solids.

  12. Magnetic resonance imaging of DNP enhancements in a rotor spinning at the magic angle

    SciTech Connect

    Perras, Frederic A.; Kobayashi, Takeshi; Pruski, Marek

    2016-02-23

    Simulations performed on model, static, samples have shown that the microwave power is non-uniformly distributed in the magic angle spinning (MAS) rotor when using conventional dynamic nuclear polarization (DNP) instrumentation. Here, we applied the stray-field magic angle spinning imaging (STRAFI–MAS) experiment to generate a spatial map of the DNP enhancements in a full rotor, which is spun at a low rate in a commercial DNP–MAS NMR system. Notably, we observed that the enhancement factors produced in the center of the rotor can be twice as large as those produced at the top of the rotor. Surprisingly, we observed that the largest enhancement factors are observed along the axis of the rotor as opposed to against its walls, which are most directly irradiated by the microwave beam. We lastly observed that the distribution of enhancement factors can be moderately improved by degassing the sample and increasing the microwave power. The inclusion of dielectric particles greatly amplifies the enhancement factors throughout the rotor. Furthermore, the STRAFI–MAS approach can provide useful guidance for optimizing the access of microwave power to the sample, and thereby lead to further increases in sensitivity of DNP–MAS NMR.

  13. Isotropic diffusion weighting in PGSE NMR by magic-angle spinning of the q-vector.

    PubMed

    Eriksson, Stefanie; Lasic, Samo; Topgaard, Daniel

    2013-01-01

    When PGSE NMR is applied to water in microheterogeneous materials such as liquid crystals, foodstuffs, porous rocks, and biological tissues, the signal attenuation is often multi-exponential, indicating the presence of pores having a range of sizes or anisotropic domains having a spread of orientations. Here we modify the standard PGSE experiment by introducing low-amplitude harmonically modulated gradients, which effectively make the q-vector perform magic-angle spinning (MAS) about an axis fixed in the laboratory frame. With this new technique, denoted q-MAS PGSE, the signal attenuation depends on the isotropic average of the local diffusion tensor. The capability of q-MAS PGSE to distinguish between pore size and domain orientation dispersion is demonstrated by experiments on a yeast cell suspension and a polydomain anisotropic liquid crystal. In the latter case, the broad distribution of apparent diffusivities observed with PGSE is narrowed to its isotropic average with q-MAS PGSE in a manner that is analogous to the narrowing of chemical shift anisotropy powder patterns using magic-angle sample spinning in solid-state NMR. The new q-MAS PGSE technique could be useful for resolving size/orientation ambiguities in the interpretation of PGSE data from, e.g., water confined within the axons of human brain tissue. Copyright © 2012 Elsevier Inc. All rights reserved.

  14. A MR compatible mechatronic system to facilitate magic angle experiments in vivo.

    PubMed

    Elhawary, Haytham; Zivanovic, Aleksandar; Rea, Marc; Tse, Zion Tsz Ho; McRobbie, Donald; Young, Ian; Paley, Martyn; Davies, Brian; Lampérth, Michael

    2007-01-01

    When imaging tendons and cartilage in a MRI scanner, an increase in signal intensity is observed when they are oriented at 55 degrees with respect to Bo (the "magic angle"). There is a clear clinical importance for considering this effect as part of the diagnosis of orthopaedic and other injury. Experimental studies of this phenomenon have been made harder by practical difficulties of tissue positioning and orientation in the confined environment of cylindrical scanners. An MRI compatible mechatronic system has been developed to position a variety of limbs inside the field of view of the scanner, to be used as a diagnostic and research tool. It is actuated with a novel pneumatic motor comprised of a heavily geared down air turbine, and is controlled in a closed loop using standard optical encoders. MR compatibility is demonstrated as well as the results of preliminary trials used to image the Achilles tendon of human volunteers at different orientations. A 4 to 13 fold increase in signal at the tendon is observed at the magic angle.

  15. Magnetic resonance imaging of DNP enhancements in a rotor spinning at the magic angle.

    PubMed

    Perras, Frédéric A; Kobayashi, Takeshi; Pruski, Marek

    2016-03-01

    Simulations performed on model, static, samples have shown that the microwave power is non-uniformly distributed in the magic angle spinning (MAS) rotor when using conventional dynamic nuclear polarization (DNP) instrumentation. Here, we applied the stray-field magic angle spinning imaging (STRAFI-MAS) experiment to generate a spatial map of the DNP enhancements in a full rotor, which is spun at a low rate in a commercial DNP-MAS NMR system. Notably, we observed that the enhancement factors produced in the center of the rotor can be twice as large as those produced at the top of the rotor. Surprisingly, we observed that the largest enhancement factors are observed along the axis of the rotor as opposed to against its walls, which are most directly irradiated by the microwave beam. We lastly observed that the distribution of enhancement factors can be moderately improved by degassing the sample and increasing the microwave power. The inclusion of dielectric particles greatly amplifies the enhancement factors throughout the rotor. The STRAFI-MAS approach can provide useful guidance for optimizing the access of microwave power to the sample, and thereby lead to further increases in sensitivity of DNP-MAS NMR. Published by Elsevier Inc.

  16. Method for high resolution magnetic resonance analysis using magic angle technique

    DOEpatents

    Wind, Robert A.; Hu, Jian Zhi

    2003-11-25

    A method of performing a magnetic resonance analysis of a biological object that includes placing the biological object in a main magnetic field and in a radio frequency field, the main magnetic field having a static field direction; rotating the biological object at a rotational frequency of less than about 100 Hz around an axis positioned at an angle of about 54.degree.44' relative to the main magnetic static field direction; pulsing the radio frequency to provide a sequence that includes a magic angle turning pulse segment; and collecting data generated by the pulsed radio frequency. According to another embodiment, the radio frequency is pulsed to provide a sequence capable of producing a spectrum that is substantially free of spinning sideband peaks.

  17. The effect of Hartmann-Hahn mismatching on polarization inversion spin exchange at the magic angle.

    PubMed

    Fu, Riqiang; Tian, Changlin; Kim, Hyeongnam; Smith, Scott A; Cross, Timothy A

    2002-12-01

    The effect of the Hartmann-Hahn mismatch delta = omega(eff)-omega(1S) during polarization inversion spin exchange at the magic angle (PISEMA) has been investigated, where omega(eff) and omega(1S) represent the amplitudes of the 1H effective spin-locking field at the magic angle and the 15N RF spin-locking field, respectively. During the PISEMA evolution period, the exact Hartmann-Hahn match condition (i.e., delta = 0) yields a maximum dipolar scaling factor of 0.816 for PISEMA experiments, while any mismatch results in two different effective fields for the first and second half of each frequency switched Lee-Goldburg (FSLG) cycle. The mismatch effect on the scaling factor depends strongly on the transition angle from one effective field to the other within each FSLG cycle as well as on the cycle time. At low RF spin-lock amplitudes in which the FSLG cycle time is relatively long, the scaling factor rapidly becomes smaller as omega(1S) becomes greater than omega(eff). On the other hand, when omega(1S) < omega(eff), there is relatively little effect on the scaling factor with variation in delta. As a result, the presence of RF inhomogeneities may significantly broaden the line-width in the dipolar dimension because of the mismatch effect. Higher RF spin-lock amplitudes result in a relatively small variation for the scaling factor. Furthermore, ramped amplitude of the 15N RF spin-lock field in synchronization with the flip-flop of the FSLG sequence minimizes the transition angle between the two effective fields within the FSLG cycle. It is shown experimentally that such a ramped amplitude not only gives rise to the same scaling factor but also results in a narrower dipolar line-width in comparison with the rectangular amplitude.

  18. Magic angle-enhanced MRI of fibrous microstructures in sclera and cornea with and without intraocular pressure loading.

    PubMed

    Ho, Leon C; Sigal, Ian A; Jan, Ning-Jiun; Squires, Alexander; Tse, Zion; Wu, Ed X; Kim, Seong-Gi; Schuman, Joel S; Chan, Kevin C

    2014-08-07

    The structure and biomechanics of the sclera and cornea are central to several eye diseases such as glaucoma and myopia. However, their roles remain unclear, partly because of limited noninvasive techniques to assess their fibrous microstructures globally, longitudinally, and quantitatively. We hypothesized that magic angle-enhanced magnetic resonance imaging (MRI) can reveal the structural details of the corneoscleral shell and their changes upon intraocular pressure (IOP) elevation. Seven ovine eyes were extracted and fixed at IOP = 50 mm Hg to mimic ocular hypertension, and another 11 eyes were unpressurized. The sclera and cornea were scanned at different angular orientations relative to the main magnetic field inside a 9.4-Tesla MRI scanner. Relative MRI signal intensities and intrinsic transverse relaxation times (T2 and T2*) were determined to quantify the magic angle effect on the corneoscleral shells. Three loaded and eight unloaded tendon samples were scanned as controls. At magic angle, high-resolution MRI revealed distinct scleral and corneal lamellar fibers, and light/dark bands indicative of collagen fiber crimps in the sclera and tendon. Magic angle enhancement effect was the strongest in tendon and the least strong in cornea. Loaded sclera, cornea, and tendon possessed significantly higher T2 and T2* than unloaded tissues at magic angle. Magic angle-enhanced MRI can detect ocular fibrous microstructures without contrast agents or coatings and can reveal their MR tissue property changes with IOP loading. This technique may open up new avenues for assessment of the biomechanical and biochemical properties of ocular tissues in aging and in diseases involving the corneoscleral shell. Copyright 2014 The Association for Research in Vision and Ophthalmology, Inc.

  19. MAPS - a Magic Angle Positioning System for Enhanced Imaging in High-Field Small-Bore MRI.

    PubMed

    Squires, Alexander; Chan, Kevin C; Ho, Leon C; Sigal, Ian A; Jan, Ning-Jiun; Tse, Zion Tsz Ho

    2016-03-01

    The "magic angle" MRI effect can enhance signal intensity in aligned collagenous structures oriented at approximately 55° with respect to the main magnetic field. The difficulty of positioning tissue inside closed-bore scanners has hampered magic angle use in research and clinics. An MRI-conditional mechatronic system has been developed to control sample orientation inside a 9.4T small bore MRI scanner. The system orients samples to within 0.5° and enables a 600% increase in tendon signal intensity.

  20. Method for non-destructive testing

    DOEpatents

    Akers, Douglas W [Idaho Falls, ID

    2011-08-30

    Non-destructive testing method may include providing a source material that emits positrons in response to bombardment of the source material with photons. The source material is exposed to photons. The source material is positioned adjacent the specimen, the specimen being exposed to at least some of the positrons emitted by the source material. Annihilation gamma rays emitted by the specimen are detected.

  1. Efficient dipolar double quantum filtering under magic angle spinning without a 1H decoupling field

    NASA Astrophysics Data System (ADS)

    Courtney, Joseph M.; Rienstra, Chad M.

    2016-08-01

    We present a systematic study of dipolar double quantum (DQ) filtering in 13C-labeled organic solids over a range of magic-angle spinning rates, using the SPC-n recoupling sequence element with a range of n symmetry values from 3 to 11. We find that efficient recoupling can be achieved for values n ⩾ 7, provided that the 13C nutation frequency is on the order of 100 kHz or greater. The decoupling-field dependence was investigated and explicit heteronuclear decoupling interference conditions identified. The major determinant of DQ filtering efficiency is the decoupling interference between 13C and 1H fields. For 13C nutation frequencies greater than 75 kHz, optimal performance is observed without an applied 1H field. At spinning rates exceeding 20 kHz, symmetry conditions as low as n = 3 were found to perform adequately.

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

    PubMed

    Rosay, Melanie; Blank, Monica; Engelke, Frank

    2016-03-01

    Advances in dynamic nuclear polarization (DNP) instrumentation and methodology have been key factors in the recent growth of solid-state DNP NMR applications. We review the current state of the art of solid-state DNP NMR instrumentation primarily based on available commercial platforms. We start with a general system overview, including options for microwave sources and DNP NMR probes, and then focus on specific developments for DNP at 100K with magic angle spinning (MAS). Gyrotron microwave sources, passive components to transmit microwaves, the DNP MAS probe, a cooling device for low-temperature MAS, and sample preparation procedures including radicals for DNP are considered. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. High resolution 11B NMR of MgB2 using cryogenic magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Stern, Raivo; Beckett, Peter; Denning, Mark S.; Heinmaa, Ivo; Dimri, Mukesh C.; Young, Edward A.; Carravetta, Marina

    2013-03-01

    Static and magic-angle spinning (MAS) 11B NMR data at 4.7 T and 8.5 T have been obtained under cryogenic conditions on a diluted sample of magnesium diboride powder in the normal and superconducting state. We demonstrate that MAS NMR is possible on type-II superconductors despite the sample rotation. The data provide accurate information on the magnetic shift variation and longitudinal relaxation data down to a temperature of 8 K, with a resolution improvement over the entire temperature range. The onset of superconductivity is unaffected by the sample rotation, as revealed by a steep variation of the magnetic shift just below the critical temperature. Appeared in JCP 137, 114201, http://dx.doi.org/10.1063/1.4751476

  4. Magic-angle spinning NMR of intact bacteriophages: Insights into the capsid, DNA and their interface

    NASA Astrophysics Data System (ADS)

    Abramov, Gili; Morag, Omry; Goldbourt, Amir

    2015-04-01

    Bacteriophages are viruses that infect bacteria. They are complex macromolecular assemblies, which are composed of multiple protein subunits that protect genomic material and deliver it to specific hosts. Various biophysical techniques have been used to characterize their structure in order to unravel phage morphogenesis. Yet, most bacteriophages are non-crystalline and have very high molecular weights, in the order of tens of MegaDaltons. Therefore, complete atomic-resolution characterization on such systems that encompass both capsid and DNA is scarce. In this perspective article we demonstrate how magic-angle spinning solid-state NMR has and is used to characterize in detail bacteriophage viruses, including filamentous and icosahedral phage. We discuss the process of sample preparation, spectral assignment of both capsid and DNA and the use of chemical shifts and dipolar couplings to probe the capsid-DNA interface, describe capsid structure and dynamics and extract structural differences between viruses.

  5. Magic-angle spinning NMR of intact bacteriophages: insights into the capsid, DNA and their interface.

    PubMed

    Abramov, Gili; Morag, Omry; Goldbourt, Amir

    2015-04-01

    Bacteriophages are viruses that infect bacteria. They are complex macromolecular assemblies, which are composed of multiple protein subunits that protect genomic material and deliver it to specific hosts. Various biophysical techniques have been used to characterize their structure in order to unravel phage morphogenesis. Yet, most bacteriophages are non-crystalline and have very high molecular weights, in the order of tens of MegaDaltons. Therefore, complete atomic-resolution characterization on such systems that encompass both capsid and DNA is scarce. In this perspective article we demonstrate how magic-angle spinning solid-state NMR has and is used to characterize in detail bacteriophage viruses, including filamentous and icosahedral phage. We discuss the process of sample preparation, spectral assignment of both capsid and DNA and the use of chemical shifts and dipolar couplings to probe the capsid-DNA interface, describe capsid structure and dynamics and extract structural differences between viruses.

  6. The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning

    SciTech Connect

    Mance, Deni; Baldus, Marc; Gast, Peter; Huber, Martina; Ivanov, Konstantin L.

    2015-06-21

    We develop a theoretical description of Dynamic Nuclear Polarization (DNP) in solids under Magic Angle Spinning (MAS) to describe the magnetic field dependence of the DNP effect. The treatment is based on an efficient scheme for numerical solution of the Liouville-von Neumann equation, which explicitly takes into account the variation of magnetic interactions during the sample spinning. The dependence of the cross-effect MAS-DNP on various parameters, such as the hyperfine interaction, electron-electron dipolar interaction, microwave field strength, and electron spin relaxation rates, is analyzed. Electron spin relaxation rates are determined by electron paramagnetic resonance measurements, and calculations are compared to experimental data. Our results suggest that the observed nuclear magnetic resonance signal enhancements provided by MAS-DNP can be explained by discriminating between “bulk” and “core” nuclei and by taking into account the slow DNP build-up rate for the bulk nuclei.

  7. The magnetic field dependence of cross-effect dynamic nuclear polarization under magic angle spinning.

    PubMed

    Mance, Deni; Gast, Peter; Huber, Martina; Baldus, Marc; Ivanov, Konstantin L

    2015-06-21

    We develop a theoretical description of Dynamic Nuclear Polarization (DNP) in solids under Magic Angle Spinning (MAS) to describe the magnetic field dependence of the DNP effect. The treatment is based on an efficient scheme for numerical solution of the Liouville-von Neumann equation, which explicitly takes into account the variation of magnetic interactions during the sample spinning. The dependence of the cross-effect MAS-DNP on various parameters, such as the hyperfine interaction, electron-electron dipolar interaction, microwave field strength, and electron spin relaxation rates, is analyzed. Electron spin relaxation rates are determined by electron paramagnetic resonance measurements, and calculations are compared to experimental data. Our results suggest that the observed nuclear magnetic resonance signal enhancements provided by MAS-DNP can be explained by discriminating between "bulk" and "core" nuclei and by taking into account the slow DNP build-up rate for the bulk nuclei.

  8. Non-Fermi-liquid magic angle effects in high magnetic fields

    NASA Astrophysics Data System (ADS)

    Lebed, A. G.

    2016-07-01

    We investigate a theoretical problem of electron-electron interactions in an inclined magnetic field in a quasi-one-dimensional (Q1D) conductor. We show that they result in strong non-Fermi-liquid corrections to a specific heat, provided that the direction of the magnetic field is far from the so-called Lebed's magic angles (LMAs). If magnetic field is directed close to one of the LMAs, the specific heat corrections become small and the Fermi-liquid picture restores. As a result, we predict Fermi-liquid-non-Fermi-liquid angular crossovers in the vicinities of the LMA directions of the field. We suggest to perform the corresponding experiment in the Q1D conductor (Per) 2Au (mnt) 2 under pressure in magnetic fields of the order of H ≃25 T .

  9. Applications of high-resolution magic angle spinning MRS in biomedical studies II-Human diseases.

    PubMed

    Dietz, Christopher; Ehret, Felix; Palmas, Francesco; Vandergrift, Lindsey A; Jiang, Yanni; Schmitt, Vanessa; Dufner, Vera; Habbel, Piet; Nowak, Johannes; Cheng, Leo L

    2017-09-15

    High-resolution magic angle spinning (HRMAS) MRS is a powerful method for gaining insight into the physiological and pathological processes of cellular metabolism. Given its ability to obtain high-resolution spectra of non-liquid biological samples, while preserving tissue architecture for subsequent histopathological analysis, the technique has become invaluable for biochemical and biomedical studies. Using HRMAS MRS, alterations in measured metabolites, metabolic ratios, and metabolomic profiles present the possibility to improve identification and prognostication of various diseases and decipher the metabolomic impact of drug therapies. In this review, we evaluate HRMAS MRS results on human tissue specimens from malignancies and non-localized diseases reported in the literature since the inception of the technique in 1996. We present the diverse applications of the technique in understanding pathological processes of different anatomical origins, correlations with in vivo imaging, effectiveness of therapies, and progress in the HRMAS methodology. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Rapid proton-detected NMR assignment for proteins with fast magic angle spinning.

    PubMed

    Barbet-Massin, Emeline; Pell, Andrew J; Retel, Joren S; Andreas, Loren B; Jaudzems, Kristaps; Franks, W Trent; Nieuwkoop, Andrew J; Hiller, Matthias; Higman, Victoria; Guerry, Paul; Bertarello, Andrea; Knight, Michael J; Felletti, Michele; Le Marchand, Tanguy; Kotelovica, Svetlana; Akopjana, Inara; Tars, Kaspars; Stoppini, Monica; Bellotti, Vittorio; Bolognesi, Martino; Ricagno, Stefano; Chou, James J; Griffin, Robert G; Oschkinat, Hartmut; Lesage, Anne; Emsley, Lyndon; Herrmann, Torsten; Pintacuda, Guido

    2014-09-03

    Using a set of six (1)H-detected triple-resonance NMR experiments, we establish a method for sequence-specific backbone resonance assignment of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of 5-30 kDa proteins. The approach relies on perdeuteration, amide (2)H/(1)H exchange, high magnetic fields, and high-spinning frequencies (ωr/2π ≥ 60 kHz) and yields high-quality NMR data, enabling the use of automated analysis. The method is validated with five examples of proteins in different condensed states, including two microcrystalline proteins, a sedimented virus capsid, and two membrane-embedded systems. In comparison to contemporary (13)C/(15)N-based methods, this approach facilitates and accelerates the MAS NMR assignment process, shortening the spectral acquisition times and enabling the use of unsupervised state-of-the-art computational data analysis protocols originally developed for solution NMR.

  11. Magic-angle-spinning NMR studies of acid sites in zeolite H-ZSM-5

    SciTech Connect

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

    1991-01-01

    {sup 1}H, {sup 13}C, {sup 27}Al, and {sup 29}Si magic-angle-spinning (MAS) NMR was used to elucidate the nature of the catalytic activity of zeolite H-ZSM-5. {sup 1}H MAS NMR of sealed samples after mild hydrothermal dealumination shows that the enhanced activity for n-hexane cracking is not due to an enhanced Bronstead acidity. The concentrations of the various OH groups and aluminous species suggest that the reason for the enhanced catalytic activity is the interaction of the n-hexane molecule with a bridging hydroxyl group and with extra-framework aluminium species, which give rise to the enhanced activity, cannot be easily removed from their positions, and are therefore immobilized by the zeolitic framework.

  12. Rapid Proton-Detected NMR Assignment for Proteins with Fast Magic Angle Spinning

    PubMed Central

    2015-01-01

    Using a set of six 1H-detected triple-resonance NMR experiments, we establish a method for sequence-specific backbone resonance assignment of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of 5–30 kDa proteins. The approach relies on perdeuteration, amide 2H/1H exchange, high magnetic fields, and high-spinning frequencies (ωr/2π ≥ 60 kHz) and yields high-quality NMR data, enabling the use of automated analysis. The method is validated with five examples of proteins in different condensed states, including two microcrystalline proteins, a sedimented virus capsid, and two membrane-embedded systems. In comparison to contemporary 13C/15N-based methods, this approach facilitates and accelerates the MAS NMR assignment process, shortening the spectral acquisition times and enabling the use of unsupervised state-of-the-art computational data analysis protocols originally developed for solution NMR. PMID:25102442

  13. Characterization of two forms of cadmium phosphide by magic-angle spinning 31P NMR.

    PubMed

    Holl, S M; Kowalewski, T; Schaefer, J

    1996-02-01

    Annealing of commercial grade cadmium phosphide (CD3P2) at 600 K produces a material which, in magic-angle spinning spin-lattice 31P NMR relaxation experiments, has broad lines and multiple T1 values. By contrast, sublimation at 900 K results in a crystalline material with narrow lines and a single T1. However, both materials have the same Cd-P lattice spacings as determined by rotational-echo, double-resonance 31P NMR with 113Cd dephasing. Both materials also have closely similar X-ray diffraction powder patterns. These results are interpreted in terms of a distribution of lattice vacancies in the annealed material, creating structural heterogeneity but with no substantial change in lattice parameters from those of the sublimed cadmium phosphide.

  14. Efficient dipolar double quantum filtering under magic angle spinning without a (1)H decoupling field.

    PubMed

    Courtney, Joseph M; Rienstra, Chad M

    2016-08-01

    We present a systematic study of dipolar double quantum (DQ) filtering in (13)C-labeled organic solids over a range of magic-angle spinning rates, using the SPC-n recoupling sequence element with a range of n symmetry values from 3 to 11. We find that efficient recoupling can be achieved for values n⩾7, provided that the (13)C nutation frequency is on the order of 100kHz or greater. The decoupling-field dependence was investigated and explicit heteronuclear decoupling interference conditions identified. The major determinant of DQ filtering efficiency is the decoupling interference between (13)C and (1)H fields. For (13)C nutation frequencies greater than 75kHz, optimal performance is observed without an applied (1)H field. At spinning rates exceeding 20kHz, symmetry conditions as low as n=3 were found to perform adequately.

  15. Magic Angle Spinning NMR Spectroscopy: A Versatile Technique for Structural and Dynamic Analysis of Solid-Phase Systems

    PubMed Central

    Polenova, Tatyana; Gupta, Rupal; Goldbourt, Amir

    2016-01-01

    Magic Angle Spinning (MAS) NMR spectroscopy is a powerful method for analysis of a broad range of systems, including inorganic materials, pharmaceuticals, and biomacromolecules. The recent developments in MAS NMR instrumentation and methodologies opened new vistas to atomic-level characterization of a plethora of chemical environments previously inaccessible to analysis, with unprecedented sensitivity and resolution. PMID:25794311

  16. Adiabatic sweep cross-polarization magic-angle-spinning NMR of half-integer quadrupolar spins

    NASA Astrophysics Data System (ADS)

    Wi, Sungsool; Kim, Chul; Schurko, Robert; Frydman, Lucio

    2017-04-01

    The use of frequency-swept radiofrequency (rf) pulses for enhancing signals in the magic-angle spinning (MAS) spectra of half-integer quadrupolar nuclides was explored. The broadband adiabatic inversion cross-polarization magic-angle spinning (BRAIN-CPMAS) method, involving an adiabatic inversion pulse on the S-channel and a simultaneous rectangular spin-lock pulse on the I-channel (1H), was applied to I(1/2) → S(3/2) systems. Optimal BRAIN-CPMAS matching conditions were found to involve low rf pulse strengths for both the I- and S-spin channels. At these low and easily attainable rf field strengths, level-crossing events among the energy levels | 3 / 2 >, | 1 / 2 >, | - 1 / 2 >, | - 3 / 2 > that are known to complicate the CPMAS of quadrupolar nuclei, are mostly avoided. Zero- and double-quantum polarization transfer modes, akin to those we have observed for I(1/2) → S(1/2) polarization transfers, were evidenced by these analyses even in the presence of the quadrupolar interaction. 1H-23Na and 1H-11B BRAIN-CPMAS conditions were experimentally explored on model compounds by optimizing the width of the adiabatic sweep, as well as the rf pulse powers of the 1H and 23Na/11B channels, for different MAS rates. The experimental data obtained on model compounds containing spin-3/2 nuclides, matched well predictions from numerical simulations and from an average Hamiltonian theory model. Extensions to half-integer spin nuclides with higher spins and potential applications of this BRAIN-CPMAS approach are discussed.

  17. Hybrid holographic non-destructive test system

    NASA Technical Reports Server (NTRS)

    Kurtz, R. L. (Inventor)

    1978-01-01

    An automatic hybrid holographic non-destructive testing (HNDT) method and system capable of detecting flaws or debonds contained within certain materials are described. This system incorporates the techniques of optical holography, acoustical/optical holography and holographic correlation in determining the structural integrity of a test object. An automatic processing system including a detector and automatic data processor is used in conjunction with the three holographic techniques for correlating and interpreting the information supplied by the non-destructive systems. The automatic system also includes a sensor which directly translates an optical data format produced by the holographic techniques into electrical signals and then transmits this information to a digital computer for indicating the structural properties of the test object. The computer interprets the data gathered and determines whether further testing is necessary as well as the format of this new testing procedure.

  18. Non-Destructive State Machine Reverse Engineering

    SciTech Connect

    Smith, Jessica L.

    2013-10-10

    Most of the integrated circuits (ICs) that are in electronic systems today are based on state machines. We are taking advantage of this to develop a hardware reverse engineering method that discovers the IC’s underlying state machine, rather than its transistors and gates. While there are other methods for destructively reverse engineering ICs or for non-destructively characterizing ICs, our method offers a fast and accurate analysis while remaining non-destructive. To do this, we present an intelligent brute-force method of exploring the logic of the IC using only the input and outputs designed into the IC - the I/O pins. From this exploration, we can apply a folding algorithm to discover the designed state machine.

  19. Non-Destructive Evaluation of Aerospace Composites

    DTIC Science & Technology

    2009-03-01

    Master of Science in Materials Science Jeremy D. Johnson, BS Captain, USAF March 2009 APPROVED FOR PUBLIC RELEASE; DISTRIBUTION UNLIMITED...non-destructive material evaluation (NDE) were used to inspect various forms of damage commonly found in aerospace fiberglass composites: voids...ultrasound, and flash IR thermography were analyzed for the detection of defects. Test results and analysis of each NDE method’s capabilities

  20. MAPS – a Magic Angle Positioning System for Enhanced Imaging in High-Field Small-Bore MRI

    PubMed Central

    Squires, Alexander; Chan, Kevin C.; Ho, Leon C.; Sigal, Ian A.; Jan, Ning-Jiun

    2016-01-01

    The “magic angle” MRI effect can enhance signal intensity in aligned collagenous structures oriented at approximately 55° with respect to the main magnetic field. The difficulty of positioning tissue inside closed-bore scanners has hampered magic angle use in research and clinics. An MRI-conditional mechatronic system has been developed to control sample orientation inside a 9.4T small bore MRI scanner. The system orients samples to within 0.5° and enables a 600% increase in tendon signal intensity. PMID:28713864

  1. In vivo high-resolution magic angle spinning proton NMR spectroscopy of Drosophila melanogaster flies as a model system to investigate mitochondrial dysfunction in Drosophila GST2 mutants.

    PubMed

    Righi, Valeria; Apidianakis, Yiorgos; Psychogios, Nikolaos; Rahme, Laurence G; Tompkins, Ronald G; Tzika, A Aria

    2014-07-01

    In vivo nuclear magnetic resonance spectroscopy (NMR), a non-destructive biochemical tool used for investigating live organisms, has recently been performed in studies of the fruit fly Drosophila melanogaster, a useful model organism for investigating genetics and physiology. We used a novel high-resolution magic angle-spinning (HRMAS) NMR method to investigate live Drosophila GST2 mutants using a conventional 14.1-T NMR spectrometer equipped with an HRMAS probe. The results showed that, compared to wild-type (wt) controls, the GST2 mutants had a 48% greater (CH(2))n lipid signal at 1.33 ppm, which is an insulin resistance biomarker in Drosophila skeletal muscle (P=0.0444). The mutants also had a 57% greater CH(2)C= lipid signal at 2.02 ppm (P=0.0276) and a 100% greater -CH=CH- signal at 5.33 ppm (P=0.0251). Since the -CH=CH- signal encompasses protons from ceramide, this latter difference is consistent with the hypothesis that the GST2 mutation is associated with insulin resistance and apoptosis. The findings of this study corroborate our previous results, support the hypothesis that the GST2 mutation is associated with insulin signaling and suggest that the IMCL level may be a biomarker of insulin resistance. Furthermore, direct links between GST2 mutation (the Drosophila ortholog of the GSTA4 gene in mammals) and insulin resistance, as suggested in this study, have not been made previously. These findings may thus be directly relevant to a wide range of metabolically disruptive conditions, such as trauma, aging and immune system deficiencies, that lead to increased susceptibility to infection.

  2. Magic-angle sample spinning electron paramagnetic resonance--instrumentation, performance, and limitations.

    PubMed

    Hessinger, D; Bauer, C; Hubrich, M; Jeschke, G; Spiess, H W

    2000-12-01

    An electron paramagnetic resonance (EPR) setup for line narrowing experiments with fast sample spinning at variable angles between the rotation axis and the static magnetic field is described and applied in the magic-angle sample spinning (MAS) EPR experiment at X-band frequencies (9.5 GHz). Sample spinning speeds up to 17 kHz at temperatures down to 200 K can be achieved with rotors of 4-mm outer and 2.5-mm inner diameter without severe losses in microwave amplitude compared to standard pulse EPR probeheads. A phase cycle is introduced that provides pure absorption MAS EPR spectra and allows one to distinguish between positive and negative frequency offsets (pseudo-quadrature detection). Possible broadening mechanisms in MAS EPR spectra are discussed. It is demonstrated both by theory and by experiment that the MAS EPR experiment requires excitation bandwidths that are comparable to the total spectral width, since otherwise destructive interference between contributions of spins with similar resonance offsets suppresses the signal. Experimental observations on the E(1) center in gamma-irradiated silica glass and on the SO(-)(3) radical in gamma-irradiated sulfamic acid are reported.

  3. Structural characterization of GNNQQNY amyloid fibrils by magic angle spinning NMR.

    PubMed

    van der Wel, Patrick C A; Lewandowski, Józef R; Griffin, Robert G

    2010-11-09

    Several human diseases are associated with the formation of amyloid aggregates, but experimental characterization of these amyloid fibrils and their oligomeric precursors has remained challenging. Experimental and computational analysis of simpler model systems has therefore been necessary, for instance, on the peptide fragment GNNQQNY7−13 of yeast prion protein Sup35p. Expanding on a previous publication, we report here a detailed structural characterization of GNNQQNY fibrils using magic angle spinning (MAS) NMR. On the basis of additional chemical shift assignments we confirm the coexistence of three distinct peptide conformations within the fibrillar samples, as reflected in substantial chemical shift differences. Backbone torsion angle measurements indicate that the basic structure of these coexisting conformers is an extended β-sheet. We structurally characterize a previously identified localized distortion of the β-strand backbone specific to one of the conformers. Intermolecular contacts are consistent with each of the conformers being present in its own parallel and in-register sheet. Overall the MAS NMR data indicate a substantial difference between the structure of the fibrillar and crystalline forms of these peptides, with a clearly increased complexity in the GNNQQNY fibril structure. These experimental data can provide guidance for future work, both experimental and theoretical, and provide insights into the distinction between fibril growth and crystal formation.

  4. Magic angle effect plays a major role in both T1rho and T2 relaxation in articular cartilage.

    PubMed

    Shao, H; Pauli, C; Li, S; Ma, Y; Tadros, A S; Kavanaugh, A; Chang, E Y; Tang, G; Du, J

    2017-02-01

    To investigate the effect of sample orientation on T1rho and T2 values of articular cartilage in histologically confirmed normal and abnormal regions using a whole-body 3T scanner. Eight human cadaveric patellae were evaluated using a 2D CPMG sequence for T2 measurement as well as a 2D spin-locking prepared spiral sequence and a 3D magnetization-prepared angle-modulated partitioned-k-space spoiled gradient echo snapshots (3D MAPSS) sequence for T1rho measurement. Each sample was imaged at six angles from 0° to 100° relative to the B0 field. T2 and T1rho values were measured for three regions (medial, apex and lateral) with three layers (10% superficial, 60% middle, 30% deep). Multiple histopathologically confirmed normal and abnormal regions were used to evaluate the angular dependence of T2 and T1rho relaxation in articular cartilage. Our study demonstrated a strong magic angle effect for T1rho and T2 relaxation in articular cartilage, especially in the deeper layers of cartilage. On average, T2 values were increased by 231.8% (72.2% for superficial, 237.6% for middle, and 187.9% for deep layers) while T1rho values were increased by 92% (31.7% for superficial, 69% for middle, and 140% for deep layers) near the magic angle. Both normal and abnormal cartilage showed similar T1rho and T2 magic angle effect. Changes in T1rho and T2 values due to the magic angle effect can be several times more than that caused by degeneration, and this may significantly complicate the clinical application of T1rho and T2 as an early surrogate marker for degeneration. Copyright © 2017 Osteoarthritis Research Society International. Published by Elsevier Ltd. All rights reserved.

  5. FIRST 100 T NON-DESTRUCTIVE MAGNET

    SciTech Connect

    J. R. SIMS; ET AL

    1999-10-01

    The first 100 T non-destructive (100 T ND) magnet and power supplies as currently designed are described. This magnet will be installed as part of the user facility research equipment at the National High Magnetic Field Laboratory (NHMFL) Pulsed Field Facility at Los Alamos National Laboratory. The 100 T ND magnet will provide a 100 T pulsed field of 5 ms duration (above 90% of full field) in a 15 mm diameter bore once per hour. Magnet operation will be non-destructive. The magnet will consist of a controlled power outer coil set which produces a 47 T platform field in a 225 mm diameter bore. Located within the outer coil set will be a 220 mm outer diameter capacitor powered insert coil. Using inertial energy storage a synchronous motor/generator will provide ac power to a set of seven ac-dc converters rated at 64 MW/80 MVA each. These converters will energize three independent coil circuits to create 170 MJ of field energy in the outer coil set at the platform field of 47 T. The insert will then be energized to produce the balance of the 100 T peak field using a 2.3 MJ, 18 kV (charged to 15 kV), 14.4 mF capacitor bank controlled with solid-state switches. The magnet will be the first of its kind and the first non-destructive, reusable 100 T pulsed magnet. The operation of the magnet will be described along with special features of its design and construction.

  6. Recoupling of chemical shift anisotropy by R-symmetry sequences in magic angle spinning NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Hou, Guangjin; Byeon, In-Ja L.; Ahn, Jinwoo; Gronenborn, Angela M.; Polenova, Tatyana

    2012-10-01

    13C and 15N chemical shift (CS) interaction is a sensitive probe of structure and dynamics in a wide variety of biological and inorganic systems, and in the recent years several magic angle spinning NMR approaches have emerged for residue-specific measurements of chemical shift anisotropy (CSA) tensors in uniformly and sparsely enriched proteins. All of the currently existing methods are applicable to slow and moderate magic angle spinning (MAS) regime, i.e., MAS frequencies below 20 kHz. With the advent of fast and ultrafast MAS probes capable of spinning frequencies of 40-100 kHz, and with the superior resolution and sensitivity attained at such high frequencies, development of CSA recoupling techniques working under such conditions is necessary. In this work, we present a family of R-symmetry based pulse sequences for recoupling of 13C/15N CSA interactions that work well in both natural abundance and isotopically enriched systems. We demonstrate that efficient recoupling of either first-rank (σ1) or second-rank (σ2) spatial components of CSA interaction is attained with appropriately chosen γ-encoded RNnv symmetry sequences. The advantage of these γ-encoded RNnv-symmetry based CSA (RNCSA) recoupling schemes is that they are suitable for CSA recoupling under a wide range of MAS frequencies, including fast MAS regime. Comprehensive analysis of the recoupling properties of these RNnv symmetry sequences reveals that the σ1-CSA recoupling symmetry sequences exhibit large scaling factors; however, the partial homonuclear dipolar Hamiltonian components are symmetry allowed, which makes this family of sequences suitable for CSA measurements in systems with weak homonuclear dipolar interactions. On the other hand, the γ-encoded symmetry sequences for σ2-CSA recoupling have smaller scaling factors but they efficiently suppress the homonuclear dipole-dipole interactions. Therefore, the latter family of sequences is applicable for measurements of CSA parameters in

  7. Complementary Electromagnetic Non-Destructive Evaluation

    NASA Astrophysics Data System (ADS)

    Tian, Gui Yun; Wilson, John; Morozov, Maxim

    2011-06-01

    The use of non-destructive evaluation (NDE) for defect detection and failure prediction in structures and specimens is widespread in energy industries, aimed at ageing power plants and pipelines, material degradation, fatigue and radiation damage, etc. At present there are no suitable electromagnetic NDE methods for the measurement and characterization of material degradation, in irradiated samples in particular, which is very important and timely for the nuclear power industry in the UK. This paper reports recent developments in the field of electromagnetic (EM) NDE at Newcastle University, including pulsed eddy current (PEC), pulsed magnetic flux leakage (PMFL), magnetic Barkhausen emission (MBE) and magneto-acoustic emission (MAE). As different EM methods have different strengths, an integrative EM framework is introduced. Case studies through the second round robin tests organized by the Universal Network for Magnetic Non-Destructive Evaluation (UNMNDE), representing eighteen leading research groups worldwide in the area of electromagnetic NDE, are reported. Twelve samples with different ageing times and rolling reduction ratios were tested using different magnetic methods among the UNMNDE members. Based on the studies, the complementary characteristics of electromagnetic techniques for NDE are discussed.

  8. Double-quantum homonuclear rotary resonance: Efficient dipolar recovery in magic-angle spinning nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Nielsen, N. C.; Bildsøe, H.; Jakobsen, H. J.; Levitt, M. H.

    1994-08-01

    We describe an efficient method for the recovery of homonuclear dipole-dipole interactions in magic-angle spinning NMR. Double-quantum homonuclear rotary resonance (2Q-HORROR) is established by fulfilling the condition ωr=2ω1, where ωr is the sample rotation frequency and ω1 is the nutation frequency around an applied resonant radio frequency (rf) field. This resonance can be used for double-quantum filtering and measurement of homonuclear dipolar interactions in the presence of magic-angle spinning. The spin dynamics depend only weakly on crystallite orientation allowing good performance for powder samples. Chemical shift effects are suppressed to zeroth order. The method is demonstrated for singly and doubly 13C labeled L-alanine.

  9. High Resolution H-1 NMR Spectroscopy in a Live Mouse subjected to 1.5 Hz Magic Angle Spinning

    SciTech Connect

    Wind, Robert A.; Hu, Jian Zhi; Rommereim, Donald N.

    2003-12-03

    It is demonstrated that the resolution of the 1H NMR metabolite spectrum in a live mouse can be significantly enhanced by an ultra-slow magic angle spinning of the animal combined with a modified phase-corrected magic angle turning (PHORMAT) pulse sequence. Proton NMR spectra were measured of the torso and the top part of the belly of a female BALBc mouse in about one hour in a 2T field, while spinning the animal at a speed of 1.5 Hz. It was found that even in this relatively low field with PHORMAT an isotropic spectrum is obtained with line widths that are a factor 4.6 smaller than those obtained in a stationary mouse. It is concluded that in vivo PHORMAT has the potential to significantly increase the utility of 1H NMR spectroscopy for biochemical and biomedical animal research.

  10. Development of a magic-angle spinning nuclear magnetic resonance probe with a cryogenic detection system for sensitivity enhancement.

    PubMed

    Mizuno, Takashi; Hioka, Katsuya; Fujioka, Koji; Takegoshi, K

    2008-04-01

    A novel nuclear magnetic resonance (NMR) probe for high-resolution solid-state NMR has been developed. In this probe, temperature of the detection coil is kept at cryogenic temperature (approximately 12 K) for sensitivity enhancement, which is achieved not only by suppression of thermal noise but also by increment of a Q factor of the coil. A marked feature of this probe is that a sample rotating at magic angle is thermally isolated from the cryogenic system in order to realize high-resolution solid-state NMR measurement at various sample temperatures. We call this system as cryocoil magic-angle spinning (cryocoil MAS). (1)H MAS NMR with the coil temperature of approximately 20 K was successfully observed for solid adamantane rotating at room temperature, and signal-to-noise increment due to this cryocoil approach was confirmed.

  11. Sensitivity enhancement by multiple-contact cross-polarization under magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Raya, J.; Hirschinger, J.

    2017-08-01

    Multiple-contact cross-polarization (MC-CP) is applied to powder samples of ferrocene and L-alanine under magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. The combination of a two-step memory function approach and the Anderson-Weiss approximation is found to be particularly useful to derive approximate analytical solutions for single-contact Hartmann-Hahn CP (HHCP) and MC-CP dynamics under MAS. We show that the MC-CP sequence requiring no pulse-shape optimization yields higher polarizations at short contact times than optimized adiabatic passage through the HH condition CP (APHH-CP) when the MAS frequency is comparable to the heteronuclear dipolar coupling, i.e., when APHH-CP through a single sideband matching condition is impossible or difficult to perform. It is also shown that the MC-CP sideband HH conditions are generally much broader than for single-contact HHCP and that efficient polarization transfer at the centerband HH condition can be reintroduced by rotor-asynchronous multiple equilibrations-re-equilibrations with the proton spin bath. Boundary conditions for the successful use of the MC-CP experiment when relying on spin-lattice relaxation for repolarization are also examined.

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

    PubMed

    Shmyreva, Anna A; Safdari, Majid; Furó, István; Dvinskikh, Sergey V

    2016-06-14

    Orders of magnitude decrease of (207)Pb and (199)Hg NMR longitudinal relaxation times T1 upon magic-angle-spinning (MAS) are observed and systematically investigated in solid lead and mercury halides MeX2 (Me = Pb, Hg and X = Cl, Br, I). In lead(ii) halides, the most dramatic decrease of T1 relative to that in a static sample is in PbI2, while it is smaller but still significant in PbBr2, and not detectable in PbCl2. 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.

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

    NASA Astrophysics Data System (ADS)

    Shmyreva, Anna A.; Safdari, Majid; Furó, István; Dvinskikh, Sergey V.

    2016-06-01

    Orders of magnitude decrease of 207Pb and 199Hg NMR longitudinal relaxation times T1 upon magic-angle-spinning (MAS) are observed and systematically investigated in solid lead and mercury halides MeX2 (Me = Pb, Hg and X = Cl, Br, I). In lead(ii) halides, the most dramatic decrease of T1 relative to that in a static sample is in PbI2, while it is smaller but still significant in PbBr2, and not detectable in PbCl2. 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. Magic-angle spinning solid-state multinuclear NMR on low-field instrumentation.

    PubMed

    Sørensen, Morten K; Bakharev, Oleg; Jensen, Ole; Jakobsen, Hans J; Skibsted, Jørgen; Nielsen, Niels Chr

    2014-01-01

    Mobile and cost-effective NMR spectroscopy exploiting low-field permanent magnets is a field of tremendous development with obvious applications for arrayed large scale analysis, field work, and industrial screening. So far such demonstrations have concentrated on relaxation measurements and lately high-resolution liquid-state NMR applications. With high-resolution solid-state NMR spectroscopy being increasingly important in a broad variety of applications, we here introduce low-field magic-angle spinning (MAS) solid-state multinuclear NMR based on a commercial ACT 0.45 T 62 mm bore Halbach magnet along with a homebuilt FPGA digital NMR console, amplifiers, and a modified standard 45 mm wide MAS probe for 7 mm rotors. To illustrate the performance of the instrument and address cases where the low magnetic field may offer complementarity to high-field NMR experiments, we demonstrate applications for (23)Na MAS NMR with enhanced second-order quadrupolar coupling effects and (31)P MAS NMR where reduced influence from chemical shift anisotropy at low field may facilitate determination of heteronuclear dipole-dipole couplings. Copyright © 2013 Elsevier Inc. All rights reserved.

  15. Magic-angle spinning solid-state multinuclear NMR on low-field instrumentation

    NASA Astrophysics Data System (ADS)

    Sørensen, Morten K.; Bakharev, Oleg; Jensen, Ole; Jakobsen, Hans J.; Skibsted, Jørgen; Nielsen, Niels Chr.

    2014-01-01

    Mobile and cost-effective NMR spectroscopy exploiting low-field permanent magnets is a field of tremendous development with obvious applications for arrayed large scale analysis, field work, and industrial screening. So far such demonstrations have concentrated on relaxation measurements and lately high-resolution liquid-state NMR applications. With high-resolution solid-state NMR spectroscopy being increasingly important in a broad variety of applications, we here introduce low-field magic-angle spinning (MAS) solid-state multinuclear NMR based on a commercial ACT 0.45 T 62 mm bore Halbach magnet along with a homebuilt FPGA digital NMR console, amplifiers, and a modified standard 45 mm wide MAS probe for 7 mm rotors. To illustrate the performance of the instrument and address cases where the low magnetic field may offer complementarity to high-field NMR experiments, we demonstrate applications for 23Na MAS NMR with enhanced second-order quadrupolar coupling effects and 31P MAS NMR where reduced influence from chemical shift anisotropy at low field may facilitate determination of heteronuclear dipole-dipole couplings.

  16. Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization

    PubMed Central

    Barnes, Alexander B.; Mak-Jurkauskas, Melody L.; Matsuki, Yoh; Bajaj, Vikram S.; van der Wel, Patrick C. A.; DeRocher, Ronald; Bryant, Jeffrey; Sirigiri, Jagadishwar R.; Temkin, Richard J.; Lugtenburg, Johan; Herzfeld, Judith; Griffin, Robert G.

    2009-01-01

    We describe a cryogenic sample exchange system that dramatically improves the efficiency of magic angle spinning (MAS) dynamic nuclear polarization (DNP) experiments by reducing the time required to change samples and by improving long-term instrument stability. Changing samples in conventional cryogenic MAS DNP/NMR experiments involves warming the probe to room temperature, detaching all cryogenic, RF, and microwave connections, removing the probe from the magnet, replacing the sample, and reversing all the previous steps, with the entire cycle requiring a few hours. The sample exchange system described here — which relies on an eject pipe attached to the front of the MAS stator and a vacuum jacketed dewar with a bellowed hole — circumvents these procedures. To demonstrate the excellent sensitivity, resolution, and stability achieved with this quadruple resonance sample exchange probe, we have performed high precision distance measurements on the active site of the membrane protein bacteriorhodopsin. We also include a spectrum of the tripeptide N-f-MLF-OH at 100 K which shows 30 Hz linewidths. PMID:19356957

  17. A unified heteronuclear decoupling strategy for magic-angle-spinning solid-state NMR spectroscopy

    SciTech Connect

    Equbal, Asif; Bjerring, Morten; Nielsen, Niels Chr. E-mail: ncn@inano.au.dk; Madhu, P. K. E-mail: ncn@inano.au.dk

    2015-05-14

    A unified strategy of two-pulse based heteronuclear decoupling for solid-state magic-angle spinning nuclear magnetic resonance is presented. The analysis presented here shows that different decoupling sequences like two-pulse phase-modulation (TPPM), X-inverse-X (XiX), and finite pulse refocused continuous wave (rCW{sup A}) are basically specific solutions of a more generalized decoupling scheme which incorporates the concept of time-modulation along with phase-modulation. A plethora of other good decoupling conditions apart from the standard, TPPM, XiX, and rCW{sup A} decoupling conditions are available from the unified decoupling approach. The importance of combined time- and phase-modulation in order to achieve the best decoupling conditions is delineated. The consequences of different indirect dipolar interactions arising from cross terms comprising of heteronuclear and homonuclear dipolar coupling terms and also those between heteronuclear dipolar coupling and chemical-shift anisotropy terms are presented in order to unfold the effects of anisotropic interactions under different decoupling conditions. Extensive numerical simulation results are corroborated with experiments on standard amino acids.

  18. Spin dynamics of polarization inversion spin exchange at the magic angle in multiple spin systems.

    PubMed

    Gan, Z

    2000-03-01

    Polarization inversion spin exchange at the magic angle (PISEMA) [J. Magn. Reson. A 109, 270 (1994)] is an important experiment in NMR structural characterization of membrane proteins in oriented lipid bilayers. This paper presents a theoretical and experimental study of the spin dynamics in PISEMA to investigate the line-narrowing mechanism. The study focuses on the effect of neighboring protons on the spin exchange of a strongly coupled spin pair. The spin exchange is solved analytically for simple spin systems and is numerically simulated for many-spin systems. The results show that the dipolar couplings from the neighboring protons of a strongly coupled spin pair perturb the spin exchange only in the second order, therefore it has little contribution to the linewidth of PISEMA spectra in comparison to the separated-local-field spectra. The effects from proton resonance offset and the mismatch of the Hartmann-Hahn condition are also discussed along with experimental results using model single-crystal samples.

  19. Cryogenic sample exchange NMR probe for magic angle spinning dynamic nuclear polarization.

    PubMed

    Barnes, Alexander B; Mak-Jurkauskas, Melody L; Matsuki, Yoh; Bajaj, Vikram S; van der Wel, Patrick C A; Derocher, Ronald; Bryant, Jeffrey; Sirigiri, Jagadishwar R; Temkin, Richard J; Lugtenburg, Johan; Herzfeld, Judith; Griffin, Robert G

    2009-06-01

    We describe a cryogenic sample exchange system that dramatically improves the efficiency of magic angle spinning (MAS) dynamic nuclear polarization (DNP) experiments by reducing the time required to change samples and by improving long-term instrument stability. Changing samples in conventional cryogenic MAS DNP/NMR experiments involves warming the probe to room temperature, detaching all cryogenic, RF, and microwave connections, removing the probe from the magnet, replacing the sample, and reversing all the previous steps, with the entire cycle requiring a few hours. The sample exchange system described here-which relies on an eject pipe attached to the front of the MAS stator and a vacuum jacketed dewar with a bellowed hole-circumvents these procedures. To demonstrate the excellent sensitivity, resolution, and stability achieved with this quadruple resonance sample exchange probe, we have performed high precision distance measurements on the active site of the membrane protein bacteriorhodopsin. We also include a spectrum of the tripeptide N-f-MLF-OH at 100K which shows 30 Hz linewidths.

  20. Dynamic nuclear polarization at 40 kHz magic angle spinning.

    PubMed

    Chaudhari, Sachin R; Berruyer, Pierrick; Gajan, David; Reiter, Christian; Engelke, Frank; Silverio, Daniel L; Copéret, Christophe; Lelli, Moreno; Lesage, Anne; Emsley, Lyndon

    2016-04-21

    DNP-enhanced solid-state NMR spectroscopy under magic angle spinning (MAS) is rapidly developing into a powerful analytical tool to investigate the structure of a wide range of solid materials, because it provides unsurpassed sensitivity gains. Most developments and applications of DNP MAS NMR were so far reported at moderate spinning frequencies (up to 14 kHz using 3.2 mm rotors). Here, using a 1.3 mm MAS DNP probe operating at 18.8 T and ∼100 K, we show that signal amplification factors can be increased by up to a factor two when using smaller volume rotors as compared to 3.2 mm rotors, and report enhancements of around 60 over a range of sample spinning rates from 10 to 40 kHz. Spinning at 40 kHz is also shown to increase (29)Si coherence lifetimes by a factor three as compared to 10 kHz, substantially increasing sensitivity in CPMG type experiments. The contribution of quenching effects to the overall sensitivity gain at very fast MAS is evaluated, and applications are reported on a functionalised mesostructured organic-inorganic material.

  1. Sensitivity enhancement by multiple-contact cross-polarization under magic-angle spinning.

    PubMed

    Raya, J; Hirschinger, J

    2017-08-01

    Multiple-contact cross-polarization (MC-CP) is applied to powder samples of ferrocene and l-alanine under magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. The combination of a two-step memory function approach and the Anderson-Weiss approximation is found to be particularly useful to derive approximate analytical solutions for single-contact Hartmann-Hahn CP (HHCP) and MC-CP dynamics under MAS. We show that the MC-CP sequence requiring no pulse-shape optimization yields higher polarizations at short contact times than optimized adiabatic passage through the HH condition CP (APHH-CP) when the MAS frequency is comparable to the heteronuclear dipolar coupling, i.e., when APHH-CP through a single sideband matching condition is impossible or difficult to perform. It is also shown that the MC-CP sideband HH conditions are generally much broader than for single-contact HHCP and that efficient polarization transfer at the centerband HH condition can be reintroduced by rotor-asynchronous multiple equilibrations-re-equilibrations with the proton spin bath. Boundary conditions for the successful use of the MC-CP experiment when relying on spin-lattice relaxation for repolarization are also examined. Copyright © 2017 Elsevier Inc. All rights reserved.

  2. Selectively Dispersed Isotope Labeling for Protein Structure Determination by Magic Angle Spinning NMR

    PubMed Central

    Eddy, Matthew T.; Belenky, Marina; Sivertsen, Astrid; Griffin, Robert G.; Herzfeld, Judith

    2013-01-01

    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, [1-13C] acetate does not label α 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 [2-13C] 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. PMID:23990199

  3. Structure of fully protonated proteins by proton-detected magic-angle spinning NMR.

    PubMed

    Andreas, Loren B; Jaudzems, Kristaps; Stanek, Jan; Lalli, Daniela; Bertarello, Andrea; Le Marchand, Tanguy; Cala-De Paepe, Diane; Kotelovica, Svetlana; Akopjana, Inara; Knott, Benno; Wegner, Sebastian; Engelke, Frank; Lesage, Anne; Emsley, Lyndon; Tars, Kaspars; Herrmann, Torsten; Pintacuda, Guido

    2016-08-16

    Protein structure determination by proton-detected magic-angle spinning (MAS) NMR has focused on highly deuterated samples, in which only a small number of protons are introduced and observation of signals from side chains is extremely limited. Here, we show in two fully protonated proteins that, at 100-kHz MAS and above, spectral resolution is high enough to detect resolved correlations from amide and side-chain protons of all residue types, and to reliably measure a dense network of (1)H-(1)H proximities that define a protein structure. The high data quality allowed the correct identification of internuclear distance restraints encoded in 3D spectra with automated data analysis, resulting in accurate, unbiased, and fast structure determination. Additionally, we find that narrower proton resonance lines, longer coherence lifetimes, and improved magnetization transfer offset the reduced sample size at 100-kHz spinning and above. Less than 2 weeks of experiment time and a single 0.5-mg sample was sufficient for the acquisition of all data necessary for backbone and side-chain resonance assignment and unsupervised structure determination. We expect the technique to pave the way for atomic-resolution structure analysis applicable to a wide range of proteins.

  4. Proton-Detected Solid-State NMR Spectroscopy of Bone with Ultrafast Magic Angle Spinning

    NASA Astrophysics Data System (ADS)

    Mroue, Kamal H.; Nishiyama, Yusuke; Kumar Pandey, Manoj; Gong, Bo; McNerny, Erin; Kohn, David H.; Morris, Michael D.; Ramamoorthy, Ayyalusamy

    2015-07-01

    While obtaining high-resolution structural details from bone is highly important to better understand its mechanical strength and the effects of aging and disease on bone ultrastructure, it has been a major challenge to do so with existing biophysical techniques. Though solid-state NMR spectroscopy has the potential to reveal the structural details of bone, it suffers from poor spectral resolution and sensitivity. Nonetheless, recent developments in magic angle spinning (MAS) NMR technology have made it possible to spin solid samples up to 110 kHz frequency. With such remarkable capabilities, 1H-detected NMR experiments that have traditionally been challenging on rigid solids can now be implemented. Here, we report the first application of multidimensional 1H-detected NMR measurements on bone under ultrafast MAS conditions to provide atomistic-level elucidation of the complex heterogeneous structure of bone. Our investigations demonstrate that two-dimensional 1H/1H chemical shift correlation spectra for bone are obtainable using fp-RFDR (finite-pulse radio-frequency-driven dipolar recoupling) pulse sequence under ultrafast MAS. Our results infer that water exhibits distinct 1H-1H dipolar coupling networks with the backbone and side-chain regions in collagen. These results show the promising potential of proton-detected ultrafast MAS NMR for monitoring structural and dynamic changes caused by mechanical loading and disease in bone.

  5. A permanent MRI magnet for magic angle imaging having its field parallel to the poles

    NASA Astrophysics Data System (ADS)

    McGinley, John V. M.; Ristic, Mihailo; Young, Ian R.

    2016-10-01

    A novel design of open permanent magnet is presented, in which the magnetic field is oriented parallel to the planes of its poles. The paper describes the methods whereby such a magnet can be designed with a field homogeneity suitable for Magnetic Resonance Imaging (MRI). Its primary purpose is to take advantage of the Magic Angle effect in MRI of human extremities, particularly the knee joint, by being capable of rotating the direction of the main magnetic field B0 about two orthogonal axes around a stationary subject and achieve all possible angulations. The magnet comprises a parallel pair of identical profiled arrays of permanent magnets backed by a flat steel yoke such that access in lateral directions is practical. The paper describes the detailed optimization procedure from a target 150 mm DSV to the achievement of a measured uniform field over a 130 mm DSV. Actual performance data of the manufactured magnet, including shimming and a sample image, is presented. The overall magnet system mounting mechanism is presented, including two orthogonal axes of rotation of the magnet about its isocentre.

  6. A permanent MRI magnet for magic angle imaging having its field parallel to the poles.

    PubMed

    McGinley, John V M; Ristic, Mihailo; Young, Ian R

    2016-10-01

    A novel design of open permanent magnet is presented, in which the magnetic field is oriented parallel to the planes of its poles. The paper describes the methods whereby such a magnet can be designed with a field homogeneity suitable for Magnetic Resonance Imaging (MRI). Its primary purpose is to take advantage of the Magic Angle effect in MRI of human extremities, particularly the knee joint, by being capable of rotating the direction of the main magnetic field B0 about two orthogonal axes around a stationary subject and achieve all possible angulations. The magnet comprises a parallel pair of identical profiled arrays of permanent magnets backed by a flat steel yoke such that access in lateral directions is practical. The paper describes the detailed optimization procedure from a target 150mm DSV to the achievement of a measured uniform field over a 130mm DSV. Actual performance data of the manufactured magnet, including shimming and a sample image, is presented. The overall magnet system mounting mechanism is presented, including two orthogonal axes of rotation of the magnet about its isocentre.

  7. Characterization of brain metastases using high-resolution magic angle spinning MRS.

    PubMed

    Sjøbakk, Torill E; Johansen, Roar; Bathen, Tone F; Sonnewald, Ursula; Juul, Roar; Torp, Sverre H; Lundgren, Steinar; Gribbestad, Ingrid S

    2008-02-01

    The objectives of this study were to (a) explore the spectral characteristics of brain metastases, focusing on the origin of the primary cancer, and (b) evaluate the correlation with clinical outcome using multivariate analysis. High-resolution magic angle spinning (HR-MAS) MR spectra (n = 26) were obtained from 16 patients with brain metastases using a Bruker Avance DRX600 instrument. Standard pulse-acquired and spin-echo (TE 32 and 285 ms) (1)H spectra were obtained. These were examined using principal component analysis (PCA) and partial least squares regression analysis (PLS) relating spectral data to clinical outcome. The PCA score plot of pulse-acquired HR-MAS spectra showed a trend of clustering due to the origin of the metastases, mainly based on differences in the lipid signals at 1.3 and 0.9 ppm. With PLS, spectra of patients who died less than 5 months after surgery appeared to cluster in the lower left quadrant of the score plot. These preliminary results on brain metastasis classification and prediction of survival must be validated in a larger patient cohort. However, the possibility of differentiating metastases according to origin and predicting survival on the basis of HR-MAS spectra suggests that this method may be useful for diagnosing and planning treatment for brain metastases and also for guiding decisions about terminating further treatment.

  8. Spectral editing: selection of methyl groups in multidimensional solid-state magic-angle spinning NMR.

    PubMed

    Jehle, Stefan; Hiller, Matthias; Rehbein, Kristina; Diehl, Anne; Oschkinat, Hartmut; van Rossum, Barth-Jan

    2006-11-01

    A simple spectroscopic filtering technique is presented that may aid the assignment of (13)C and (15)N resonances of methyl-containing amino-acids in solid-state magic-angle spinning (MAS) NMR. A filtering block that selects methyl resonances is introduced in two-dimensional (2D) (13)C-homonuclear and (15)N-(13)C heteronuclear correlation experiments. The 2D (13)C-(13)C correlation spectra are recorded with the methyl filter implemented prior to a (13)C-(13)C mixing step. It is shown that these methyl-filtered (13)C-homonuclear correlation spectra are instrumental in the assignment of C(delta) resonances of leucines by suppression of C(gamma)-C(delta) cross peaks. Further, a methyl filter is implemented prior to a (15)N-(13)C transferred-echo double resonance (TEDOR) exchange scheme to obtain 2D (15)N-(13)C heteronuclear correlation spectra. These experiments provide correlations between methyl groups and backbone amides. Some of the observed sequential (15)N-(13)C correlations form the basis for initial sequence-specific assignments of backbone signals of the outer-membrane protein G.

  9. Magic angle sample spinning sup 13 C nuclear magnetic resonance of isotopically labeled bacteriorhodopsin

    SciTech Connect

    Engelhard, M.; Hess, B.; Emeis, D.; Metz, G.; Kreutz, W.; Siebert, F. )

    1989-05-02

    Bacteriorhodopsin (bR), the light-driven proton pump protein from Halobacterium halobium, was biosynthetically labeled with (4-{sup 13}C)Asp. The incorporation yield was 48%. The magic angle sample spinning (MASS) {sup 13}C nuclear magnetic resonance (NMR) spectrum of this sample revealed six different peaks superimposed on a broad band of naturally abundant peptide-bond {sup 13}C. Two of the six carbonyl signals can be attributed to internal-protonated Asp carboxyl groups, one of which might be Asp115. An additional resonance at 110 ppm can be associated with the C-11 carbon of Trp, indicating an unusual biosynthetic pathway of this amino acid in Halobacterium halobium. Similar measurements performed on papain-treated purple membrane which lacks the C-terminal tail display two new intense signals at 178 and 178.9 ppm. If the same spectrum is taken without cross-polarization, these signals do not decrease or disappear. On the basis of their intensities and their chemical shifts, one can assign in addition to the C-terminal Asp four Asp residues facing the cytoplasmic phase. In native bR, at least two of these form a salt-bridge-like bond which also might include the C-terminal tail. These experiments not only provide data about the chemical environment of the Asp residues within the hydrophobic core of bacteriorhodopsin but also yield information about the interactions between surface components.

  10. Solid-state NMR spectra of lipid-anchored proteins under magic angle spinning.

    PubMed

    Nomura, Kaoru; Harada, Erisa; Sugase, Kenji; Shimamoto, Keiko

    2014-03-06

    Solid-state NMR is a promising tool for elucidating membrane-related biological phenomena. We achieved the measurement of high-resolution solid-state NMR spectra for a lipid-anchored protein embedded in lipid bilayers under magic angle spinning (MAS). To date, solid-state NMR measurements of lipid-anchored proteins have not been accomplished due to the difficulty in supplying sufficient amount of stable isotope labeled samples in the overexpression of lipid-anchored proteins requiring complex posttranslational modification. We designed a pseudo lipid-anchored protein in which the protein component was expressed in E. coli and attached to a chemically synthesized lipid-anchor mimic. Using two types of membranes, liposomes and bicelles, we demonstrated different types of insertion procedures for lipid-anchored protein into membranes. In the liposome sample, we were able to observe the cross-polarization and the (13)C-(13)C chemical shift correlation spectra under MAS, indicating that the liposome sample can be used to analyze molecular interactions using dipolar-based NMR experiments. In contrast, the bicelle sample showed sufficient quality of spectra through scalar-based experiments. The relaxation times and protein-membrane interaction were capable of being analyzed in the bicelle sample. These results demonstrated the applicability of two types of sample system to elucidate the roles of lipid-anchors in regulating diverse biological phenomena.

  11. Second-order dipolar order in magic-angle spinning nuclear magnetic resonance.

    PubMed

    van Beek, Jacco D; Hemmi, Adrian; Ernst, Matthias; Meier, Beat H

    2011-10-21

    Generating dipolar order under magic-angle spinning (MAS) conditions is explored for different pulse sequences and dipolar-coupling networks. It is shown that under MAS second-order dipolar order can be generated reliably with 10% to 30% efficiency using the Jeener-Broekaert sequence in systems where the second-order average Hamiltonian is a (near) constant of the motion. When using adiabatic demagnetization and remagnetization, second-order dipolar order can be generated and reverted back to Zeeman order with up to 60% efficiency. This requires a maximum field strength with a nutation frequency that is less than one-quarter of the rotor frequency, and that the spin system can be properly spinlocked under such conditions. A simple coherent description accounts for the principal features of the spin dynamics, even using the smallest possible system of three coupled spins. For the systems investigated, the lifetime of second-order dipolar order under MAS was found to be on the order of T(1). © 2011 American Institute of Physics

  12. Paramagnetic Properties of a Crystalline Iron-Sulfur Protein by Magic-Angle Spinning NMR Spectroscopy.

    PubMed

    Bertarello, Andrea; Schubeis, Tobias; Fuccio, Carmelo; Ravera, Enrico; Fragai, Marco; Parigi, Giacomo; Emsley, Lyndon; Pintacuda, Guido; Luchinat, Claudio

    2017-06-05

    We present the first solid-state NMR study of an iron-sulfur protein. The combined use of very fast (60 kHz) magic-angle spinning and tailored radiofrequency irradiation schemes allows the detection and the assignment of most of the (1)H and (13)C resonances of the oxidized high-potential iron-sulfur protein I from Ectothiorhodospira halophila (EhHiPIP I), including those in residues coordinating the Fe4S4 cluster. For these residues, contact shifts as large as 100 and 400 ppm for (1)H and (13)C resonances, respectively, were observed, which represent the most shifted solid-state NMR signals ever measured in metalloproteins. Interestingly, by targeting EhHiPIP I in a crystalline environment, we were able to capture distinct paramagnetic signatures from the two conformations present in the asymmetric unit. The magnetic properties of the system were verified by following the temperature dependence of the contact-shifted cysteine resonances.

  13. Magic angle spinning NMR of proteins: high-frequency dynamic nuclear polarization and (1)H detection.

    PubMed

    Su, Yongchao; Andreas, Loren; Griffin, Robert G

    2015-01-01

    Magic angle spinning (MAS) NMR studies of amyloid and membrane proteins and large macromolecular complexes are an important new approach to structural biology. However, the applicability of these experiments, which are based on (13)C- and (15)N-detected spectra, would be enhanced if the sensitivity were improved. Here we discuss two advances that address this problem: high-frequency dynamic nuclear polarization (DNP) and (1)H-detected MAS techniques. DNP is a sensitivity enhancement technique that transfers the high polarization of exogenous unpaired electrons to nuclear spins via microwave irradiation of electron-nuclear transitions. DNP boosts NMR signal intensities by factors of 10(2) to 10(3), thereby overcoming NMR's inherent low sensitivity. Alternatively, it permits structural investigations at the nanomolar scale. In addition, (1)H detection is feasible primarily because of the development of MAS rotors that spin at frequencies of 40 to 60 kHz or higher and the preparation of extensively (2)H-labeled proteins.

  14. Structure of fully protonated proteins by proton-detected magic-angle spinning NMR

    PubMed Central

    Jaudzems, Kristaps; Stanek, Jan; Lalli, Daniela; Bertarello, Andrea; Le Marchand, Tanguy; Cala-De Paepe, Diane; Kotelovica, Svetlana; Akopjana, Inara; Knott, Benno; Wegner, Sebastian; Engelke, Frank; Lesage, Anne; Emsley, Lyndon; Tars, Kaspars; Herrmann, Torsten; Pintacuda, Guido

    2016-01-01

    Protein structure determination by proton-detected magic-angle spinning (MAS) NMR has focused on highly deuterated samples, in which only a small number of protons are introduced and observation of signals from side chains is extremely limited. Here, we show in two fully protonated proteins that, at 100-kHz MAS and above, spectral resolution is high enough to detect resolved correlations from amide and side-chain protons of all residue types, and to reliably measure a dense network of 1H-1H proximities that define a protein structure. The high data quality allowed the correct identification of internuclear distance restraints encoded in 3D spectra with automated data analysis, resulting in accurate, unbiased, and fast structure determination. Additionally, we find that narrower proton resonance lines, longer coherence lifetimes, and improved magnetization transfer offset the reduced sample size at 100-kHz spinning and above. Less than 2 weeks of experiment time and a single 0.5-mg sample was sufficient for the acquisition of all data necessary for backbone and side-chain resonance assignment and unsupervised structure determination. We expect the technique to pave the way for atomic-resolution structure analysis applicable to a wide range of proteins. PMID:27489348

  15. Quantitative neuropathology by high resolution magic angle spinning proton magnetic resonance spectroscopy

    PubMed Central

    Cheng, L. L.; Ma, M. J.; Becerra, L.; Ptak, T.; Tracey, I.; Lackner, A.; González, R. G.

    1997-01-01

    We describe a method that directly relates tissue neuropathological analysis to medical imaging. Presently, only indirect and often tenuous relationships are made between imaging (such as MRI or x-ray computed tomography) and neuropathology. We present a biochemistry-based, quantitative neuropathological method that can help to precisely quantify information provided by in vivo proton magnetic resonance spectroscopy (1HMRS), an emerging medical imaging technique. This method, high resolution magic angle spinning (HRMAS) 1HMRS, is rapid and requires only small amounts of unprocessed samples. Unlike chemical extraction or other forms of tissue processing, this method analyzes tissue directly, thus minimizing artifacts. We demonstrate the utility of this method by assessing neuronal damage using multiple tissue samples from differently affected brain regions in a case of Pick disease, a human neurodegenerative disorder. Among different regions, we found an excellent correlation between neuronal loss shown by traditional neurohistopathology and decrease of the neuronal marker N-acetylaspartate measured by HRMAS 1HMRS. This result demonstrates for the first time, to our knowledge, a direct, quantitative link between a decrease in N-acetylaspartate and neuronal loss in a human neurodegenerative disease. As a quantitative method, HRMAS 1HMRS has potential applications in experimental and clinical neuropathologic investigations. It should also provide a rational basis for the interpretation of in vivo 1HMRS studies of human neurological disorders. PMID:9177231

  16. Ultrashort echo time magnetization transfer (UTE-MT) imaging and modeling: magic angle independent biomarkers of tissue properties.

    PubMed

    Ma, Ya-Jun; Shao, Hongda; Du, Jiang; Chang, Eric Y

    2016-11-01

    MRI biomarkers such as T2 , T2 * and T1rho have been widely used, but are confounded by the magic angle effect. The purpose of this study is to investigate the use of the two-dimensional ultrashort echo time magnetization transfer (UTE-MT) sequence for potential magic angle independent MR biomarkers. Magnetization transfer was investigated in cadaveric Achilles tendon samples using the UTE-MT sequence at five MT powers and five frequency offsets ranging from 2 to 50 kHz. The protocol was applied at five sample orientations ranging from 0 to 90° relative to the B0 field. The results were analyzed with a two-pool quantitative MT model. Multiple TE data were also acquired and mono-exponential T2 * was calculated for each orientation. Macromolecular proton fractions and exchange rates derived from UTE-MT modeling did not appreciably change between the various orientations, whereas the T2 * relaxation time demonstrated up to a sixfold increase from 0° to 55°. The UTE-MT technique with two-pool modeling shows promise as a clinically compatible technique that is resistant to the magic angle effect. This method provides information on the macromolecular proton pool that cannot be directly obtained by other methods, including regular UTE techniques.

  17. High zenith angle observations of PKS 2155-304 with the MAGIC-I telescope

    NASA Astrophysics Data System (ADS)

    Aleksić, J.; Alvarez, E. A.; Antonelli, L. A.; Antoranz, P.; Asensio, M.; Backes, M.; Barres de Almeida, U.; Barrio, J. A.; Bastieri, D.; Becerra González, J.; Bednarek, W.; Berdyugin, A.; Berger, K.; Bernardini, E.; Biland, A.; Blanch, O.; Bock, R. K.; Boller, A.; Bonnoli, G.; Borla Tridon, D.; Braun, I.; Bretz, T.; Cañellas, A.; Carmona, E.; Carosi, A.; Colin, P.; Colombo, E.; Contreras, J. L.; Cortina, J.; Cossio, L.; Covino, S.; Dazzi, F.; De Angelis, A.; De Caneva, G.; De Cea del Pozo, E.; De Lotto, B.; Delgado Mendez, C.; Diago Ortega, A.; Doert, M.; Domínguez, A.; Dominis Prester, D.; Dorner, D.; Doro, M.; Eisenacher, D.; Elsaesser, D.; Ferenc, D.; Fonseca, M. V.; Font, L.; Fruck, C.; García López, R. J.; Garczarczyk, M.; Garrido, D.; Giavitto, G.; Godinović, N.; Gozzini, S. R.; Hadasch, D.; Häfner, D.; Herrero, A.; Hildebrand, D.; Höhne-Mönch, D.; Hose, J.; Hrupec, D.; Jogler, T.; Kellermann, H.; Klepser, S.; Krähenbühl, T.; Krause, J.; Kushida, J.; La Barbera, A.; Lelas, D.; Leonardo, E.; Lewandowska, N.; Lindfors, E.; Lombardi, S.; López, M.; López, R.; López-Oramas, A.; Lorenz, E.; Makariev, M.; Maneva, G.; Mankuzhiyil, N.; Mannheim, K.; Maraschi, L.; Marcote, B.; Mariotti, M.; Martínez, M.; Mazin, D.; Meucci, M.; Miranda, J. M.; Mirzoyan, R.; Moldón, J.; Moralejo, A.; Munar-Adrover, P.; Niedzwiecki, A.; Nieto, D.; Nilsson, K.; Nowak, N.; Orito, R.; Paiano, S.; Paneque, D.; Paoletti, R.; Pardo, S.; Paredes, J. M.; Partini, S.; Perez-Torres, M. A.; Persic, M.; Peruzzo, L.; Pilia, M.; Pochon, J.; Prada, F.; Prada Moroni, P. G.; Prandini, E.; Puerto Gimenez, I.; Puljak, I.; Reichardt, I.; Reinthal, R.; Rhode, W.; Ribó, M.; Rico, J.; Rügamer, S.; Saggion, A.; Saito, K.; Saito, T. Y.; Salvati, M.; Satalecka, K.; Scalzotto, V.; Scapin, V.; Schultz, C.; Schweizer, T.; Shayduk, M.; Shore, S. N.; Sillanpää, A.; Sitarek, J.; Snidaric, I.; Sobczynska, D.; Spanier, F.; Spiro, S.; Stamatescu, V.; Stamerra, A.; Steinke, B.; Storz, J.; Strah, N.; Sun, S.; Surić, T.; Takalo, L.; Takami, H.; Tavecchio, F.; Temnikov, P.; Terzić, T.; Tescaro, D.; Teshima, M.; Tibolla, O.; Torres, D. F.; Treves, A.; Uellenbeck, M.; Vankov, H.; Vogler, P.; Wagner, R. M.; Weitzel, Q.; Zabalza, V.; Zandanel, F.; Zanin, R.

    2012-08-01

    Context. The high frequency peaked BL Lac PKS 2155-304 with a redshift of z = 0.116 was discovered in 1997 in the very high energy (VHE, E > 100 GeV) γ-ray range by the University of Durham Mark VI γ-ray Cherenkov telescope in Australia with a flux corresponding to 20% of the Crab Nebula flux. It was later observed and detected with high significance by the southern Cherenkov observatory H.E.S.S. establishing this source as the best studied southern TeV blazar. Detection from the northern hemisphere is difficult due to challenging observation conditions under large zenith angles. In July 2006, the H.E.S.S. collaboration reported an extraordinary outburst of VHE γ-emission. During the outburst, the VHE γ-ray emission was found to be variable on the time scales of minutes and with a mean flux of ~7 times the flux observed from the Crab Nebula. Follow-up observations with the MAGIC-I standalone Cherenkov telescope were triggered by this extraordinary outburst and PKS 2155-304 was observed between 28 July to 2 August 2006 for 15 h at large zenith angles. Aims: We studied the behavior of the source after its extraordinary flare. Furthermore, we developed an analysis method in order to analyze these data taken under large zenith angles. Methods: Here we present an enhanced analysis method for data taken at high zenith angles. We developed improved methods for event selection that led to a better background suppression. Results: The quality of the results presented here is superior to the results presented previously for this data set: detection of the source on a higher significance level and a lower analysis threshold. The averaged energy spectrum we derived has a spectral index of (-3.5 ± 0.2) above 400 GeV, which is in good agreement with the spectral shape measured by H.E.S.S. during the major flare on MJD 53 944. Furthermore, we present the spectral energy distribution modeling of PKS 2155-304. With our observations we increased the duty cycle of the source

  18. Non-destructive testing method and apparatus

    DOEpatents

    Akers, Douglas W [Idaho Falls, ID

    2011-10-04

    Non-destructive testing apparatus may comprise a photon source and a source material that emits positrons in response to bombardment of the source material with photons. The source material is positionable adjacent the photon source and a specimen so that when the source material is positioned adjacent the photon source it is exposed to photons produced thereby. When the source material is positioned adjacent the specimen, the specimen is exposed to at least some of the positrons emitted by the source material. A detector system positioned adjacent the specimen detects annihilation gamma rays emitted by the specimen. Another embodiment comprises a neutron source and a source material that emits positrons in response to neutron bombardment.

  19. NON-DESTRUCTIVE FLAW DETECTION APPARATUS

    DOEpatents

    Stateman, M.J.; Holloway, H.R.

    1957-12-17

    An apparatus is described for the non-destructive detection of flaws in electrical conducting articles. The particular feature of the detection apparatus is that a flaw in the front or back of the test article will not be masked by signals caused by the passage of the end and front of the article through the detection apparatus. The present invention alleviates the above problem by mounting detection coils on directly opposite sides of the test passageway so that the axes of the pickup coils are perpendicular to the axis of an energizing coil through which the article is passed. A flaw in the article will cause a change in the voltage induced in one pickup coil, but passage of the end or front of the article will not produce unequal signals. The signals are compared in appropriate electrical circuitry to actuate a recorder only when unequal signals are present, indicating the presence of a flaw.

  20. Non-destructive evaluation of composites

    NASA Technical Reports Server (NTRS)

    Chu, Tsuchin Philip

    1996-01-01

    The composite materials have been used in aerospace industries for quite some time. Several non-destructive evaluation (NDE) methods have been developed to inspect composites in order to detect flaws, matrix cracking, and delamination. These methods include ultrasonics, acoustic emission, shearography, thermography, X-ray, and digital image correlation. The NDE Branch of Marshall Space Flight Center has recently acquired a thermal imaging NDE system. The same system has been used at NASA Langley Research Center for detecting disbonds. In order to compare different NDE methods, three carbon/carbon composite panels were used for experiment using ultrasonic C-scan, shearography, and thermography methods. These panels have teflon inserts to simulate the delamination between plies in a composite panel. All three methods have successfully located the insert. The experiment and results are presented in the following sections.

  1. Microwave field distribution in a magic angle spinning dynamic nuclear polarization NMR probe

    NASA Astrophysics Data System (ADS)

    Nanni, Emilio A.; Barnes, Alexander B.; Matsuki, Yoh; Woskov, Paul P.; Corzilius, Björn; Griffin, Robert G.; Temkin, Richard J.

    2011-05-01

    We present a calculation of the microwave field distribution in a magic angle spinning (MAS) probe utilized in dynamic nuclear polarization (DNP) experiments. The microwave magnetic field (B 1 S) profile was obtained from simulations performed with the High Frequency Structure Simulator (HFSS) software suite, using a model that includes the launching antenna, the outer Kel-F stator housing coated with Ag, the RF coil, and the 4 mm diameter sapphire rotor containing the sample. The predicted average B 1 S field is 13 μT/W 1/2, where S denotes the electron spin. For a routinely achievable input power of 5 W the corresponding value is γSB 1 S = 0.84 MHz. The calculations provide insights into the coupling of the microwave power to the sample, including reflections from the RF coil and diffraction of the power transmitted through the coil. The variation of enhancement with rotor wall thickness was also successfully simulated. A second, simplified calculation was performed using a single pass model based on Gaussian beam propagation and Fresnel diffraction. This model provided additional physical insight and was in good agreement with the full HFSS simulation. These calculations indicate approaches to increasing the coupling of the microwave power to the sample, including the use of a converging lens and fine adjustment of the spacing of the windings of the RF coil. The present results should prove useful in optimizing the coupling of microwave power to the sample in future DNP experiments. Finally, the results of the simulation were used to predict the cross effect DNP enhancement ( ɛ) vs. ω1 S/(2 π) for a sample of 13C-urea dissolved in a 60:40 glycerol/water mixture containing the polarizing agent TOTAPOL; very good agreement was obtained between theory and experiment.

  2. High resolution magic angle spinning 1H NMR of childhood brain and nervous system tumours.

    PubMed

    Wilson, Martin; Davies, Nigel P; Brundler, Marie-Anne; McConville, Carmel; Grundy, Richard G; Peet, Andrew C

    2009-02-10

    Brain and nervous system tumours are the most common solid cancers in children. Molecular characterisation of these tumours is important for providing novel biomarkers of disease and identifying molecular pathways which may provide putative targets for new therapies. 1H magic angle spinning NMR spectroscopy (1H HR-MAS) is a powerful tool for determining metabolite profiles from small pieces of intact tissue and could potentially provide important molecular information. Forty tissue samples from 29 children with glial and primitive neuro-ectodermal tumours were analysed using HR-MAS (600 MHz Varian gHX nanoprobe). Tumour spectra were fitted to a library of individual metabolite spectra to provide metabolite values. These values were then used in a two tailed t-test and multi-variate analysis employing a principal component analysis and a linear discriminant analysis. Classification accuracy was estimated using a leave-one-out analysis and B632+ bootstrapping. Glial tumours had significantly (two tailed t-test p < 0.05) higher creatine and glutamine and lower taurine, phosphoethanolamine, phosphorylcholine and choline compared with primitive neuro-ectodermal tumours. Classification accuracy was 90%. Medulloblastomas (n = 9) had significantly (two tailed t-test p < 0.05) higher creatine, glutamine, phosphorylcholine, glycine and scyllo-inositol than neuroblastomas (n = 7), classification accuracy was 94%. Supratentorial primitive neuro-ectodermal tumours had metabolite profiles in keeping with other primitive neuro-ectodermal tumours whilst ependymomas (n = 2) had metabolite profiles intermediate between pilocytic astrocytomas (n = 10) and primitive neuro-ectodermal tumours. HR-MAS identified key differences in the metabolite profiles of childhood brain and nervous system improving the molecular characterisation of these tumours. Further investigation of the underlying molecular pathways is required to assess their potential as targets for new agents.

  3. Rotor design for high pressure magic angle spinning nuclear magnetic resonance.

    PubMed

    Turcu, Romulus V F; Hoyt, David W; Rosso, Kevin M; Sears, Jesse A; Loring, John S; Felmy, Andrew R; Hu, Jian Zhi

    2013-01-01

    High pressure magic angle spinning (MAS) nuclear magnetic resonance (NMR) with a sample spinning rate exceeding 2.1 kHz and pressure greater than 165 bar has never been realized. In this work, a new sample cell design is reported, suitable for constructing cells of different sizes. Using a 7.5 mm high pressure MAS rotor as an example, internal pressure as high as 200 bar at a sample spinning rate of 6 kHz is achieved. The new high pressure MAS rotor is re-usable and compatible with most commercial NMR set-ups, exhibiting low (1)H and (13)C NMR background and offering maximal NMR sensitivity. As an example of its many possible applications, this new capability is applied to determine reaction products associated with the carbonation reaction of a natural mineral, antigorite ((Mg,Fe(2+))(3)Si(2)O(5)(OH)(4)), in contact with liquid water in water-saturated supercritical CO(2) (scCO(2)) at 150 bar and 50°C. This mineral is relevant to the deep geologic disposal of CO(2), but its iron content results in too many sample spinning sidebands at low spinning rate. Hence, this chemical system is a good case study to demonstrate the utility of the higher sample spinning rates that can be achieved by our new rotor design. We expect this new capability will be useful for exploring solid-state, including interfacial, chemistry at new levels of high-pressure in a wide variety of fields.

  4. Rotor design for high pressure magic angle spinning nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Turcu, Romulus V. F.; Hoyt, David W.; Rosso, Kevin M.; Sears, Jesse A.; Loring, John S.; Felmy, Andrew R.; Hu, Jian Zhi

    2013-01-01

    High pressure magic angle spinning (MAS) nuclear magnetic resonance (NMR) with a sample spinning rate exceeding 2.1 kHz and pressure greater than 165 bar has never been realized. In this work, a new sample cell design is reported, suitable for constructing cells of different sizes. Using a 7.5 mm high pressure MAS rotor as an example, internal pressure as high as 200 bar at a sample spinning rate of 6 kHz is achieved. The new high pressure MAS rotor is re-usable and compatible with most commercial NMR set-ups, exhibiting low 1H and 13C NMR background and offering maximal NMR sensitivity. As an example of its many possible applications, this new capability is applied to determine reaction products associated with the carbonation reaction of a natural mineral, antigorite ((Mg,Fe2+)3Si2O5(OH)4), in contact with liquid water in water-saturated supercritical CO2 (scCO2) at 150 bar and 50 °C. This mineral is relevant to the deep geologic disposal of CO2, but its iron content results in too many sample spinning sidebands at low spinning rate. Hence, this chemical system is a good case study to demonstrate the utility of the higher sample spinning rates that can be achieved by our new rotor design. We expect this new capability will be useful for exploring solid-state, including interfacial, chemistry at new levels of high-pressure in a wide variety of fields.

  5. Rotor Design for High Pressure Magic Angle Spinning Nuclear Magnetic Resonance

    SciTech Connect

    Turcu, Romulus V.F.; Hoyt, David W.; Rosso, Kevin M.; Sears, Jesse A.; Loring, John S.; Felmy, Andrew R.; Hu, Jian Z.

    2013-01-01

    High pressure magic angle spinning (MAS) nuclear magnetic resonance (NMR) with a sample spinning rate exceeding 2.1 kHz and pressure greater than 165 bar has never been realized. In this work, a new sample cell design is reported, suitable for constructing cells of different sizes. Using a 7.5 mm high pressure MAS rotor as an example, internal pressure as high as 200 bar at a sample spinning rate of 6 kHz is achieved. The new high pressure MAS rotor is re-usable and compatible with most commercial NMR set-ups, exhibiting low 1H and 13C NMR background and offering maximal NMR sensitivity. As an example of its many possible applications, this new capability is applied to determine reaction products associated with the carbonation reaction of a natural mineral, antigorite ((Mg,Fe2+)3Si2O5(OH)4), in contact with liquid water in water-saturated supercritical CO2 (scCO2) at 150 bar and 50 deg C. This mineral is relevant to the deep geologic disposal of CO2, but its iron content results in too many sample spinning sidebands at low spinning rate. Hence, this chemical system is a good case study to demonstrate the utility of the higher sample spinning rates that can be achieved by our new rotor design. We expect this new capability will be useful for exploring solid-state, including interfacial, chemistry at new levels of high-pressure in a wide variety of fields.

  6. Method of non-destructively inspecting a curved wall portion

    DOEpatents

    Fong, James T.

    1996-01-01

    A method of non-destructively inspecting a curved wall portion of a large and thick walled vessel for a defect by computed tomography is provided. A collimated source of radiation is placed adjacent one side of the wall portion and an array of detectors for the radiation is placed on the other side adjacent the source. The radiation from the source passing through the wall portion is then detected with the detectors over a limited angle, dependent upon the curvature of the wall of the vessel, to obtain a dataset. The source and array are then coordinately moved relative to the wall portion in steps and a further dataset is obtained at each step. The plurality of datasets obtained over the limited angle is then processed to produce a tomogram of the wall portion to determine the presence of a defect therein. In a preferred embodiment, the curved wall portion has a center of curvature so that the source and the array are positioned at each step along a respective arc curved about the center. If desired, the detector array and source can be reoriented relative to a new wall portion and an inspection of the new wall portion can be easily obtained. Further, the source and detector array can be indexed in a direction perpendicular to a plane including the limited angle in a plurality of steps so that by repeating the detecting and moving steps at each index step, a three dimensional image can be created of the wall portion.

  7. Non destructive testing of soft body armor

    NASA Astrophysics Data System (ADS)

    Bhise, Karan

    Pristine bullet proof vests are extremely effective at halting pre-determined projectile threats and have saved over 3000 lives. However, the effectiveness of these vests to halt a bullet is seen to decrease over time.Owing to the importance of bullet proof vests over a period of time, tests to determine their effectiveness have been carried out on every batch of vests at the time of inception and at certain time intervals by shooting a bullet through them. A few vests from every batch are picked up and shot at to check for bullet penetration during this process while these results are extrapolated onto the other vests from the batch.One of the main issues with this method is the fact that testing a few jackets among a large set of jackets does not guarantee the safety of every jacket in the entire batch.Further the jackets that are shot-at have the possibility of undergoing substantial damage during the process thus compromising its safety rendering them unsafe for future use.As the vest penetration phenomenon is extremely complex too, there arose a need for a better testing procedure that could not only help ensure more safety, but also save time and money.The new testing procedure proposed a non-destructive evaluation of the jackets that would solve the issues previous faced in testing the vests. This would lead to the building of a portable set up which could be carried to any location to test jackets in a matter of minutes thus saving time and money.

  8. Cryogenic Storage Tank Non-Destructive Evaluation

    NASA Technical Reports Server (NTRS)

    Arens, Ellen

    2010-01-01

    This slide presentation reviews the work in non-destructive evaluation (NDE) of cryogenic storage tanks. Four large cryogenic tanks, constructed in 1965 with perlite insulation in the annular regions, are of concern. The construction of the tanks, two Liquid Oxygen (LOX) and two Liquid Hydrogen (LH2), are described. The loss rate for the LOX tank at Pad A is slightly higher than that for the one at Pad B. The concerns for the LH2 tank at Pad B are that there is a significantly higher boil-off rate than that at Pad A, that there is mold growth, indicative of increased heat flow, that there is a long down-time needed for repairs, and that 3 of 5 full thermal cycles have been used on the Pad B LH2 tank. The advantages and disadvantages of thermal imaging are given. A detailed description of what is visible of the structures in the infra-red is given and views of the thermal images are included. Missing Perlite is given as the probable cause of the cold spot on the Pad B LH2 tank. There is no indications of problematic cold regions on the Pad A LH2 tank, as shown by the thermal images given in the presentation. There is definite indication of a cold region on the Pad A LOX tank. There is however concerns with thermal imaging, as thermal images can be significantly effected by environmental conditions, image differences on similar days but with different wind speeds. Other effects that must be considered include ambient temperature, humidity levels/dew, and cloud reflections

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

    PubMed

    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

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

    NASA Astrophysics Data System (ADS)

    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

  11. In Vivo Detection of the Cyclic Osmoregulated Periplasmic Glucan of Ralstonia solanacearum by High-Resolution Magic Angle Spinning NMR

    NASA Astrophysics Data System (ADS)

    Wieruszeski, J.-M.; Bohin, A.; Bohin, J.-P.; Lippens, G.

    2001-07-01

    We investigate the mobility of the osmoregulated periplasmic glucans of Ralstonia solanacearum in the bacterial periplasm through the use of high-resolution (HR) NMR spectroscopy under static and magic angle spinning (MAS) conditions. Because the nature of periplasm is far from an isotropic aqueous solution, the molecules could be freely diffusing or rather associated to a periplasmic protein, a membrane protein, a lipid, or the peptidoglycan. HR MAS NMR spectroscopy leads to more reproducible results and allows the in vivo detection and characterization of the complex molecule.

  12. Use of rotary echoes in 2H magic-angle spinning NMR for the quantitative study of molecular dynamics

    NASA Astrophysics Data System (ADS)

    Hogg, Naomi H. M.; Boulton, Paul J. T.; Zorin, Vadim E.; Harris, Robin K.; Hodgkinson, Paul

    2009-06-01

    The interaction of sample spinning and chemical dynamics is analysed in the context of 2H magic-angle spinning NMR. We develop previous analyses and show that a metric based on the intensity of rotational echoes allows kinetic information to be derived without the need for full modelling of the NMR response. This approach is illustrated on the conformational exchange of 1,4-dioxane included in the channel solvate hydrate formed with finasteride. An activation barrier in excellent agreement with previous experimental and theoretical estimates is obtained, without the need for modelling which would be very challenging due to the anisotropic tumbling of the solvent molecules.

  13. High Resolution Magic Angle Spinning 1H-NMR Metabolic Profiling of Nanoliter Biological Tissues at High Magnetic Field

    SciTech Connect

    Feng, Ju; Hu, Jian Z.; Burton, Sarah D.; Hoyt, David W.

    2013-03-05

    It is demonstrated that a high resolution magic angle spinning 1H-NMR spectrum of biological tissue samples with volumes as small as 150 nanoliters, or 0.15 mg in weight, can be acquired in a few minutes at 21.1 T magnetic field using a commercial 1.6 mm fast-MAS probe with minor modification of the MAS rotor. The strategies of sealing the samples inside the MAS rotor to avoid fluid leakage as well as the ways of optimizing the signal to noise are discussed.

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

    DOEpatents

    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.

  15. NON-DESTRUCTIVE SOIL CARBON ANALYZER.

    SciTech Connect

    Wielopolski, Lucian; Hendrey, G.; Orion, I.; Prior, S.; Rogers, H.; Runion, B.; Torbert, A.

    2004-02-01

    This report describes the feasibility, calibration, and safety considerations of a non-destructive, in situ, quantitative, volumetric soil carbon analytical method based on inelastic neutron scattering (INS). The method can quantify values as low as 0.018 gC/cc, or about 1.2% carbon by weight with high precision under the instrument's configuration and operating conditions reported here. INS is safe and easy to use, residual soil activation declines to background values in under an hour, and no radiological requirements are needed for transporting the instrument. The labor required to obtain soil-carbon data is about 10-fold less than with other methods, and the instrument offers a nearly instantaneous rate of output of carbon-content values. Furthermore, it has the potential to quantify other elements, particularly nitrogen. New instrumentation was developed in response to a research solicitation from the U.S. Department of Energy (DOE LAB 00-09 Carbon Sequestration Research Program) supporting the Terrestrial Carbon Processes (TCP) program of the Office of Science, Biological and Environmental Research (BER). The solicitation called for developing and demonstrating novel techniques for quantitatively measuring changes in soil carbon. The report includes raw data and analyses of a set of proof-of-concept, double-blind studies to evaluate the INS approach in the first phase of developing the instrument. Managing soils so that they sequester massive amounts of carbon was suggested as a means to mitigate the atmospheric buildup of anthropogenic CO{sub 2}. Quantifying changes in the soils' carbon stocks will be essential to evaluating such schemes and documenting their performance. Current methods for quantifying carbon in soil by excavation and core sampling are invasive, slow, labor-intensive and locally destroy the system being observed. Newly emerging technologies, such as Laser Induced Breakdown Spectroscopy and Near-Infrared Spectroscopy, offer soil

  16. Parameter independent low-power heteronuclear decoupling for fast magic-angle spinning solid-state NMR

    NASA Astrophysics Data System (ADS)

    Equbal, Asif; Madhu, P. K.; Meier, Beat H.; Nielsen, Niels Chr.; Ernst, Matthias; Agarwal, Vipin

    2017-02-01

    Major advances have recently been made in the field of heteronuclear dipolar decoupling in solid-state nuclear magnetic resonance (NMR). These developments have improved the resolution and sensitivity of the NMR spectrum of spins coupled to protons. One such new scheme, denoted as rCWApA, has proven to be robust with practically no need for parameter optimization [A. Equbal et al. Chem. Phys. Lett., 635, 339 (2015)]. Most of the experiments with rCWApA have been carried out in the regimes of slow to moderate magic-angle spinning while simultaneously applying high decoupling radio-frequency amplitudes. Here, we explore the performance of the rCWApA sequence and its predecessor rCWA in the regime of low-power radio-frequency irradiation and fast magic-angle spinning. The robustness of the refocused continuous-wave (rCW) schemes to experimental parameters such as pulse lengths and offset irradiation is demonstrated. Numerical simulations and analytical theory have been used to understand the effects of various nuclear spin interactions on the decoupling performance of the low-power rCW decoupling scheme relative to other decoupling methods. This has lead to the design of an "optimum low-power decoupling sequence" that can be used without parameter optimization. This result is particularly important in the context of samples with low signal to noise.

  17. Studying Dynamics by Magic-Angle Spinning Solid-State NMR Spectroscopy: Principles and Applications to Biomolecules

    PubMed Central

    Schanda, Paul; Ernst, Matthias

    2016-01-01

    Magic-angle spinning solid-state NMR spectroscopy is an important technique to study molecular structure, dynamics and interactions, and is rapidly gaining importance in biomolecular sciences. Here we provide an overview of experimental approaches to study molecular dynamics by MAS solid-state NMR, with an emphasis on the underlying theoretical concepts and differences of MAS solid-state NMR compared to solution-state NMR. The theoretical foundations of nuclear spin relaxation are revisited, focusing on the particularities of spin relaxation in solid samples under magic-angle spinning. We discuss the range of validity of Redfield theory, as well as the inherent multi-exponential behavior of relaxation in solids. Experimental challenges for measuring relaxation parameters in MAS solid-state NMR and a few recently proposed relaxation approaches are discussed, which provide information about time scales and amplitudes of motions ranging from picoseconds to milliseconds. We also discuss the theoretical basis and experimental measurements of anisotropic interactions (chemical-shift anisotropies, dipolar and quadrupolar couplings), which give direct information about the amplitude of motions. The potential of combining relaxation data with such measurements of dynamically-averaged anisotropic interactions is discussed. Although the focus of this review is on the theoretical foundations of dynamics studies rather than their application, we close by discussing a small number of recent dynamics studies, where the dynamic properties of proteins in crystals are compared to those in solution. PMID:27110043

  18. Lipid bilayer preparations of membrane proteins for oriented and magic-angle spinning solid-state NMR samples

    PubMed Central

    Das, Nabanita; Murray, Dylan T; Cross, Timothy A

    2014-01-01

    Solid-state NMR spectroscopy has been used successfully for characterizing the structure and dynamics of membrane proteins as well as their interactions with other proteins in lipid bilayers. such an environment is often necessary for achieving native-like structures. sample preparation is the key to this success. Here we present a detailed description of a robust protocol that results in high-quality membrane protein samples for both magic-angle spinning and oriented-sample solid-state NMR. the procedure is demonstrated using two proteins: CrgA (two transmembrane helices) and rv1861 (three transmembrane helices), both from Mycobacterium tuberculosis. the success of this procedure relies on two points. First, for samples for both types of NMR experiment, the reconstitution of the protein from a detergent environment to an environment in which it is incorporated into liposomes results in ‘complete’ removal of detergent. second, for the oriented samples, proper dehydration followed by rehydration of the proteoliposomes is essential. By using this protocol, proteoliposome samples for magic-angle spinning NMR and uniformly aligned samples (orientational mosaicity of <1°) for oriented-sample NMR can be obtained within 10 d. PMID:24157546

  19. Parameter independent low-power heteronuclear decoupling for fast magic-angle spinning solid-state NMR.

    PubMed

    Equbal, Asif; Madhu, P K; Meier, Beat H; Nielsen, Niels Chr; Ernst, Matthias; Agarwal, Vipin

    2017-02-28

    Major advances have recently been made in the field of heteronuclear dipolar decoupling in solid-state nuclear magnetic resonance (NMR). These developments have improved the resolution and sensitivity of the NMR spectrum of spins coupled to protons. One such new scheme, denoted as rCW(ApA), has proven to be robust with practically no need for parameter optimization [A. Equbal et al. Chem. Phys. Lett., 635, 339 (2015)]. Most of the experiments with rCW(ApA) have been carried out in the regimes of slow to moderate magic-angle spinning while simultaneously applying high decoupling radio-frequency amplitudes. Here, we explore the performance of the rCW(ApA) sequence and its predecessor rCW(A) in the regime of low-power radio-frequency irradiation and fast magic-angle spinning. The robustness of the refocused continuous-wave (rCW) schemes to experimental parameters such as pulse lengths and offset irradiation is demonstrated. Numerical simulations and analytical theory have been used to understand the effects of various nuclear spin interactions on the decoupling performance of the low-power rCW decoupling scheme relative to other decoupling methods. This has lead to the design of an "optimum low-power decoupling sequence" that can be used without parameter optimization. This result is particularly important in the context of samples with low signal to noise.

  20. Floquet-Magnus expansion for general N-coupled spins systems in magic-angle spinning nuclear magnetic resonance spectra

    NASA Astrophysics Data System (ADS)

    Mananga, Eugene Stephane; Charpentier, Thibault

    2015-04-01

    In this paper we present a theoretical perturbative approach for describing the NMR spectrum of strongly dipolar-coupled spin systems under fast magic-angle spinning. Our treatment is based on two approaches: the Floquet approach and the Floquet-Magnus expansion. The Floquet approach is well known in the NMR community as a perturbative approach to get analytical approximations. Numerical procedures are based on step-by-step numerical integration of the corresponding differential equations. The Floquet-Magnus expansion is a perturbative approach of the Floquet theory. Furthermore, we address the " γ -encoding" effect using the Floquet-Magnus expansion approach. We show that the average over " γ " angle can be performed for any Hamiltonian with γ symmetry.

  1. Effective Floquet Hamiltonians for dipolar and quadrupolar coupled N-spin systems in solid state nuclear magnetic resonance under magic angle spinning.

    PubMed

    Pandey, Manoj Kumar; Krishnan, Mangala Sunder

    2010-11-07

    Spin dynamics under magic angle spinning has been studied using different theoretical approaches and also by extensive numerical simulation programs. In this article we present a general theoretical approach that leads to analytic forms for effective Hamiltonians for an N-spin dipolar and quadrupolar coupled system under magic angle spinning (MAS) conditions, using a combination of Floquet theory and van Vleck (contact) transformation. The analytic forms presented are shown to be useful for the study of MAS spin dynamics in solids with the help of a number of simulations in two, three, and four coupled, spin-1/2 systems as well as spins in which quadrupolar interactions are also present.

  2. Non-Destructive Classification Approaches for Equilibrated Ordinary Chondrites

    NASA Astrophysics Data System (ADS)

    Righter, K.; Harrington, R.; Schroeder, C.; Morris, R. V.

    2013-09-01

    In order to compare a few non-destructive classification techniques with the standard approaches, we have characterized a group of chondrites from the Larkman Nunatak region using magnetic susceptibility and Mössbauer spectroscopy.

  3. NON-DESTRUCTIVE TESTING METHODS FOR GEOTHERMAL PIPING.

    SciTech Connect

    BERNDT,M.L.

    2001-03-23

    Non-destructive testing is a key component of optimized plant inspection and maintenance programs. Risk based inspection, condition based maintenance and reliability centered maintenance systems all require detection, location and sizing of defects or flaws by non-destructive methods. Internal damage of geothermal piping by corrosion and erosion-corrosion is an ongoing problem requiring inspection and subsequent maintenance decisions to ensure safe and reliable performance. Conventional manual ultrasonic testing to determine remaining wall thickness has major limitations, particularly when damage is of a random and localized nature. Therefore, it is necessary to explore alternative non-destructive methods that offer potential benefits in terms of accurate quantification of size, shape and location of damage, probability of detection, ability to use on-line over long ranges, and economics. A review of non-destructive methods and their applicability to geothermal piping was performed. Based on this, ongoing research will concentrate on long range guided wave and dynamic methods.

  4. A Review of Non-destructive Detection for Fruit Quality

    NASA Astrophysics Data System (ADS)

    Gao, Haisheng; Zhu, Fengmei; Cai, Jinxing

    An overview of non-destructive detection in quality of post-harvest fruit was presented in this paper, and the research and application were discussed. This paper elaborated the fruit quality detection methods which were based on one of the following properties: optical properties, sonic vibration, machine vision technique, nuclear magnetic resonance (NMR), electronic noses, electrical properties, computed tomography. At last, the main problems of non-destructive detection in application were also explained.

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

    SciTech Connect

    Mao, Kanmi

    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

  6. High resolution magic angle spinning NMR applied to the analysis of organic compounds bound to solid supports.

    PubMed

    Espinosa, Juan F

    2011-01-01

    In situ structural characterization of organic compounds attached to solid supports can be achieved by high-resolution magic angle spinning NMR (HRMAS NMR), a technique that provides solution-like spectra for resin-bound molecules. This review outlines the principles of the technique, the influence of the solid support on data quality, and NMR experiments that are useful for obtaining valuable information. The review describes, with multiple examples mainly from the last 7 years, how HRMAS NMR has been applied to monitor solid-phase reactions, elucidate reaction products and quantify compound loading on a solid support. Other applications, such as conformational analysis of immobilized compounds and investigation of molecular interactions with compounds in solution, are also discussed.

  7. Experimental study of resolution of proton chemical shifts in solids: Combined multiple pulse NMR and magic-angle spinning

    SciTech Connect

    Ryan, L.M.; Taylor, R.E.; Paff, A.J.; Gerstein, B.C.

    1980-01-01

    High-resolution nuclear magnetic resonance spectra of protons in rigid, randomly oriented solids have been measured using combined homonuclear dipolar decoupling (via multiple pulse techniques) and attenuation of chemical shift anisotropies (via magic-angle sample spinning). Under those conditions, isotropic proton chemical shifts were recorded for a variety of chemical species, with individual linewidths varying from about 55 to 110 Hz (1--2 ppm). Residual line broadening was due predominately to (i) magnetic-field instability and inhomogeneity, (ii) unresolved proton--proton spin couplings, (iii) chemical shift dispersion, (iv) residual dipolar broadening, and (v) lifetime broadening under the multiple pulse sequences used. The magnitudes of those effects and the current limits of resolution for this experiment in our spectrometer have been investigated. The compounds studied included organic solids (4, 4'-dimethylbenzophenone, 2, 6-dimethylbenzoic acid, and aspirin), polymers (polystyrene and polymethylmethacrylate), and the vitrain portion of a bituminous coal.

  8. Measurement of lateral diffusion rates in membranes by pulsed magnetic field gradient, magic angle spinning-proton nuclear magnetic resonance.

    PubMed

    Gawrisch, Klaus; Gaede, Holly C

    2007-01-01

    Membrane organization, including the presence of domains, can be characterized by measuring lateral diffusion rates of lipids and membrane-bound substances. Magic angle spinning (MAS) yields well-resolved proton nuclear magnetic resonance (NMR) of lipids in biomembranes. When combined with pulsed-field gradient NMR (rendering what is called "pulsed magnetic field gradients-MAS-NMR"), it permits precise diffusion measurements on the micrometer lengths scale for any substance with reasonably well-resolved proton MAS-NMR resonances, without the need of preparing oriented samples. Sample preparation procedures, the technical requirements for the NMR equipment, and spectrometer settings are described. Additionally, equations for analysis of diffusion data obtained from unoriented samples, and a method for correcting the data for liposome curvature are provided.

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

    PubMed

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A

    2017-02-22

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

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

    PubMed

    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.

  11. Effect of positional isomerism and vanadium substitution on (51)V magic angle spinning NMR Spectra Of Wells-Dawson polyoxotungstates.

    PubMed

    Gupta, Rupal; Huang, Wenlin; Francesconi, Lynn C; Polenova, Tatyana

    We examined the positional isomerism and vanadium substitution on the (51)V magic angle spinning NMR spectra of potassium salts of vanadium-substituted polyoxotungstates of the Wells-Dawson series. NMR parameters of this class of catalytically active polyoxotungstates effect of are reported. Multiple species, indicative of differences in the local environment at the substitution sites, are observed in solid-state NMR spectra of the di- and tri- substituted complexes in contrast to solution NMR spectra, where single average chemical shift was observed. The quadrupolar and chemical shift anisotropy parameters depend strongly on the position and the degree of the vanadium substitution into the oxoanion core establishing (51)V SATRAS NMR spectroscopy as a sensitive probe of the local electronic environment in these catalytically active solids. Copyright © 2016 Elsevier Inc. All rights reserved.

  12. Detailed mechanisms of (1)H spin-lattice relaxation in ammonium dihydrogen phosphate confirmed by magic angle spinning.

    PubMed

    Hayashi, Shigenobu; Jimura, Keiko

    2017-07-08

    Mechanisms of the (1)H spin-lattice relaxation in NH4H2PO4 were studied in detail by use of the effect of magic angle spinning on the relaxation. The acid and the ammonium protons have different relaxation times at the spinning rates higher than 10 kHz due to suppression of spin diffusion between the two kinds of protons. The intrinsic relaxation times not affected by the spin diffusion and the spin-diffusion assisted relaxation times were evaluated separately, taking into consideration temperature dependence. Both mechanisms contribute to the (1)H relaxation of the acid protons comparatively. The spin-diffusion assisted relaxation mechanism was suppressed to the level lower than the experimental errors at the spinning rate of 30 kHz. Copyright © 2017 Elsevier Inc. All rights reserved.

  13. Chemical shift powder spectra enhanced by multiple-contact cross-polarization under slow magic-angle spinning.

    PubMed

    Raya, Jésus; Perrone, Barbara; Hirschinger, Jérôme

    2013-02-01

    A simple multiple-contact cross-polarization (CP) scheme is applied to a powder sample of ferrocene and β-calcium formate under static and magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. We show that multiple equilibrations-re-equilibrations with the proton spin bath improves the polarization transfer efficiency at short contact times and provides higher signal enhancements than state-of-the art techniques such as adiabatic passage through the Hartmann-Hahn condition CP (APHH-CP) when MAS is applied. The resulting chemical shift powder spectra then are identical to the ones obtained by using ROtor-Directed Exchange of Orientations CP (APHH-RODEO-CP) with intensity gains of a factor 1.1-1.3.

  14. Chemical shift powder spectra enhanced by multiple-contact cross-polarization under slow magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Raya, Jésus; Perrone, Barbara; Hirschinger, Jérôme

    2013-02-01

    A simple multiple-contact cross-polarization (CP) scheme is applied to a powder sample of ferrocene and β-calcium formate under static and magic-angle spinning (MAS) conditions. The method is described analytically through the density matrix formalism. We show that multiple equilibrations-re-equilibrations with the proton spin bath improves the polarization transfer efficiency at short contact times and provides higher signal enhancements than state-of-the art techniques such as adiabatic passage through the Hartmann-Hahn condition CP (APHH-CP) when MAS is applied. The resulting chemical shift powder spectra then are identical to the ones obtained by using ROtor-Directed Exchange of Orientations CP (APHH-RODEO-CP) with intensity gains of a factor 1.1-1.3.

  15. Nondestructive high-resolution solid-state NMR of rotating thin films at the magic-angle.

    PubMed

    Inukai, Munehiro; Noda, Yasuto; Takeda, Kazuyuki

    2011-12-01

    We present a new approach to nondestructive magic-angle spinning (MAS) nuclear magnetic resonance (NMR) for thin films. In this scheme, the sample put on the top of a rotor is spun using the conventional MAS system, and the NMR signals are detected with an additional coil. Stable spinning of disk-shaped samples with diameters of 7 mm and 12 mm at 14.2 and 7 kHz are feasible. We present 7Li MAS NMR experiments of a thin-film sample of LiCoO2 with a thickness of 200 nm. Taking advantage of the nondestructive feature of the experiment, we also demonstrate ex situ experiments, by tracing conformation change upon annealing for various durations. This approach opens the door for in situ MAS NMR of thin-film devices as well. Copyright © 2011 Elsevier Inc. All rights reserved.

  16. Magic Angle Spinning NMR Investigation of Influenza A M218-60: Support for an Allosteric Mechanism of Inhibition

    PubMed Central

    Andreas, Loren B.; Eddy, Matthew T.; Pielak, Rafal M.; Chou, James; Griffin, Robert G.

    2010-01-01

    The tetrameric M2 proton channel from influenza A virus conducts protons at low pH and is inhibited by aminoadamantyl drugs such as amantadine and rimantadine. We report magic angle spinning NMR spectra of POPC and DPhPC membrane embedded M218-60, both apo and in the presence of rimantadine. Similar linewidths in spectra of apo and bound M2 indicate that rimantadine does not have a significant impact on the dynamics or conformational heterogeneity of this construct. Substantial chemical shift changes for many residues in the transmembrane region support an allosteric mechanism of inhibition. A Rmt titration supports a binding stoichiometry of >1 Rmt molecule per channel while showing that nonspecific bindin0g or changes in membrane composition are unlikely sources of the chemical shift changes. In addition, doubling of spectral lines in all of the observed samples provides evidence that the channel assembles with twofold symmetry. PMID:20698642

  17. Properties of mixtures of cholesterol with phosphatidylcholine or with phosphatidylserine studied by (13)C magic angle spinning nuclear magnetic resonance.

    PubMed Central

    Epand, Richard M; Bain, Alex D; Sayer, Brian G; Bach, Diana; Wachtel, Ellen

    2002-01-01

    The behavior of cholesterol is different in mixtures with phosphatidylcholine as compared with phosphatidylserine. In (13)C cross polarization/magic angle spinning nuclear magnetic resonance spectra, resonance peaks of the vinylic carbons of cholesterol are a doublet in samples containing 0.3 or 0.5 mol fraction cholesterol with 1-palmitoyl-2-oleoyl phosphatidylserine (POPS) or in cholesterol monohydrate crystals, but a singlet with mixtures of cholesterol and 1-palmitoyl-2-oleoyl phosphatidylcholine (POPC). At these molar fractions of cholesterol with POPS, resonances of the C-18 of cholesterol appear at the same chemical shifts as in pure cholesterol monohydrate crystals. These resonances do not appear in samples of POPS with 0.2 mol fraction cholesterol or with POPC up to 0.5 mol fraction cholesterol. In addition, there is another resonance from the cholesterol C18 that appears in all of the mixtures of phospholipid and cholesterol but not in pure cholesterol monohydrate crystals. Using direct polarization, the fraction of cholesterol present as crystallites in POPS with 0.5 mol fraction cholesterol is found to be 80%, whereas with the same mol fraction of cholesterol and POPC none of the cholesterol is crystalline. After many hours of incubation, cholesterol monohydrate crystals in POPS undergo a change that results in an increase in the intensity of certain resonances of cholesterol monohydrate in (13)C cross polarization/magic angle spinning nuclear magnetic resonance, indicating a rigidification of the C and D rings of cholesterol but not other regions of the molecule. PMID:12324423

  18. NonDestructive Evaluation for Industrial & Development Applications

    SciTech Connect

    Hunter, James F.

    2016-10-12

    Provide overview of weld inspection for Non-Destructive Testing at LANL. This includes radiography (RT/DR/CR/CT for x-ray & neutron sources), ultrasonic testing (UT/PAUT), dye penetrant inspection (PT), eddy current inspection (ET) and magnetic particle testing (MT). Facilities and capabilities for weld inspection will be summarized with examples.

  19. Non-destructive methods for food texture assessment

    USDA-ARS?s Scientific Manuscript database

    Food texture is important to the successful marketing and profitability of food products. Non-destructive sensing would allow food producers and processors to inspect, sort, grade, or track individual product items, so that they can deliver consistent, superior food products to the marketplace. Over...

  20. Shocked quartz: A {sup 29}Si magic-angle-spinning nuclear magnetic resonance study

    SciTech Connect

    Fiske, P.S.; Nellis, W.J.; Xu, Z.; Stebbins, J.F.

    1998-11-01

    Quantitative {sup 29}Si NMR spectra of single-crystal {alpha}-quartz, shock compressed to 12--38 GPa and recovered, provide new information about the complex response of quartz to shock loading. Spectra from samples recovered from shock pressures of 12--20 GPa show a broadening of the {sup 29}Si NMR peak and the development of asymmetry toward lower NMR frequency (indicating an increase in the mean Si-O-Si intertetrahedral bond angle). NMR spectra of samples shock compressed above {approximately}25 GPa show increasing amounts of a separate amorphous phase of SiO{sub 2} with a mean Si-O-Si bond angle roughly 5{degree} narrower, and 10--15% denser, than fused SiO{sub 2}. Small amounts of crystalline material remain with a mean Si-O-Si bond angle up to 3{degree} larger than unshocked {alpha}-quartz. The recovery of dense glass indicates that post-shock temperatures were sufficiently low to also preserve stishovite, had any been created in the experiments. The paucity of stishovite or Si in an amorphous phase in the recovered samples suggests that the formation of stable, high-coordinated Si is kinetically hindered in shock compression experiments up to about 35--40 GPa, except in regions of high temperature, such as planar deformation features (PDFs), microfaults (pseudotachylites), or voids.

  1. Satellite transitions acquired in real time by magic angle spinning (STARTMAS): ``Ultrafast'' high-resolution MAS NMR spectroscopy of spin I =3/2 nuclei

    NASA Astrophysics Data System (ADS)

    Thrippleton, Michael J.; Ball, Thomas J.; Wimperis, Stephen

    2008-01-01

    The satellite transitions acquired in real time by magic angle spinning (STARTMAS) NMR experiment combines a train of pulses with sample rotation at the magic angle to refocus the first- and second-order quadrupolar broadening of spin I =3/2 nuclei in a series of echoes, while allowing the isotropic chemical and quadrupolar shifts to evolve. The result is real-time isotropic NMR spectra at high spinning rates using conventional MAS equipment. In this paper we describe in detail how STARTMAS data can be acquired and processed with ease on commercial equipment. We also discuss the advantages and limitations of the approach and illustrate the discussion with numerical simulations and experimental data from four different powdered solids.

  2. 15N photochemically induced dynamic nuclear polarization magic-angle spinning NMR analysis of the electron donor of photosystem II

    PubMed Central

    Diller, Anna; Roy, Esha; Gast, Peter; van Gorkom, Hans J.; de Groot, Huub J. M.; Glaubitz, Clemens; Jeschke, Gunnar; Matysik, Jörg; Alia, A.

    2007-01-01

    In natural photosynthesis, the two photosystems that operate in series to drive electron transport from water to carbon dioxide are quite similar in structure and function, but operate at widely different potentials. In both systems photochemistry begins by photo-oxidation of a chlorophyll a, but that in photosystem II (PS2) has a 0.7 eV higher midpoint potential than that in photosystem I (PS1), so their electronic structures must be very different. Using reaction centers from 15N-labeled spinach, these electronic structures are compared by their photochemically induced dynamic nuclear polarization (photo-CIDNP) in magic-angle spinning (MAS) NMR measurements. The results show that the electron spin distribution in PS1, apart from its known delocalization over 2 chlorophyll molecules, reveals no marked disturbance, whereas the pattern of electron spin density distribution in PS2 is inverted in the oxidized radical state. A model for the donor of PS2 is presented explaining the inversion of electron spin density based on a tilt of the axial histidine toward pyrrole ring IV causing π-π overlap of both aromatic systems. PMID:17652174

  3. Evaluating Human Breast Ductal Carcinomas with High-Resolution Magic-Angle Spinning Proton Magnetic Resonance Spectroscopy

    NASA Astrophysics Data System (ADS)

    Cheng, Leo Ling; Chang, I.-Wen; Smith, Barbara L.; Gonzalez, R. Gilberto

    1998-11-01

    We report the results of a study of human breast ductal carcinomas, conducted by using high resolution magic angle spinning proton magnetic resonance spectroscopy (HRMAS 1HMRS). This recently developed spectroscopic technique can measure tissue metabolism from intact pathological specimens and identify tissue biochemical changes, which closely correspond to tumorin vivostate. This procedure objectively indicates diagnostic parameters, independent of the skill and experience of the investigator, and has the potential to reduce the sampling errors inherently associated with procedures of conventional histopathology. In this study, we measured 19 cases of female ductal carcinomas. Our results demonstrate that: (1) highly resolved spectra of intact specimens of human breast ductal carcinomas can be obtained; (2) carcinoma-free tissues and carcinomas are distinguishable by alterations in the intensities and the spin-spin relaxation time T2 of cellular metabolites; and (3) tumor metabolic markers, such as phosphocholine, lactate, and lipids, may correlate with the histopathological grade determined from evaluation of the adjacent specimen. Our results suggest that biochemical markers thus measured may function as a valuable adjunct to histopathology to improve the accuracy of and reduce the time frame required for the diagnosis of human breast cancer.

  4. Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K.

    PubMed

    Thurber, Kent R; Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

    2013-01-01

    We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20-25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier, but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30 mW circularly polarized microwave source at 264 GHz, MAS at 6.8 kHz, and 21 K sample temperature, greater than 25-fold enhancements of cross-polarized (13)C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional (13)C MAS NMR spectra of frozen solutions of uniformly (13)C-labeled l-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly (13)C-labeled amino acids. Published by Elsevier Inc.

  5. Solid state nuclear magnetic resonance with magic-angle spinning and dynamic nuclear polarization below 25 K

    PubMed Central

    Thurber, Kent R.; Potapov, Alexey; Yau, Wai-Ming; Tycko, Robert

    2012-01-01

    We describe an apparatus for solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS) at 20–25 K and 9.4 Tesla. The MAS NMR probe uses helium to cool the sample space and nitrogen gas for MAS drive and bearings, as described earlier (Thurber et al., J. Magn. Reson. 2008) [1], but also includes a corrugated waveguide for transmission of microwaves from below the probe to the sample. With a 30 mW circularly polarized microwave source at 264 GHz, MAS at 6.8 kHz, and 21 K sample temperature, greater than 25-fold enhancements of cross-polarized 13C NMR signals are observed in spectra of frozen glycerol/water solutions containing the triradical dopant DOTOPA-TEMPO when microwaves are applied. As demonstrations, we present DNP-enhanced one-dimensional and two-dimensional 13C MAS NMR spectra of frozen solutions of uniformly 13C-labeled L-alanine and melittin, a 26-residue helical peptide that we have synthesized with four uniformly 13C-labeled amino acids. PMID:23238592

  6. Metabolic profiling of lung granuloma in Mycobacterium tuberculosis infected guinea pigs: ex vivo 1H magic angle spinning NMR studies.

    PubMed

    Somashekar, B S; Amin, Anita G; Rithner, Christopher D; Troudt, JoLynn; Basaraba, Randall; Izzo, Angelo; Crick, Dean C; Chatterjee, Delphi

    2011-09-02

    A crucial and distinctive feature of tuberculosis infection is that Mycobacterium tuberculosis (Mtb) resides in granulomatous lesion at various stages of disease development and necrosis, an aspect that is little understood. We used a novel approach, applying high resolution magic angle spinning nuclear magnetic resonance spectroscopy (HRMAS NMR) directly to infected tissues, allowing us to study the development of tuberculosis granulomas in guinea pigs in an untargeted manner. Significant up-regulation of lactate, alanine, acetate, glutamate, oxidized and the reduced form of glutathione, aspartate, creatine, phosphocholine, glycerophosphocholine, betaine, trimethylamine N-oxide, myo-inositol, scyllo-inositol, and dihydroxyacetone was clearly visualized and was identified as the infection progressed. Concomitantly, phosphatidylcholine was down-regulated. Principal component analysis of NMR data revealed clear group separation between infected and uninfected tissues. These metabolites are suggestive of utilization of alternate energy sources by the infiltrating cells that generate much of the metabolites in the increasingly necrotic and hypoxic developing granuloma through the glycolytic, pentose phosphate, and tricarboxylic acid pathways. The most relevant changes seen are, surprisingly, very similar to metabolic changes seen in cancer during tumor development.

  7. Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning.

    PubMed

    Thurber, Kent; Tycko, Robert

    2016-03-01

    We describe novel instrumentation for low-temperature solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS), focusing on aspects of this instrumentation that have not been described in detail in previous publications. We characterize the performance of an extended interaction oscillator (EIO) microwave source, operating near 264 GHz with 1.5 W output power, which we use in conjunction with a quasi-optical microwave polarizing system and a MAS NMR probe that employs liquid helium for sample cooling and nitrogen gas for sample spinning. Enhancement factors for cross-polarized (13)C NMR signals in the 100-200 range are demonstrated with DNP at 25K. The dependences of signal amplitudes on sample temperature, as well as microwave power, polarization, and frequency, are presented. We show that sample temperatures below 30K can be achieved with helium consumption rates below 1.3 l/h. To illustrate potential applications of this instrumentation in structural studies of biochemical systems, we compare results from low-temperature DNP experiments on a calmodulin-binding peptide in its free and bound states.

  8. Closed-cycle cold helium magic-angle spinning for sensitivity-enhanced multi-dimensional solid-state NMR.

    PubMed

    Matsuki, Yoh; Nakamura, Shinji; Fukui, Shigeo; Suematsu, Hiroto; Fujiwara, Toshimichi

    2015-10-01

    Magic-angle spinning (MAS) NMR is a powerful tool for studying molecular structure and dynamics, but suffers from its low sensitivity. Here, we developed a novel helium-cooling MAS NMR probe system adopting a closed-loop gas recirculation mechanism. In addition to the sensitivity gain due to low temperature, the present system has enabled highly stable MAS (vR=4-12 kHz) at cryogenic temperatures (T=35-120 K) for over a week without consuming helium at a cost for electricity of 16 kW/h. High-resolution 1D and 2D data were recorded for a crystalline tri-peptide sample at T=40 K and B0=16.4 T, where an order of magnitude of sensitivity gain was demonstrated versus room temperature measurement. The low-cost and long-term stable MAS strongly promotes broader application of the brute-force sensitivity-enhanced multi-dimensional MAS NMR, as well as dynamic nuclear polarization (DNP)-enhanced NMR in a temperature range lower than 100 K.

  9. Evaluation of Cancer Metabolomics Using ex vivo High Resolution Magic Angle Spinning (HRMAS) Magnetic Resonance Spectroscopy (MRS)

    PubMed Central

    Fuss, Taylor L.; Cheng, Leo L.

    2016-01-01

    According to World Health Organization (WHO) estimates, cancer is responsible for more deaths than all coronary heart disease or stroke worldwide, serving as a major public health threat around the world. High resolution magic angle spinning (HRMAS) magnetic resonance spectroscopy (MRS) has demonstrated its usefulness in the identification of cancer metabolic markers with the potential to improve diagnosis and prognosis for the oncology clinic, due partially to its ability to preserve tissue architecture for subsequent histological and molecular pathology analysis. Capable of the quantification of individual metabolites, ratios of metabolites, and entire metabolomic profiles, HRMAS MRS is one of the major techniques now used in cancer metabolomic research. This article reviews and discusses literature reports of HRMAS MRS studies of cancer metabolomics published between 2010 and 2015 according to anatomical origins, including brain, breast, prostate, lung, gastrointestinal, and neuroendocrine cancers. These studies focused on improving diagnosis and understanding patient prognostication, monitoring treatment effects, as well as correlating with the use of in vivo MRS in cancer clinics. PMID:27011205

  10. Rotational resonance for a heteronuclear spin pair under magic-angle spinning in solid-state NMR

    NASA Astrophysics Data System (ADS)

    Kamihara, Takayuki; Takegoshi, K.

    2017-04-01

    Rotational resonance (R2) is one of the widely applied techniques in solid-state NMR for recoupling a homonuclear dipolar interaction under magic-angle spinning (MAS). R2 occurs as the result of interference between the difference of the chemical shifts and MAS. In this work, we extend R2 to a heteronuclear dipolar interaction in the interaction frame of RF irradiation. Based on the average Hamiltonian theory, we show that the recoupling of the heteronuclear dipolar (I-S) interaction occurs at the recoupling conditions written as ΩI'±ΩS' =k ωr (k =0 ,±1 ,±2 ), where ΩX' is the RF offset for spin-X (X = I or S) scaled by RF irradiation. The new recoupling sequence for a heteronuclear spin pair is referred to as offset-driven cross polarization along the z axis (OD-CPZ). With the robustness for RF inhomogeneity and ten recoupling conditions to choose, OD-CPZ can be a useful frequency-selective cross polarization method. Experiments and numerical simulations are shown with the results of the theoretical analysis.

  11. Magic angle spinning NMR study of the ferroelectric transition of KH2PO4: definitive evidence of a displacive component

    NASA Astrophysics Data System (ADS)

    Kweon, Jin Jung; Fu, Riqiang; Choi, Eun Sang; Dalal, Naresh S.

    2017-04-01

    Variable temperature magic angle spinning (MAS) NMR measurements are reported on 1H and 31P nuclei in KH2PO4 (KDP) in the vicinity of its paraelectric-ferroelectric phase transition temperature, T c, of 123 K, to examine the transition mechanism, in particular if this is a model order-disorder type or whether it also involves a displacive component. It has been well established that the temperature variation of the isotropic chemical shift, δ iso, in NMR measurements of the nuclei directly involved in the transition should remain constant or change smoothly through T c for an order-disorder type transition but it should show an anomalous change for a displacive one. Here we demonstrate that the δ iso for both 31P and 1H nuclei in KDP show clear anomalies as a function of temperature around KDP’s T c, providing direct evidence of a displacive component for the phase transition of KDP in contrast to the generally accepted notion that it is a model order-disorder type.

  12. Solid state 31P cross-polarization/magic angle sample spinning nuclear magnetic resonance studies of crystalline glycogen phosphorylase b

    PubMed Central

    Taguchi, Jocelyn E.; Heyes, Stephen J.; Barford, David; Johnson, Louise N.; Dobson, Christopher M.

    1993-01-01

    31P cross-polarization/magic angle sample spinning nuclear magnetic resonance spectra have been obtained for pyridoxal 5′-phosphate (PLP) bound to glycogen phosphorylase b (GPb) in two different crystalline forms, monoclinic and tetragonal. Analysis of the intensities of the spinning sidebands in the nuclear magnetic resonance spectra has enabled estimates of the principal values of the 31P chemical shift tensors to be obtained. Differences between the two sets of values suggest differences in the environment of the phosphate moiety of the pyridoxal phosphate in the two crystalline forms. The tensor for the tetragonal crystalline form, T state GPb, is fully consistent with those found for dianionic phosphate groups in model compounds. The spectrum for the monoclinic crystalline form, R state GPb, although closer to that of dianionic than monoanionic model phosphate compounds, deviates significantly from that expected for a simple dianion or monoanion. This is likely to result from specific interactions between the PLP phosphate group and residues in its binding site in the protein. A possible explanation for the spectrum of the monoclinic crystals is that the shift tensor is averaged by a proton exchange process between different ionization states of the PLP associated with the presence of a sulfate ion bound in the vicinity of the PLP. PMID:8457673

  13. 31P Magic Angle Spinning NMR Spectroscopy of Paramagnetic Rare Earth-Substituted Keggin and Wells-Dawson Solids

    PubMed Central

    Huang, Wenlin; Schopfer, Mark; Zhang, Cheng; Howell, Robertha C.; Todaro, Louis; Gee, Becky A.; Francesconi, Lynn C.; Polenova, Tatyana

    2008-01-01

    Paramagnetic rare-earth elements have been examined as NMR structural probes in polyoxoanionic solids, which have a variety of applications as luminescent materials that are usually disordered and therefore intractable by traditional structural methods. Thirteen Keggin and Wells-Dawson polyoxotungstates containing substitutions with lanthanides of different effective magnetic moments have been examined by 31P magic angle spinning NMR spectroscopy. The electron-nuclear dipolar interaction dominating the spinning sideband envelopes is determined by the lanthanide’s magnetic moment and was found to be a sensitive probe of the nature of the polyoxoanion, of the positional isomerism, and of the ion stoichiometry. Electron-nuclear dipolar anisotropies computed based on the point-dipole approximation are generally in good agreement with the experimental results. The choice of a specific lanthanide as a structural probe can be tailored to the desired distance range between the phosphorus atoms and the paramagnetic centers to be probed. This approach is expected to be particularly useful in the paramagnetic polyoxoanionic materials lacking long-range order. PMID:18095677

  14. Applications of high-resolution magic angle spinning MRS in biomedical studies I-cell line and animal models.

    PubMed

    Kaebisch, Eva; Fuss, Taylor L; Vandergrift, Lindsey A; Toews, Karin; Habbel, Piet; Cheng, Leo L

    2017-06-01

    High-resolution magic angle spinning (HRMAS) MRS allows for direct measurements of non-liquid tissue and cell specimens to present valuable insights into the cellular metabolisms of physiological and pathological processes. HRMAS produces high-resolution spectra comparable to those obtained from solutions of specimen extracts but without complex metabolite extraction processes, and preserves the tissue cellular structure in a form suitable for pathological examinations following spectroscopic analysis. The technique has been applied in a wide variety of biomedical and biochemical studies and become one of the major platforms of metabolomic studies. By quantifying single metabolites, metabolite ratios, or metabolic profiles in their entirety, HRMAS presents promising possibilities for diagnosis and prediction of clinical outcomes for various diseases, as well as deciphering of metabolic changes resulting from drug therapies or xenobiotic interactions. In this review, we evaluate HRMAS MRS results on animal models and cell lines reported in the literature, and present the diverse applications of the method for the understanding of pathological processes and the effectiveness of therapies, development of disease animal models, and new progress in HRMAS methodology. Copyright © 2017 John Wiley & Sons, Ltd.

  15. High-resolution magic angle spinning (1) H NMR measurement of ligand concentration in solvent-saturated chromatographic beads.

    PubMed

    Elwinger, Fredrik; Furó, István

    2016-04-01

    A method based on (1) H high-resolution magic angle spinning NMR has been developed for measuring concentration accurately in heterogeneous materials like that of ligands in chromatography media. Ligand concentration is obtained by relating the peak integrals for a butyl ligand in the spectrum of a water-saturated chromatography medium to the integral of the added internal reference. The method is fast, with capacity of 10 min total sample preparation and analysis time per sample; precise, with a reproducibility expressed as 1.7% relative standard deviation; and accurate, as indicated by the excellent agreement of derived concentration with that obtained previously by (13) C single-pulse excitation MAS NMR. The effects of radiofrequency field inhomogeneity, spin rate, temperature increase due to spinning, and distribution and re-distribution of medium and reference solvent both inside the rotor during spinning and between bulk solvent and pore space are discussed in detail. © 2016 The Authors Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd. © 2016 The Authors Magnetic Resonance in Chemistry published by John Wiley & Sons Ltd.

  16. Combination of high-resolution magic angle spinning proton magnetic resonance spectroscopy and microscale genomics to type brain tumor biopsies.

    PubMed

    Tzika, A Aria; Astrakas, Loukas; Cao, Haihui; Mintzopoulos, Dionyssios; Andronesi, Ovidiu C; Mindrinos, Michael; Zhang, Jiangwen; Rahme, Laurence G; Blekas, Konstantinos D; Likas, Aristidis C; Galatsanos, Nikolas P; Carroll, Rona S; Black, Peter M

    2007-08-01

    Advancements in the diagnosis and prognosis of brain tumor patients, and thus in their survival and quality of life, can be achieved using biomarkers that facilitate improved tumor typing. We introduce and implement a combinatorial metabolic and molecular approach that applies state-of-the-art, high-resolution magic angle spinning (HRMAS) proton (1H) MRS and gene transcriptome profiling to intact brain tumor biopsies, to identify unique biomarker profiles of brain tumors. Our results show that samples as small as 2 mg can be successfully processed, the HRMAS 1H MRS procedure does not result in mRNA degradation, and minute mRNA amounts yield high-quality genomic data. The MRS and genomic analyses demonstrate that CNS tumors have altered levels of specific 1H MRS metabolites that directly correspond to altered expression of Kennedy pathway genes; and exhibit rapid phospholipid turnover, which coincides with upregulation of cell proliferation genes. The data also suggest Sonic Hedgehog pathway (SHH) dysregulation may play a role in anaplastic ganglioglioma pathogenesis. That a strong correlation is seen between the HRMAS 1H MRS and genomic data cross-validates and further demonstrates the biological relevance of the MRS results. Our combined metabolic/molecular MRS/genomic approach provides insights into the biology of anaplastic ganglioglioma and a new potential tumor typing methodology that could aid neurologists and neurosurgeons to improve the diagnosis, treatment, and ongoing evaluation of brain tumor patients.

  17. Discrimination of Basal Cell Carcinoma from Normal Skin Tissue Using High-Resolution Magic Angle Spinning 1H NMR Spectroscopy.

    PubMed

    Mun, Je-Ho; Lee, Heonho; Yoon, Dahye; Kim, Byung-Soo; Kim, Moon-Bum; Kim, Shukmann

    2016-01-01

    High-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR) spectroscopy is a useful tool for investigating the metabolism of various cancers. Basal cell carcinoma (BCC) is the most common skin cancer. However, to our knowledge, data on metabolic profiling of BCC have not been reported in the literature. The objective of the present study was to investigate the metabolic profiling of cutaneous BCC using HR-MAS (1)H NMR spectroscopy. HR-MAS (1)H NMR spectroscopy was used to analyze the metabolite profile and metabolite intensity of histopathologically confirmed BCC tissues and normal skin tissue (NST) samples. The metabolic intensity normalized to the total spectral intensities in BCC and NST was compared, and multivariate analysis was performed with orthogonal partial least-squares discriminant analysis (OPLS-DA). P values < 0.05 were considered statistically significant. Univariate analysis revealed 9 metabolites that showed statistically significant difference between BCC and NST. In multivariate analysis, the OPLS-DA models built with the HR-MAS NMR metabolic profiles revealed a clear separation of BCC from NST. The receiver operating characteristic curve generated from the results revealed an excellent discrimination of BCC from NST with an area under the curve (AUC) value of 0.961. The present study demonstrated that the metabolite profile and metabolite intensity differ between BCC and NST, and that HR-MAS (1)H NMR spectroscopy can be a valuable tool in the diagnosis of BCC.

  18. Discrimination of Basal Cell Carcinoma from Normal Skin Tissue Using High-Resolution Magic Angle Spinning 1H NMR Spectroscopy

    PubMed Central

    Mun, Je-Ho; Lee, Heonho; Yoon, Dahye; Kim, Byung-Soo; Kim, Moon-Bum; Kim, Shukmann

    2016-01-01

    High-resolution magic angle spinning nuclear magnetic resonance (HR-MAS NMR) spectroscopy is a useful tool for investigating the metabolism of various cancers. Basal cell carcinoma (BCC) is the most common skin cancer. However, to our knowledge, data on metabolic profiling of BCC have not been reported in the literature. The objective of the present study was to investigate the metabolic profiling of cutaneous BCC using HR-MAS 1H NMR spectroscopy. HR-MAS 1H NMR spectroscopy was used to analyze the metabolite profile and metabolite intensity of histopathologically confirmed BCC tissues and normal skin tissue (NST) samples. The metabolic intensity normalized to the total spectral intensities in BCC and NST was compared, and multivariate analysis was performed with orthogonal partial least-squares discriminant analysis (OPLS-DA). P values < 0.05 were considered statistically significant. Univariate analysis revealed 9 metabolites that showed statistically significant difference between BCC and NST. In multivariate analysis, the OPLS-DA models built with the HR-MAS NMR metabolic profiles revealed a clear separation of BCC from NST. The receiver operating characteristic curve generated from the results revealed an excellent discrimination of BCC from NST with an area under the curve (AUC) value of 0.961. The present study demonstrated that the metabolite profile and metabolite intensity differ between BCC and NST, and that HR-MAS 1H NMR spectroscopy can be a valuable tool in the diagnosis of BCC. PMID:26934749

  19. Evaluation of Cancer Metabolomics Using ex vivo High Resolution Magic Angle Spinning (HRMAS) Magnetic Resonance Spectroscopy (MRS).

    PubMed

    Fuss, Taylor L; Cheng, Leo L

    2016-03-22

    According to World Health Organization (WHO) estimates, cancer is responsible for more deaths than all coronary heart disease or stroke worldwide, serving as a major public health threat around the world. High resolution magic angle spinning (HRMAS) magnetic resonance spectroscopy (MRS) has demonstrated its usefulness in the identification of cancer metabolic markers with the potential to improve diagnosis and prognosis for the oncology clinic, due partially to its ability to preserve tissue architecture for subsequent histological and molecular pathology analysis. Capable of the quantification of individual metabolites, ratios of metabolites, and entire metabolomic profiles, HRMAS MRS is one of the major techniques now used in cancer metabolomic research. This article reviews and discusses literature reports of HRMAS MRS studies of cancer metabolomics published between 2010 and 2015 according to anatomical origins, including brain, breast, prostate, lung, gastrointestinal, and neuroendocrine cancers. These studies focused on improving diagnosis and understanding patient prognostication, monitoring treatment effects, as well as correlating with the use of in vivo MRS in cancer clinics.

  20. Structural Analysis of Human Cofilin 2/Filamentous Actin Assemblies: Atomic-Resolution Insights from Magic Angle Spinning NMR Spectroscopy

    PubMed Central

    Yehl, Jenna; Kudryashova, Elena; Reisler, Emil; Kudryashov, Dmitri; Polenova, Tatyana

    2017-01-01

    Cellular actin dynamics is an essential element of numerous cellular processes, such as cell motility, cell division and endocytosis. Actin’s involvement in these processes is mediated by many actin-binding proteins, among which the cofilin family plays unique and essential role in accelerating actin treadmilling in filamentous actin (F-actin) in a nucleotide-state dependent manner. Cofilin preferentially interacts with older filaments by recognizing time-dependent changes in F-actin structure associated with the hydrolysis of ATP and release of inorganic phosphate (Pi) from the nucleotide cleft of actin. The structure of cofilin on F-actin and the details of the intermolecular interface remain poorly understood at atomic resolution. Here we report atomic-level characterization by magic angle spinning (MAS) NMR of the muscle isoform of human cofilin 2 (CFL2) bound to F-actin. We demonstrate that resonance assignments for the majority of atoms are readily accomplished and we derive the intermolecular interface between CFL2 and F-actin. The MAS NMR approach reported here establishes the foundation for atomic-resolution characterization of a broad range of actin-associated proteins bound to F-actin. PMID:28303963

  1. Metabolomics approach to thyroid nodules: a high-resolution magic-angle spinning nuclear magnetic resonance-based study.

    PubMed

    Miccoli, Paolo; Torregrossa, Liborio; Shintu, Laetitia; Magalhaes, Alviclér; Chandran, JimaNambiath; Tintaru, Aura; Ugolini, Clara; Minuto, Michele N; Miccoli, Mario; Basolo, Fulvio; Caldarelli, Stefano

    2012-12-01

    Proton magnetic resonance spectroscopy of operative specimens has been reported to successfully differentiate normal tissue from malignant thyroid tissue. We used a new high-resolution magnetic resonance spectroscopy technique for the differentiation of benign and malignant thyroid neoplasms. Histological specimens from 72 patients undergoing a total thyroidectomy were processed into a 4-mm ZrO(2) high-resolution magic angle spinning (HRMAS) rotor with 5 μL of D(2)O. A Bruker Avance spectrometer operating at 400 MHz for the (1)H frequency and equipped with a (1)H/(13)C/(31)P HRMAS probe was used. Normal and neoplastic thyroid tissues could be discriminated from each other by different relative concentrations of several amino acids and lipids, as well as benign and malignant neoplasms, that differed in terms of a greater lactate and taurine and a lesser lipid choline, phosphocholine, myo-inositol, and scyllo-inositol levels in malignant samples. A statistical analysis with a receiver operating characteristic curve revealed that 77% of the samples were accurately predicted. Similar results were obtained with specimens obtained from ex vivo aspirates. A further development of this project will be to use the metabolomics approach on specimens obtained from aspirates in vivo after the resolution of technical problems attributable to possible contamination. Copyright © 2012 Mosby, Inc. All rights reserved.

  2. Deuterium Magic Angle Spinning NMR Used to Study the Dynamics of Peptides Adsorbed onto Polystyrene and Functionalized Polystyrene Surfaces

    PubMed Central

    Breen, Nicholas F.; Li, Kun; Olsen, Gregory L.; Drobny, Gary P.

    2011-01-01

    LKα14 is a 14 amino acid peptide with a periodic sequence of leucine and lysine residues consistent with an amphipathic α-helix. This “hydrophobic periodicity” has been found to result in an α-helical secondary structure at air-water interfaces and on both polar and non-polar solid polymer surfaces. In this paper the dynamics of LKα14 peptides, selectively deuterated at a single leucine and adsorbed onto polystyrene and carboxylated polystyrene beads, are studied using 2H Magic Angle Spinning (MAS) solid state NMR over a 100 degree temperature range. We first demonstrate the sensitivity enhancement possible with 2H MAS techniques, which in turn enables us to obtain high quality 2H NMR spectra for selectively deuterated peptides adsorbed onto solid polymer surfaces. An extensive literature shows that the dynamics of leucine side chains are sensitive to the local structural environment of the protein. Therefore the degree to which the dynamics of leucine side chains and the backbone of the peptide LKα14 are influenced by surface proximity and surface chemistry is studied as a function of temperature with 2H MAS NMR. It is found that the dynamics of the leucine side chains in LKα14 depend strongly upon the orientation of the polymer on the surface, which in turn depends on whether the LKα14 peptide adsorbs onto a polar or non-polar surface. 2H MAS line shapes therefore permit probes of surface orientation over a wide temperature range. PMID:21650191

  3. Variable temperature system using vortex tube cooling and fiber optic temperature measurement for low temperature magic angle spinning NMR

    NASA Astrophysics Data System (ADS)

    Martin, Rachel W.; Zilm, Kurt W.

    2004-06-01

    We describe the construction and operation of a variable temperature (VT) system for a high field fast magic angle spinning (MAS) probe. The probe is used in NMR investigations of biological macromolecules, where stable setting and continuous measurement of the temperature over periods of several days are required in order to prevent sample overheating and degradation. The VT system described is used at and below room temperature. A vortex tube is used to provide cooling in the temperature range of -20 to 20 °C, while a liquid nitrogen-cooled heat exchanger is used below -20 °C. Using this arrangement, the lowest temperature that is practically achievable is -140 °C. Measurement of the air temperature near the spinning rotor is accomplished using a fiber optic thermometer that utilizes the temperature dependence of the absorption edge of GaAs. The absorption edge of GaAs also has a magnetic field dependence that we have measured and corrected for. This dependence was calibrated at several field strengths using the well-known temperature dependence of the 1H chemical shift difference of the protons in methanol.

  4. Variable temperature system using vortex tube cooling and fiber optic temperature measurement for low temperature magic angle spinning NMR.

    PubMed

    Martin, Rachel W; Zilm, Kurt W

    2004-06-01

    We describe the construction and operation of a variable temperature (VT) system for a high field fast magic angle spinning (MAS) probe. The probe is used in NMR investigations of biological macromolecules, where stable setting and continuous measurement of the temperature over periods of several days are required in order to prevent sample overheating and degradation. The VT system described is used at and below room temperature. A vortex tube is used to provide cooling in the temperature range of -20 to 20 degrees C, while a liquid nitrogen-cooled heat exchanger is used below -20 degrees C. Using this arrangement, the lowest temperature that is practically achievable is -140 degrees C. Measurement of the air temperature near the spinning rotor is accomplished using a fiber optic thermometer that utilizes the temperature dependence of the absorption edge of GaAs. The absorption edge of GaAs also has a magnetic field dependence that we have measured and corrected for. This dependence was calibrated at several field strengths using the well-known temperature dependence of the (1)H chemical shift difference of the protons in methanol.

  5. Gelified Biofluids for High-Resolution Magic Angle Spinning (1)H NMR Analysis: The Case of Urine.

    PubMed

    Takis, Panteleimon G; Tenori, Leonardo; Ravera, Enrico; Luchinat, Claudio

    2017-01-17

    In this letter, we propose an alternative, effective protocol for metabolomic characterization of biofluids based on their gelification and subsequent application of high-resolution magic angle spinning (HRMAS) (1)H nuclear magnetic resonance (NMR). The sample handling is very rapid and reproducible, and much less than 40 μL of neat urine are needed to obtain a sample. Our results indicate that the HRMAS spectra of gelified urine encompass all metabolites in the NMR fingerprint, as observed by solution NMR. The proposed approach can be efficiently integrated into the NMR based metabolomics analyses routines: multivariate statistical analysis of both solution and HRMAS data produced very similar statistical models, with high classification accuracy. One of the key advantages offered by the gelification approach is the improved short-term (up to 24 h) preservation of nonfrozen HRMAS NMR gel urine samples compared to the solution samples, which could lead to an alternative way for transportation or domestic collection of biofluids, without the need of cold-storage and reducing the risks of leakage.

  6. Deuterium magic angle spinning NMR used to study the dynamics of peptides adsorbed onto polystyrene and functionalized polystyrene surfaces.

    PubMed

    Breen, Nicholas F; Li, Kun; Olsen, Gregory L; Drobny, Gary P

    2011-08-04

    LKα14 is a 14 amino acid peptide with a periodic sequence of leucine and lysine residues consistent with an amphipathic α-helix. This "hydrophobic periodicity" has been found to result in an α-helical secondary structure at air-water interfaces and on both polar and nonpolar solid polymer surfaces. In this paper, the dynamics of LKα14 peptides, selectively deuterated at a single leucine and adsorbed onto polystyrene and carboxylated polystyrene beads, are studied using (2)H magic angle spinning (MAS) solid state NMR over a 100 °C temperature range. We first demonstrate the sensitivity enhancement possible with (2)H MAS techniques, which in turn enables us to obtain high-quality (2)H NMR spectra for selectively deuterated peptides adsorbed onto solid polymer surfaces. The extensive literature shows that the dynamics of leucine side chains are sensitive to the local structural environment of the protein. Therefore, the degree to which the dynamics of leucine side chains and the backbone of the peptide LKα14 are influenced by surface proximity and surface chemistry is studied as a function of temperature with (2)H MAS NMR. It is found that the dynamics of the leucine side chains in LKα14 depend strongly upon the orientation of the polymer on the surface, which in turn depends on whether the LKα14 peptide adsorbs onto a polar or nonpolar surface. (2)H MAS line shapes therefore permit probes of surface orientation over a wide temperature range.

  7. Is a magic angle effect observed in the collateral ligaments of the distal interphalangeal joint or the oblique sesamoidean ligaments during standing magnetic resonance imaging?

    PubMed

    Smith, Meredith A; Dyson, Sue J; Murray, Rachel C

    2008-01-01

    Collagen fibers oriented at 55 degrees to the static magnetic field (B0) are characterized by an artifactual increase in signal intensity due to the magic angle effect. We hypothesized that there would be increased signal intensity in the collateral ligaments of the distal interphalangeal joint and oblique sesamoidean ligaments when these ligaments were at angles approaching 55 degrees to a horizontal B0 during standing magnetic resonance (MR) imaging. MR imaging was performed on four cadaver forelimbs in a 0.27 T standing system. Transverse and dorsal images were obtained using various sequences, with limbs angled at 0 degrees, 4 degrees, 8 degrees, and 12 degrees to the vertical. Images were analyzed and the angle of each ligament to B0 determined. Mean signal intensity in the ligament and cortex of the adjacent phalanx was measured and ratios calculated. With subjective interpretation, there was increased signal intensity in the collateral ligaments of the distal interphalangeal joint and oblique sesamoidean ligaments over ranges of angles of 60-78 degrees and 57-69 degrees, respectively, to B0. In fast spin echo (FSE) sequences, with a long echo time (72ms), the effect was less pronounced. FSE sequences can help determine the significance of increased signal intensity within tissues. In spite of limited positions of a limb during standing MR imaging compared with horses under general anesthesia, deviation from a vertical posture sufficient to cause a magic angle effect can still occur in both ligaments tested. Conformation may contribute to the occurrence of the magic angle effect during standing MR imaging. Effort should be made to position horses squarely and to minimize leaning during image acquisition.

  8. Structure determination of aligned systems by solid-state NMR magic angle spinning methods.

    PubMed

    Gross, Benjamin J; Tanski, Joseph M; McDermott, Ann E

    2005-10-01

    Single crystal rotational echo double resonance (REDOR) experiments can be used to determine the three-dimensional orientation of heteronuclear bond vectors in an amino acid, as well as the crystal's orientation relative to the rotor fixed frame (RFF). We also demonstrate that for samples uniaxially aligned along the rotor axis, the polar tilt angle of a bond vector relative to the RFF can be measured by use of an analytical expression that describes the REDOR curve for that system. These bond orientations were verified by X-ray indexing of the single crystal sample, and were shown to be as accurate as +/- 1 degrees .

  9. Structure determination of aligned systems by solid-state NMR magic angle spinning methods

    NASA Astrophysics Data System (ADS)

    Gross, Benjamin J.; Tanski, Joseph M.; McDermott, Ann E.

    2005-10-01

    Single crystal rotational echo double resonance (REDOR) experiments can be used to determine the three-dimensional orientation of heteronuclear bond vectors in an amino acid, as well as the crystal's orientation relative to the rotor fixed frame (RFF). We also demonstrate that for samples uniaxially aligned along the rotor axis, the polar tilt angle of a bond vector relative to the RFF can be measured by use of an analytical expression that describes the REDOR curve for that system. These bond orientations were verified by X-ray indexing of the single crystal sample, and were shown to be as accurate as ±1°.

  10. Investigation of regional influence of magic-angle effect on t2 in human articular cartilage with osteoarthritis at 3 T.

    PubMed

    Wang, Ligong; Regatte, Ravinder R

    2015-01-01

    The objectives of this research study were to determine the magic-angle effect on different subregions of in vivo human femoral cartilage through the quantitative assessment of the effect of static magnetic field orientation (B0) on transverse (T2) relaxation time at 3.0 T. Healthy volunteers (n = 5; mean age, 36.4 years) and clinical patients (n = 5; mean age, 64 years) with early osteoarthritis (OA) were scanned at 3.0-T magnetic resonance using an 8-channel phased-array knee coil (transmit-receive). The T2 maps revealed significantly greater values in anterior than in posterior regions. When the cartilage regions were oriented at 55° to B0 (magic angle), the longest T2 values were detected in comparison with the neighboring regions oriented 90° and 180° (0°) to B0. The subregions oriented 180° (0°) to B0 showed the lowest T2 values. The differences in T2 values of different subregions suggest that magic-angle effect needs to be considered when interpreting cartilage abnormalities in OA patients. Copyright © 2015 AUR. Published by Elsevier Inc. All rights reserved.

  11. Magic angle effect in normal collateral ligaments of the distal interphalangeal joint in horses imaged with a high-field magnetic resonance imaging system.

    PubMed

    Werpy, Natasha M; Ho, Charles P; Kawcak, Christopher E

    2010-01-01

    Distal forelimb specimens of eight skeletally mature horses were imaged using proton density turbo spin echo, T1-weighted spoiled gradient echo, T2*-weighted gradient echo, short tau inversion recovery and T2-weighted fast spin echo sequences with the limb parallel to the main magnetic field, and with angulation of the limb relative to the main magnetic field. The magic angle effect can be identified in the collateral ligaments of the distal interphalangeal joint when imaged in a high-field magnetic resonance (MR) imaging system with a horizontally oriented main magnetic field. This effect has previously been described in the collateral ligaments of the distal interphalangeal joint in a low-field system with a vertically oriented main magnetic field. The curvature of the ligaments places the fibers at the magic angle in both horizontally and vertically orientated main magnetic fields. This effect can be identified on short time of echo sequences and impacts the signal pattern of the ligaments at the level of the middle phalanx with the limb in a neutral position and with angulation of the limb. Magic angle effect should be considered as a possible cause of an asymmetrical signal pattern, depending on the positioning of the limb and the sequences used for imaging, when evaluating the collateral ligaments of the distal interphalangeal joint on images acquired with a high-field MR imaging system that has a horizontally oriented main magnetic field.

  12. Investigation of Regional Influence of Magic-Angle Effect on T2 in Human Articular Cartilage with Osteoarthritis at 3 T

    PubMed Central

    Wang, Ligong; Regatte, Ravinder R.

    2014-01-01

    Rationale and Objectives The objectives of this research study were to determine the magic-angle effect on different subregions of in vivo human femoral cartilage through the quantitative assessment of the effect of static magnetic field orientation (B0) on transverse (T2) relaxation time at 3.0 T. Materials and Methods Healthy volunteers (n = 5l; mean age, 36.4 years) and clinical patients (n = 5; mean age, 64 years) with early osteoarthritis (OA) were scanned at 3.0-T magnetic resonance using an 8-channel phased-array knee coil (transmit-receive). Results The T2 maps revealed significantly greater values in ventral than in dorsal regions. When the cartilage regions were oriented at 55° to B0 (magic angle), the longest T2 values were detected in comparison with the neighboring regions oriented 90° and 180° (0°) to B0. The subregions oriented 180° (0°) to B0 showed the lowest T2 values. Conclusions The differences in T2 values of different subregions suggest that magic-angle effect needs to be considered when interpreting cartilage abnormalities in OA patients. PMID:25481517

  13. Non-destructive microstructural analysis with depth resolution

    NASA Astrophysics Data System (ADS)

    Zolotoyabko, E.; Quintana, J. P.

    2003-01-01

    A depth-sensitive X-ray diffraction technique has been developed with the aim of studying microstructural modifications in inhomogeneous polycrystalline materials. In that method, diffraction profiles are measured at different X-ray energies varied by small steps. X-rays at higher energies probe deeper layers of material. Depth-resolved structural information is retrieved by comparing energy-dependent diffraction profiles. The method provides non-destructive depth profiling of the preferred orientation, grain size, microstrain fluctuations and residual strains. This technique is applied to the characterization of seashells. Similarly, energy-variable X-ray diffraction can be used for the non-destructive characterization of different laminated structures and composite materials.

  14. Non-destructive examination system of vitreous body

    NASA Astrophysics Data System (ADS)

    Shibata, Takuma; Gong, Jin; Watanabe, Yosuke; Kabir, M. Hasnat; Masato, Makino; Furukawa, Hidemitsu; Nishitsuka, Koichi

    2014-04-01

    Eyeball plays a quite important role in acquiring the vision. Vitreous body occupies the largest part of the eyeball and consists of biological, elastic, transparent, gel materials. In the present medical examination, the non-destructive examination method of the vitreous body has not been well established. Here, we focus on an application of dynamic light scattering to this topic. We tried to apply our lab-made apparatus, scanning microscopic light scattering (SMILS), which was specially designed for observing the nanometer-scale network structure in gel materials. In order to examine the vitreous body using SMILS method, a commercial apparatus, nano Partica (Horiba Co. Ltd.) was also customized. We analyzed vitreous body using both the SMILS and the customized nano Partica. We successfully examined the vitreous bodies of healthy pigs in non-destructive way.

  15. Infrared Thermography for Temperature Measurement and Non-Destructive Testing

    PubMed Central

    Usamentiaga, Rubèn; Venegas, Pablo; Guerediaga, Jon; Vega, Laura; Molleda, Julio; Bulnes, Francisco G.

    2014-01-01

    The intensity of the infrared radiation emitted by objects is mainly a function of their temperature. In infrared thermography, this feature is used for multiple purposes: as a health indicator in medical applications, as a sign of malfunction in mechanical and electrical maintenance or as an indicator of heat loss in buildings. This paper presents a review of infrared thermography especially focused on two applications: temperature measurement and non-destructive testing, two of the main fields where infrared thermography-based sensors are used. A general introduction to infrared thermography and the common procedures for temperature measurement and non-destructive testing are presented. Furthermore, developments in these fields and recent advances are reviewed. PMID:25014096

  16. Infrared thermography for temperature measurement and non-destructive testing.

    PubMed

    Usamentiaga, Rubén; Venegas, Pablo; Guerediaga, Jon; Vega, Laura; Molleda, Julio; Bulnes, Francisco G

    2014-07-10

    The intensity of the infrared radiation emitted by objects is mainly a function of their temperature. In infrared thermography, this feature is used for multiple purposes: as a health indicator in medical applications, as a sign of malfunction in mechanical and electrical maintenance or as an indicator of heat loss in buildings. This paper presents a review of infrared thermography especially focused on two applications: temperature measurement and non-destructive testing, two of the main fields where infrared thermography-based sensors are used. A general introduction to infrared thermography and the common procedures for temperature measurement and non-destructive testing are presented. Furthermore, developments in these fields and recent advances are reviewed.

  17. Non-destructive NIR FT Raman analysis of plants

    NASA Astrophysics Data System (ADS)

    Schrader, B.; Klump, H. H.; Schenzel, K.; Schulz, H.

    1999-10-01

    Non-destructive analyses of animal and plant cells and tissues by 'classical' Raman spectroscopy with excitation in the visible range have not been possible since the samples are destroyed photochemically or their fluorescence conceals the Raman spectra completely. When excited with the Nd:YAG laser line at 1064 nm fluorescence-free Raman spectra of animal or plant cells and tissues can be recorded without special preparation. In this paper we concentrate on plants and its constituents: essential oils, natural dyes, flavors, spices, alkaloids and fibers can be characterized. The spectra allow the observation of biochemical processes, to observe the distribution of natural products, application to taxonomy, optimizing plant breeding, the harvesting time and control of food—everything non-destructively in living plants!

  18. Non-destructive techniques based on eddy current testing.

    PubMed

    García-Martín, Javier; Gómez-Gil, Jaime; Vázquez-Sánchez, Ernesto

    2011-01-01

    Non-destructive techniques are used widely in the metal industry in order to control the quality of materials. Eddy current testing is one of the most extensively used non-destructive techniques for inspecting electrically conductive materials at very high speeds that does not require any contact between the test piece and the sensor. This paper includes an overview of the fundamentals and main variables of eddy current testing. It also describes the state-of-the-art sensors and modern techniques such as multi-frequency and pulsed systems. Recent advances in complex models towards solving crack-sensor interaction, developments in instrumentation due to advances in electronic devices, and the evolution of data processing suggest that eddy current testing systems will be increasingly used in the future.

  19. Non-Destructive Techniques Based on Eddy Current Testing

    PubMed Central

    García-Martín, Javier; Gómez-Gil, Jaime; Vázquez-Sánchez, Ernesto

    2011-01-01

    Non-destructive techniques are used widely in the metal industry in order to control the quality of materials. Eddy current testing is one of the most extensively used non-destructive techniques for inspecting electrically conductive materials at very high speeds that does not require any contact between the test piece and the sensor. This paper includes an overview of the fundamentals and main variables of eddy current testing. It also describes the state-of-the-art sensors and modern techniques such as multi-frequency and pulsed systems. Recent advances in complex models towards solving crack-sensor interaction, developments in instrumentation due to advances in electronic devices, and the evolution of data processing suggest that eddy current testing systems will be increasingly used in the future. PMID:22163754

  20. A non-destructive DNA sampling technique for herbarium specimens.

    PubMed

    Shepherd, Lara D

    2017-01-01

    Herbarium specimens are an important source of DNA for plant research but current sampling methods require the removal of material for DNA extraction. This is undesirable for irreplaceable specimens such as rare species or type material. Here I present the first non-destructive sampling method for extracting DNA from herbarium specimens. DNA was successfully retrieved from robust leaves and/or stems of herbarium specimens up to 73 years old.

  1. Embedded Non-Destructive Evaluation for Glass Armor

    DTIC Science & Technology

    2011-12-05

    Unclassified In House NDE and Electromagnetic Compatibility Capabilities Millimeter wave Scanning Imager Phased Array Ultrasound Immersion Tank Low...DISTRIBUTION A: Approved for public release; distribution is unlimited Embedded NDE for Glass Armor Sensor Enhanced Armor- Non-Destructive...Standard Form 298 (Rev. 8-98) Prescribed by ANSI Std Z39-18 Unclassified Armor Solutions Tested with Ultrasonics NDT/E leading to Sensor Enhanced

  2. Non-Destructive Testing for Control of Radioactive Waste Package

    NASA Astrophysics Data System (ADS)

    Plumeri, S.; Carrel, F.

    2015-10-01

    Characterization and control of radioactive waste packages are important issues in the management of a radioactive waste repository. Therefore, Andra performs quality control inspection on radwaste package before disposal to ensure the compliance of the radwast characteristics with Andra waste disposal specifications and to check the consistency between Andra measurements results and producer declared properties. Objectives of this quality control are: assessment and improvement of producer radwaste packages quality mastery, guarantee of the radwaste disposal safety, maintain of the public confidence. To control radiological characteristics of radwaste package, non-destructive passive methods (gamma spectrometry and neutrons counting) are commonly used. These passive methods may not be sufficient, for instance to control the mass of fissile material contained inside radwaste package. This is particularly true for large concrete hull of heterogeneous radwaste containing several actinides mixed with fission products like 137Cs. Non-destructive active methods, like measurement of photofission delayed neutrons, allow to quantify the global mass of actinides and is a promising method to quantify mass of fissile material. Andra has performed different non-destructive measurements on concrete intermediate-level short lived nuclear waste (ILW-SL) package to control its nuclear material content. These tests have allowed Andra to have a first evaluation of the performance of photofission delayed neutron measurement and to identify development needed to have a reliable method, especially for fissile material mass control in intermediate-level long lived waste package.

  3. Powder-XRD and (14) N magic angle-spinning solid-state NMR spectroscopy of some metal nitrides.

    PubMed

    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.

  4. Intratumoral Agreement of High-Resolution Magic Angle Spinning Magnetic Resonance Spectroscopic Profiles in the Metabolic Characterization of Breast Cancer

    PubMed Central

    Park, Vivian Youngjean; Yoon, Dahye; Koo, Ja Seung; Kim, Eun-Kyung; Kim, Seung Il; Choi, Ji Soo; Park, Seho; Park, Hyung Seok; Kim, Suhkmann; Kim, Min Jung

    2016-01-01

    Abstract High-resolution magic angle spinning (HR-MAS) magnetic resonance (MR) spectroscopy data may serve as a biomarker for breast cancer, with only a small volume of tissue sample required for assessment. However, previous studies utilized only a single tissue sample from each patient. The aim of this study was to investigate whether intratumoral location and biospecimen type affected the metabolic characterization of breast cancer assessed by HR-MAS MR spectroscopy This prospective study was approved by the institutional review board and informed consent was obtained. Preoperative core-needle biopsies (CNBs), central, and peripheral surgical tumor specimens were prospectively collected under ultrasound (US) guidance in 31 patients with invasive breast cancer. Specimens were assessed with HR-MAS MR spectroscopy. The reliability of metabolite concentrations was evaluated and multivariate analysis was performed according to intratumoral location and biospecimen type. There was a moderate or higher agreement between the relative concentrations of 94.3% (33 of 35) of metabolites in the center and periphery, 80.0% (28 of 35) of metabolites in the CNB and central surgical specimens, and 82.9% (29 of 35) of metabolites between all 3 specimen types. However, there was no significant agreement between the concentrations of phosphocholine (PC) and phosphoethanolamine (PE) in the center and periphery. The concentrations of several metabolites (adipate, arginine, fumarate, glutamate, PC, and PE) had no significant agreement between the CNB and central surgical specimens. In conclusion, most HR-MAS MR spectroscopic data do not differ based on intratumoral location or biospecimen type. However, some metabolites may be affected by specimen-related variables, and caution is recommended in decision-making based solely on metabolite concentrations, particularly PC and PE. Further validation through future studies is needed for the clinical implementation of these biomarkers based

  5. Surface Interactions and Confinement of Methane: A High Pressure Magic Angle Spinning NMR and Computational Chemistry Study

    DOE PAGES

    Ok, Salim; Hoyt, David W.; Andersen, Amity; ...

    2017-01-18

    Characterization and modeling of the molecular-level behavior of simple hydrocarbon gases, such as methane, in the presence of both nonporous and nanoporous mineral matrices allows for predictive understanding of important processes in engineered and natural systems. In this study, we observed changes in local electromagnetic environments of the carbon atoms in methane under conditions of high pressure (up to 130 bar) and moderate temperature (up to 346 K) with 13C magic-angle spinning (MAS) NMR spectroscopy while the methane gas was mixed with two model solid substrates: a fumed nonporous, 12 nm particle size silica and a mesoporous silica with 200more » nm particle size and 4 nm average pore diameter. Examination of the interactions between methane and the silica systems over temperatures and pressures that include the supercritical regime was allowed by a novel high pressure MAS sample containment system, which provided high resolution spectra collected under in situ conditions. There was no significant thermal effects were found for the observed 13C chemical shifts at all pressures studied here (28.2, 32.6, 56.4, 65.1, 112.7, and 130.3 bar) for pure methane. However, the 13C chemical shifts of resonances arising from confined methane changed slightly with changes in temperature in mixtures with mesoporous silica. The chemical shift values of 13C nuclides in methane change measurably as a function of pressure both in the pure state and in mixtures with both silica matrices, with a more pronounced shift when meso-porous silica is present. Molecular-level simulations utilizing GCMC, MD, and DFT confirm qualitatively that the experimentally measured changes are attributed to interactions of methane with the hydroxylated silica surfaces as well as densification of methane within nanopores and on pore surfaces.« less

  6. Design of a triple resonance magic angle sample spinning probe for high field solid state nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Martin, Rachel W.; Paulson, Eric K.; Zilm, Kurt W.

    2003-06-01

    Standard design and construction practices used in building nuclear magnetic resonance (NMR) probes for the study of solid state samples become difficult if not entirely impractical to implement as the 1H resonance frequency approaches the self resonance frequency of commercial capacitors. We describe an approach that utilizes short variable transmission line segments as tunable reactances. Such an approach effectively controls stray reactances and provides a higher Q alternative to ceramic chip capacitors. The particular probe described is built to accommodate a 2.5 mm magic angle spinning rotor system, and is triply tuned to 13C, 15N, and 1H frequencies for use at 18.8 T (200, 80, and 800 MHz, respectively). Isolation of the three radio frequency (rf) channels is achieved using both a rejection trap and a transmission line notch filter. The compact geometry of this design allows three channels with high power handling capability to fit in a medium bore (63 mm) magnet. Extended time variable temperature operation is integral to the mechanical design, enabling the temperature control necessary for investigation of biological macromolecules. Accurate measurement of the air temperature near the sample rotor is achieved using a fiber optic thermometer, which does not interfere with the rf electronics. We also demonstrate that acceptable line shapes are only readily achieved using zero magnetic susceptibility wire in construction of the sample coil. Computer simulation of the circuit aided in the physical design of the probe. Representative data illustrating the efficiency, rf homogeneity, and signal to noise factor of the probe are presented.

  7. Distortional binding of transition state analogs to human purine nucleoside phosphorylase probed by magic angle spinning solid-state NMR

    PubMed Central

    Vetticatt, Mathew J.; Itin, Boris; Evans, Gary B.; Schramm, Vern L.

    2013-01-01

    Transition state analogs mimic the geometry and electronics of the transition state of enzymatic reactions. These molecules bind to the active site of the enzyme much tighter than substrate and are powerful noncovalent inhibitors. Immucillin-H (ImmH) and 4′-deaza-1′-aza-2′-deoxy-9-methylene Immucillin-H (DADMe-ImmH) are picomolar inhibitors of human purine nucleoside phosphorylase (hPNP). Although both molecules are electronically similar to the oxocarbenium-like dissociative hPNP transition state, DADMe-ImmH is more potent than ImmH. DADMe-ImmH captures more of the transition state binding energy by virtue of being a closer geometric match to the hPNP transition state than ImmH. A consequence of these similarities is that the active site of hPNP exerts greater distortional forces on ImmH than on DADMe-ImmH to “achieve” the hPNP transition state geometry. By using magic angle spinning solid-state NMR to investigate stable isotope-labeled ImmH and DADMe-ImmH, we have explored the difference in distortional binding of these two inhibitors to hPNP. High-precision determinations of internuclear distances from NMR recoupling techniques, rotational echo double resonance, and rotational resonance, have provided unprecedented atomistic insight into the geometric changes that occur upon binding of transition state analogs. We conclude that hPNP stabilizes conformations of these chemically distinct analogs having distances between the cation and leaving groups resembling those of the known transition state. PMID:24043827

  8. Lipid biomarkers of glioma cell growth arrest and cell death detected by 1 H magic angle spinning MRS.

    PubMed

    Mirbahai, Ladan; Wilson, Martin; Shaw, Christopher S; McConville, Carmel; Malcomson, Roger D G; Kauppinen, Risto A; Peet, Andrew C

    2012-11-01

    Biomarkers of early response to treatment have the potential to improve cancer therapy by allowing treatment to be tailored to the individual. Alterations in lipids detected by in vivo MRS have been suggested as noninvasive biomarkers of cell stress and early indicators of cell death. An improved understanding of the relationship between MRS lipids and cell stress in vitro would aid in the translation of this technique into clinical use. Rat BT4C glioma cells were treated with 50 µ m cis-dichlorodiammineplatinum II (cisplatin), a commonly used chemotherapeutic agent, and harvested at several time points up to 72 h. High-resolution magic angle spinning (1) H MRS of cells was then performed on a 600-MHz NMR spectrometer. The metabolites were quantified using a time domain fitting method, TARQUIN. Increases were detected in saturated and polyunsaturated fatty acid resonances early during the exposure to cisplatin. The fatty acid CH(2) /CH(3) ratio was unaltered by treatment after allowing for contributions of macromolecules. Polyunsaturated fatty acids increased on treatment, with the group -CH=CH-CH(2) -CH=CH- accounting for all the unsaturated fatty acid signals. Transmission electron microscopy, in addition to Nile red and 4',6-diamino-2-phenylindole co-staining, revealed that the lipid increase was associated with cytoplasmic neutral lipid droplets. Small numbers of apoptotic and necrotic cells were detected by trypan blue, annexin V-fluorescein isothiocyanate-labelled flow cytometry and DNA laddering after up to 48 h of cisplatin exposure. Propidium iodide flow cytometry revealed that cells accumulated in the G1 stage of the cell growth cycle. In conclusion, an increase in the size of the lipid droplets is detected in morphologically viable cells during cisplatin exposure. (1) H MRS can detect lipid alterations during cell cycle arrest and progression of cell death, and has the potential to provide a noninvasive biomarker of treatment efficacy in vivo.

  9. Metabolic Profiling of Intact Arabidopsis thaliana Leaves during Circadian Cycle Using 1H High Resolution Magic Angle Spinning NMR

    PubMed Central

    van Schadewijk, R.; de Groot, H. J. M.; Alia, A.

    2016-01-01

    Arabidopsis thaliana is the most widely used model organism for research in plant biology. While significant advances in understanding plant growth and development have been made by focusing on the molecular genetics of Arabidopsis, extracting and understanding the functional framework of metabolism is challenging, both from a technical perspective due to losses and modification during extraction of metabolites from the leaves, and from the biological perspective, due to random variation obscuring how well the function is performed. The purpose of this work is to establish the in vivo metabolic profile directly from the Arabidopsis thaliana leaves without metabolite extraction, to reduce the complexity of the results by multivariate analysis, and to unravel the mitigation of cellular complexity by predominant functional periodicity. To achieve this, we use the circadian cycle that strongly influences metabolic and physiological processes and exerts control over the photosynthetic machinery. High resolution-magic angle spinning nuclear magnetic resonance (HR-MAS NMR) was applied to obtain the metabolic profile directly from intact Arabidopsis leaves. Combining one- and two-dimensional 1H HR-MAS NMR allowed the identification of several metabolites including sugars and amino acids in intact leaves. Multivariate analysis on HR-MAS NMR spectra of leaves throughout the circadian cycle revealed modules of primary metabolites with significant and consistent variations of their molecular components at different time points of the circadian cycle. Since robust photosynthetic performance in plants relies on the functional periodicity of the circadian rhythm, our results show that HR-MAS NMR promises to be an important non-invasive method that can be used for metabolomics of the Arabidopsis thaliana mutants with altered physiology and photosynthetic efficiency. PMID:27662620

  10. Live-cell high resolution magic angle spinning magnetic resonance spectroscopy for in vivo analysis of Pseudomonas aeruginosa metabolomics

    PubMed Central

    RIGHI, VALERIA; CONSTANTINOU, CATERINA; KESARWANI, MEENU; RAHME, LAURENCE G.; TZIKA, ARIA A.

    2013-01-01

    Pseudomonas aeruginosa (PA) is a pathogenic gram-negative bacterium that is widespread in nature, inhabiting soil, water, plants and animals. PA is a prevalent cause of deleterious human infections, particularly in patients whose host defense mechanisms have been compromised. Metabolomics is an important tool used to study host-pathogen interactions and to identify novel therapeutic targets and corresponding compounds. The aim of the present study was to report the metabolic profile of live PA bacteria using in vivo high-resolution magic angle spinning (HRMAS) nuclear magnetic resonance spectroscopy (NMR), in combination with 1- and 2-dimensional HRMAS NMR. This methodology provides a new and powerful technique to rapidly interrogate the metabolome of intact bacterial cells and has several advantages over traditional techniques that identify metabolome components from disrupted cells. Furthermore, application of multidimensional HRMAS NMR, in combination with the novel technique total through-Bond correlation Spectroscopy (TOBSY), is a promising approach that may be used to obtain in vivo metabolomics information from intact live bacterial cells and can mediate such analyses in a short period of time. Moreover, HRMAS 1H NMR enables the investigation of the associations between metabolites and cell processes. In the present study, we detected and quantified several informative metabolic molecules in live PA cells, including N-acetyl, betaine, citrulline, alanine and glycine, which are important in peptidoglycan synthesis. The results provided a complete metabolic profile of PA for future studies of PA clinical isolates and mutants. In addition, this in vivo NMR biomedical approach might have clinical utility and should prove useful in gene function validation, the study of pathogenetic mechanisms, the classification of microbial strains into functional/clinical groups, the testing of anti-bacterial agents and the determination of metabolic profiles of bacterial

  11. 3D Double-Quantum/Double-Quantum Exchange Spectroscopy of Protons under 100 kHz Magic Angle Spinning.

    PubMed

    Zhang, Rongchun; Duong, Nghia Tuan; Nishiyama, Yusuke; Ramamoorthy, Ayyalusamy

    2017-06-22

    Solid-state (1)H NMR spectroscopy has attracted much attention in the recent years due to the remarkable spectral resolution improvement by ultrafast magic-angle-spinning (MAS) as well as due to the sensitivity enhancement rendered by proton detection. Although these developments have enabled the investigation of a variety of challenging chemical and biological solids, the proton spectral resolution is still poor for many rigid solid systems owing to the presence of conformational heterogeneity and the unsuppressed residual proton-proton dipolar couplings even with the use of the highest currently feasible sample spinning speed of ∼130 kHz. Although a further increase in the spinning speed of the sample could be beneficial to some extent, there is a need for alternate approaches to enhance the spectral resolution. Herein, by fully utilizing the benefits of double-quantum (DQ) coherences, we propose a single radio frequency channel proton-based 3D pulse sequence that correlates double-quantum (DQ), DQ, and single-quantum (SQ) chemical shifts of protons. In addition to the two-spin homonuclear proximity information, the proposed 3D DQ/DQ/SQ experiment also enables the extraction of three-spin and four-spin proximities, which could be beneficial for revealing the dipolar coupled proton network in the solid state. Besides, the 2D DQ/DQ spectrum sliced at different isotropic SQ chemical shift values of the 3D DQ/DQ/SQ spectrum will also facilitate the identification of DQ correlation peaks and improve the spectral resolution, as it only provides the local homonuclear correlation information associated with the specific protons selected by the SQ chemical shift frequency. The 3D pulse sequence and its efficiency are demonstrated experimentally on small molecular compounds in the solid state. We expect that this approach would create avenues for further developments by suitably combining the benefits of partial deuteration of samples, selective excitation

  12. Alterations in creatine metabolism observed in experimental autoimmune myocarditis using ex vivo proton magic angle spinning MRS.

    PubMed

    Muench, Frédéric; Retel, Joren; Jeuthe, Sarah; O h-Ici, Darach; van Rossum, Barth; Wassilew, Katharina; Schmerler, Patrick; Kuehne, Titus; Berger, Felix; Oschkinat, Hartmut; Messroghli, Daniel R

    2015-12-01

    Experimental autoimmune myocarditis (EAM) in rodents is an accepted model of myocarditis and dilated cardiomyopathy (DCM). Altered metabolism is thought to play an important role in the pathogenesis of DCM and heart failure (HF). Study of the metabolism may provide new diagnostic information and insights into the mechanisms of myocarditis and HF. Proton MRS ((1)H-MRS) has not yet been used to study the changes occurring in myocarditis and subsequent HF. We aimed to explore the changes in creatine metabolism using this model and compare them with the findings in healthy animals. Myocardial function of male young Lewis rats with EAM was quantified by performing left ventricular ejection fraction (LVEF) analysis in short-axis cine images throughout the whole heart. Inflammatory cellular infiltrate was assessed by immunohistochemistry. Myocardial tissue was analyzed using ex vivo proton magic angle spinning MRS ((1)H-MAS-MRS). Myocarditis was confirmed histologically by the presence of an inflammatory cellular infiltrate and CD68 positive staining. A significant increase in the metabolic ratio of Tau/tCr (taurine/total creatine) obtained by (1)H-MAS-MRS was observed in myocarditis compared with healthy controls (21 d acute EAM, 4.38 (±0.23); 21 d control, 2.84 (±0.08); 35 d chronic EAM, 4.47 (±0.83); 35 d control, 2.59 (±0.38); P < 0.001). LVEF was reduced in diseased animals (EAM, 55.2% (±11.3%); control, 72.6% (±3.8%); P < 0.01) and correlated with Tau/tCr ratio (R = 0.937, P < 0.001). Metabolic alterations occur acutely with the development of myocarditis. Myocardial Tau/tCr ratio as detected by (1)H-MRS correlates with LVEF and is able to differentiate between healthy myocardium and myocardium from rats with EAM.

  13. Accurate determination of chemical shift tensor orientations of single-crystals by solid-state magic angle spinning NMR.

    PubMed

    Avadhut, Yamini S; Weber, Johannes; Schmedt Auf der Günne, Jörn

    2017-09-01

    An improved implementation of single-crystal magic-angle-spinning (MAS) NMR is presented which gives access to chemical shift tensors both in orientation (relative to the crystal axis system) and principal axis values. For mounting arbitrary crystals inside ordinary MAS rotors, a mounting tool is described which allows to relate the crystal orientation determined by diffraction techniques to the rotor coordinate system. The crystal is finally mounted into a MAS rotor equipped with a special insert which allows a defined reorientation of the single-crystal by 90°. The approach is based on the idea that the dispersive spectra, which are obtained when applying read-pulses at specific rotor-phases, not only yield the size of the eigenvalues but also encode the orientation of the different chemical shift (rank-2) tensors. For this purpose two 2D-data sets with orthogonal crystal orientation are fitted simultaneously. The presented analysis for chemical shift tensors is supported by an analytical formula which allows fast calculation of phase and amplitude of individual spinning side-bands and by a protocol which solves the problem of finding the correct reference phase of the spectrum. Different rotor-synchronized pulse-sequences are introduced for the same reason. Experiments are performed on L-alanine and O-phosphorylethanolamine and the observed errors are analyzed in detail. The experimental data are opposed to DFT-computed chemical shift tensors which have been obtained by the extended embedded ion method. Copyright © 2017 Elsevier Inc. All rights reserved.

  14. Surface Interactions and Confinement of Methane: A High Pressure Magic Angle Spinning NMR and Computational Chemistry Study.

    PubMed

    Ok, Salim; Hoyt, David W; Andersen, Amity; Sheets, Julie; Welch, Susan A; Cole, David R; Mueller, Karl T; Washton, Nancy M

    2017-02-14

    Characterization and modeling of the molecular-level behavior of simple hydrocarbon gases, such as methane, in the presence of both nonporous and nanoporous mineral matrices allows for predictive understanding of important processes in engineered and natural systems. In this study, changes in local electromagnetic environments of the carbon atoms in methane under conditions of high pressure (up to 130 bar) and moderate temperature (up to 346 K) were observed with (13)C magic-angle spinning (MAS) NMR spectroscopy while the methane gas was mixed with two model solid substrates: a fumed nonporous, 12 nm particle size silica and a mesoporous silica with 200 nm particle size and 4 nm average pore diameter. Examination of the interactions between methane and the silica systems over temperatures and pressures that include the supercritical regime was allowed by a novel high pressure MAS sample containment system, which provided high resolution spectra collected under in situ conditions. For pure methane, no significant thermal effects were found for the observed (13)C chemical shifts at all pressures studied here (28.2, 32.6, 56.4, 65.1, 112.7, and 130.3 bar). However, the (13)C chemical shifts of resonances arising from confined methane changed slightly with changes in temperature in mixtures with mesoporous silica. The chemical shift values of (13)C nuclides in methane change measurably as a function of pressure both in the pure state and in mixtures with both silica matrices, with a more pronounced shift when meso-porous silica is present. Molecular-level simulations utilizing GCMC, MD, and DFT confirm qualitatively that the experimentally measured changes are attributed to interactions of methane with the hydroxylated silica surfaces as well as densification of methane within nanopores and on pore surfaces.

  15. Magic-angle-spinning NMR on solid biological systems. Analysis Of the origin of the spectral linewidths

    NASA Astrophysics Data System (ADS)

    Hemminga, M. A.; de Jager, P. A.; Krüse, J.; Lamerichs, R. M. J. N.

    Magic-angle-spinning (MAS) high-power 1H-decoupled 13C and 31P NMR has been applied to solid biological materials to obtain information about the mechanisms that determine the spectral linewidths. The line broadening in MAS 31P NMR spectra of solid tobacco mosaic virus (TMV) has been investigated by selective saturation and T2 measurements. About 90 Hz stems from homogeneous effects, whereas the inhomogeneous contribution is approximately 100 Hz. The inhomogeneous line broadening is assigned to macroscopic inhomogeneities in the sample and not to variations in the nucleotide bases along the RNA strand in TMV. It is concluded that sample preparation is of vital importance for obtaining well-resolved spectra. Under optimal preparation techniques the isotropic values of the chemical shift of the different 31P sites have been determined to obtain information about the secondary structure of the viral RNA. The chemical shift anisotropy has been determined from the relative intensities of the spinning side bands in the spectra. The chemical shift information is used to make a tentative assignment of the resonance in terms of the three structurally distinguishable phosphate groups in TMV. The origin of the linewidths in MAS NMR has been examined further by 13C NMR of approximately 10% 13C-enriched coat protein of cowpea chlorotic mottle virus, using selective excitation and saturation techniques, as well as measurements of the relaxation times T1 γ and T2. The CO resonance in the spectrum is composed of an inhomogeneous and homogeneous part with a total linewidth of 700 Hz. The homogeneous linewidth, contributing with 200 Hz, is found to arise from slow molecular motions in the solid on a millisecond timescale.

  16. Mineral Carbonation in Wet Supercritical CO2: An in situ High-Pressure Magic Angle Spinning Nuclear Magnetic Resonance Study

    NASA Astrophysics Data System (ADS)

    Turcu, R. V.; Hoyt, D. H.; Sears, J. A.; Rosso, K. M.; Felmy, A. R.; Hu, J. Z.

    2011-12-01

    Understanding the mechanisms and kinetics of mineral carbonation reactions relevant to sequestering carbon dioxide as a supercritical fluid (scCO2) in geologic formations is crucial for accurately predicting long-term storage risks. In situ probes that provide molecular-level information at geologically relevant temperatures and pressures are highly desirable and challenging to develop. Magic angle spinning nuclear magnetic resonance (MAS NMR) is a powerful tool for obtaining detailed molecular structure and dynamics information of a system regardless whether the system is in a solid, a liquid, a gaseous, a supercritical state, or a mixture thereof. However, MAS NMR under scCO2 conditions has never been realized due to the tremendous technical difficulties of achieving and maintaining high pressure within a fast spinning MAS sample rotor. In this work, we report development of a unique high pressure MAS NMR capability capable of handling fluid pressure exceeding 170 bars and temperatures up to 80°C, and its application to mineral carbonation in scCO2 under geologically relevant temperatures and pressures. Mineral carbonation reactions of the magnesium silicate mineral forsterite and the magnesium hydroxide brucite reacted with scCO2 (up to 170 bar) and containing variable content of H2O (at, below, and above saturation in scCO2) were investigated at 50 to 70°C. In situ 13C MAS NMR spectra show peaks corresponding to the reactants, intermediates, and the magnesium carbonation products in a single spectrum. For example, Figure 1 shows the reaction dynamics, i.e., the formation and conversion of reaction intermediates, i.e., HCO3- and nesquehonite, to magnesite as a function of time at 70°C. This capability offers a significant advantage over traditional ex situ 13C MAS experiments on similar systems, where, for example, CO2 and HCO3- are not directly observable.

  17. Non-destructive method for determining neutron exposure

    DOEpatents

    Gold, R.; McElroy, W.N.

    1983-11-01

    A non-destructive method for determination of neutron exposure in an object, such as a reactor pressure vessel, is based on the observation of characteristic gamma-rays emitted by activation products in the object by using a unique continuous gamma-ray spectrometer. The spectrometer views the object through appropriate collimators to determine the absolute emission rate of these characteristic gamma-rays, thereby ascertaining the absolute activity of given activation products in the object. These data can then be used to deduce the spatial and angular dependence of neutron exposure at regions of interest within the object.

  18. APPARATUS FOR NON-DESTRUCTIVE INSPECTION OF CANTILEVERED MEMBERS

    DOEpatents

    Taylor, E.R.; Mahoney, C.H.; Lay, C.R.

    1961-10-24

    An apparatus for non-destructive inspection of cantilevered members, such as compressor blades, is described. The member under inspection is vibrated with a regulated source of air under pressure. The amplitude of vibration of the member is maintained at its natural frequency. The frequency of vibration of the member is measured. An indication of an excessive decay or erratic shifting in the measured frequency above an allowable hysteretic decay is provided as an indication of a fault in the member. The member is vibrated for a selected test period. (AEC)

  19. Non-Destructive Inspection Methods for Propulsion Systems and Components

    DTIC Science & Technology

    1979-04-01

    Oftopulsion and Energetics Panel", et du "Consuiltant and Exchange Programm" d. 1’AGARD. RII* a pour but d’exarniner et do commenter l𔃾tat actual do l’art...Exchange Program" of AGARD. Its aim is to examine and comment on to-day’s state of the art, and the foreseeable or hoped progress of the non-destructive...should be recognised as such. These notes will therefore review and comment on the general problem, but emphaais will be on the application of minute

  20. Asymmetric signal intensity in normal collateral ligaments of the distal interphalangeal joint in horses with a low-field MRI system due to the magic angle effect.

    PubMed

    Spriet, Mathieu; Mai, Wilfried; McKnight, Alexia

    2007-01-01

    Increased signal intensity in one of the collateral ligaments of the distal interphalangeal (DIP) joint of sound horses in images acquired using a low-field magnet with vertical orientation of the magnetic field was investigated as a possible manifestation of the magic angle effect. Three isolated equine digits were imaged using the following pulse sequences: (1) spin echo TI, (2) turbo spin echo proton density and T2, and (3) 3D gradient echo T1, in different positions by mildly changing the orientation of the long axis of the digit, in the dorsal plane, relative to the magnetic field. The signal intensity in a ligament was significantly increased when the ligament orientation relative to the magnetic field was 55 +/- 10 degrees. The signal intensity was markedly increased in pulse sequences with short echo time (TE) 5.0, 4.9, and 3.9 times increased, respectively, for 3D gradient echo T1, spin echo T1, and turbo spin echo proton density) and to a lesser extent with pulse sequences with a longer TE (1.8 times increased for turbo spin echo T2). These changes are characteristic of the magic angle effect. Because of the anatomic orientation of the collateral ligaments of the DIP joint, a slight deviation of the long axis of the digit in the dorsal plane, from the ideal horizontal position, will induce an increased signal intensity that can be confused with desmitis. Careful positioning of the foot in magnetic resonance imaging systems where B0 is perpendicular to the long axis of the digit is critical to prevent the occurrence of the magic angle effect.

  1. Characterization of divalent metal metavanadates by 51V magic-angle spinning NMR spectroscopy of the central and satellite transitions.

    PubMed

    Nielsen, U G; Jakobsen, H J; Skibsted, J

    2000-05-15

    51V quadrupole coupling and chemical shielding tensors have been determined from 51V magic-angle spinning (MAS) NMR spectra at a magnetic field of 14.1 T for nine divalent metal metavanadates: Mg(VO3)2, Ca(VO3)2, Ca(VO3)(2).4H2O, alpha-Sr(VO3)2, Zn(VO3)2, alpha- and beta-Cd(VO3)2. The manifold of spinning sidebands (ssbs) from the central and satellite transitions, observed in the 15V MAS NMR spectra, have been analyzed using least-squares fitting and numerical error analysis. This has led to a precise determination of the eight NMR parameters characterizing the magnitudes and relative orientations of the quadrupole coupling and chemical shielding tensors. The optimized data show strong similarities between the NMR parameters for the isostructural groups of divalent metal metavanadates. This demonstrates that different types of metavanadates can easily be distinguished by their anisotropic NMR parameters. The brannerite type of divalent metal metavanadates exhibits very strong 51V quadrupole couplings (i.e., CQ = 6.46-7.50 MHz), which reflect the highly distorted octahedral environments for the V5+ ion in these phases. Linear correlations between the principal tensor elements for the 51V quadrupole coupling tensors and electric field gradient tensor elements, estimated from point-monopole calculations, are reported for the divalent metal metavanadates. These correlations are used in the assignment of the NMR parameters for the different crystallographic 51V sites of Ca(VO3)(2).4H2O, Pb(VO3)2, and Ba(VO3)2. For alpha-Sr(VO3)2, with an unknown crystal structure, the 51V NMR data strongly suggest that this metavanadate is isostructural with Ba(VO3)2, for which the crystal structure has been reported. Finally, the chemical shielding parameters for orthovanadates and mono- and divalent metal metavanadates are compared.

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

    PubMed Central

    PARTHASARATHY, SUDHAKAR; NISHIYAMA, YUSUKE; ISHII, YOSHITAKA

    2013-01-01

    CONSPECTUS Recent research in fast magic angle spinning (MAS) methods has drastically improved in the resolution and sensitivity for NMR spectroscopy of biomolecules and materials in solids. In this Account, we summarizes recent and ongoing developments in this area by presenting 13C and 1H 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 20 kHz allows us to overcome major difficulties in 1H and 13C 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) using short 1H T1 values we can perform 1H SSNMR micro-analysis of paramagnetic systems in the μg scale with greatly improved sensitivity over that for diamagnetic systems. Second, we discuss how VFMAS at a spinning speed greater than ~40 kHz can enhance the sensitivity and resolution of 13C biomolecular SSNMR measurements. Low-power 1H decoupling schemes under VFMAS offer excellent spectral resolution for 13C SSNMR by nominal 1H RF irradiation at ~10 kHz. By combining the VFMAS approach and enhanced 1H T1 relaxation by paramagnetic doping we can achieve extremely fast recycling in modern biomolecular SSNMR experiments. Experiments for 13C-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 13C SSNMR measurements for biomolecules under faster MAS at a higher field. Our preliminary 13C SSNMR data of Aβ amyloid fibrils and GB1 microcrystals acquired at 1H NMR frequencies of 750-800 MHz suggest that the combined use of the PACC approach and the ultra-high fields could allow for routine multi-dimensional SSNMR analyses of proteins at the 50-200 nmol level. Also, we briefly discuss the prospects for studying bimolecules using 13

  3. Spin dynamics in the modulation frame: application to homonuclear recoupling in magic angle spinning solid-state NMR.

    PubMed

    De Paëpe, Gaël; Lewandowski, Józef R; Griffin, Robert G

    2008-03-28

    We introduce a family of solid-state NMR pulse sequences that generalizes the concept of second averaging in the modulation frame and therefore provides a new approach to perform magic angle spinning dipolar recoupling experiments. Here, we focus on two particular recoupling mechanisms-cosine modulated rotary resonance (CMpRR) and cosine modulated recoupling with isotropic chemical shift reintroduction (COMICS). The first technique, CMpRR, is based on a cosine modulation of the rf phase and yields broadband double-quantum (DQ) (13)C recoupling using >70 kHz omega(1,C)/2pi rf field for the spinning frequency omega(r)/2=10-30 kHz and (1)H Larmor frequency omega(0,H)/2pi up to 900 MHz. Importantly, for p>or=5, CMpRR recouples efficiently in the absence of (1)H decoupling. Extension to lower p values (3.5

  4. Characterization of the magic angle effect in the equine deep digital flexor tendon using a low-field magnetic resonance system.

    PubMed

    Spriet, Mathieu; McKnight, Alexia

    2009-01-01

    Three isolated equine limbs were imaged with a low-field magnetic resonance system with a vertical magnetic field. Each limb was scanned in multiple positions with mild variation of the angle between the magnetic field and the long axis of the limb. When the long axis of the limb was not perpendicular to the magnetic field, a linear hyperintense signal was present at the palmar aspect of one of the deep digital flexor tendon lobes, at the level of the navicular bone and collateral sesamoidean ligaments, in proton density and T1-weighted pulse sequences. With increased angulation of the limb, the palmar hyperintense signal extended farther distally and proximally and additional signal hyperintensity was present at the dorsal aspect of the distal part of the other lobe of the deep digital flexor tendon. Increased signal intensity was also present in the collateral ligament of the distal interphalangeal joint on the same side as the palmar hyperintense signal in the tendon. The changes in the deep digital flexor tendon are due to the specific orientation of fibers at the palmar and dorsal aspect of the tendon, which is responsible for focal manifestation of the magic angle effect. Careful positioning of the limb perpendicular to the magnetic field can prevent this phenomenon. The association of palmar increased signal intensity in the deep digital flexor tendon with increased signal in the collateral ligament of the distal interphalangeal joint on the same side should be recognized as manifestations of the magic angle effect.

  5. Laser active thermography for non-destructive testing

    NASA Astrophysics Data System (ADS)

    Semerok, A.; Grisolia, C.; Fomichev, S. V.; Thro, P.-Y.

    2013-11-01

    Thermography methods have found their applications in different fields of human activity. The non-destructive feature of these methods along with the additional advantage by automated remote control and tests of nuclear installations without personnel attendance in the contaminated zone are of particular interest. Laser active pyrometry and laser lock-in thermography for in situ non-destructive characterization of micrometric layers on graphite substrates from European tokamaks were under extensive experimental and theoretical studies in CEA (France). The studies were aimed to obtain layer characterization with cross-checking the layer thermal contact coefficients determined by active laser pyrometry and lock-in thermography. The experimental installation comprised a Nd-YAG pulsed repetition rate laser (1 Hz - 10 kHz repetition rate frequency, homogeneous spot) and a home-made pyrometer system based on two pyrometers for the temperature measurements in 500 - 2600 K range. For both methods, the layer characterization was provided by the best fit of the experimental results and simulations. The layer thermal contact coefficients determined by both methods were quite comparable. Though there was no gain in the measurements accuracy, lock-in measurements have proved their advantage as being much more rapid. The obtained experimental and theoretical results are presented. Some practical applications and possible improvements of the methods are discussed.

  6. Local defect resonance for sensitive non-destructive testing

    NASA Astrophysics Data System (ADS)

    Adebahr, W.; Solodov, I.; Rahammer, M.; Gulnizkij, N.; Kreutzbruck, M.

    2016-02-01

    Ultrasonic wave-defect interaction is a background of ultrasound activated techniques for imaging and non-destructive testing (NDT) of materials and industrial components. The interaction, primarily, results in acoustic response of a defect which provides attenuation and scattering of ultrasound used as an indicator of defects in conventional ultrasonic NDT. The derivative ultrasonic-induced effects include e.g. nonlinear, thermal, acousto-optic, etc. responses also applied for NDT and defect imaging. These secondary effects are normally relatively inefficient so that the corresponding NDT techniques require an elevated acoustic power and stand out from conventional ultrasonic NDT counterparts for their specific instrumentation particularly adapted to high-power ultrasonic. In this paper, a consistent way to enhance ultrasonic, optical and thermal defect responses and thus to reduce an ultrasonic power required is suggested by using selective ultrasonic activation of defects based on the concept of local defect resonance (LDR). A strong increase in vibration amplitude at LDR enables to reliably detect and visualize the defect as soon as the driving ultrasonic frequency is matched to the LDR frequency. This also provides a high frequency selectivity of the LDR-based imaging, i.e. an opportunity of detecting a certain defect among a multitude of other defects in material. Some examples are shown how to use LDR in non-destructive testing techniques, like vibrometry, ultrasonic thermography and shearography in order to enhance the sensitivity of defect visualization.

  7. Non destructive testing of works of art by terahertz analysis

    NASA Astrophysics Data System (ADS)

    Bodnar, Jean-Luc; Metayer, Jean-Jacques; Mouhoubi, Kamel; Detalle, Vincent

    2013-11-01

    Improvements in technologies and the growing security needs in airport terminals lead to the development of non destructive testing devices using terahertz waves. Indeed, these waves have the advantage of being, on one hand, relatively penetrating. They also have the asset of not being ionizing. It is thus potentially an interesting contribution in the non destructive testing field. With the help of the VISIOM Company, the possibilities of this new industrial analysis method in assisting the restoration of works of art were then approached. The results obtained within this framework are presented here and compared with those obtained by infrared thermography. The results obtained show first that the THZ method, like the stimulated infrared thermography allows the detection of delamination located in murals paintings or in marquetries. They show then that the THZ method seems to allow detecting defects located relatively deeply (10 mm) and defects potentially concealed by other defects. It is an advantage compared to the stimulated infra-red thermography which does not make it possible to obtain these results. Furthermore, they show that the method does not seem sensitive to the various pigments constituting the pictorial layer, to the presence of a layer of "Japan paper" and to the presence of a layer of whitewash. It is not the case of the stimulated infrared thermography. It is another advantage of the THZ method. Finally, they show that the THZ method is limited in the detection of low-size defects. It is a disadvantage compared to the stimulated infrared thermography.

  8. 1H–13C hetero-nuclear dipole–dipole couplings of methyl groups in stationary and magic angle spinning solid-state NMR experiments of peptides and proteins

    PubMed Central

    Wu, Chin H.; Das, Bibhuti B.; Opella, Stanley J.

    2010-01-01

    13C NMR of isotopically labeled methyl groups has the potential to combine spectroscopic simplicity with ease of labeling for protein NMR studies. However, in most high resolution separated local field experiments, such as polarization inversion spin exchange at the magic angle (PISEMA), that are used to measure 1H–13C hetero-nuclear dipolar couplings, the four-spin system of the methyl group presents complications. In this study, the properties of the 1H–13C hetero-nuclear dipolar interactions of 13C-labeled methyl groups are revealed through solid-state NMR experiments on a range of samples, including single crystals, stationary powders, and magic angle spinning of powders, of 13C3 labeled alanine alone and incorporated into a protein. The spectral simplifications resulting from proton detected local field (PDLF) experiments are shown to enhance resolution and simplify the interpretation of results on single crystals, magnetically aligned samples, and powders. The complementarity of stationary sample and magic angle spinning (MAS) measurements of dipolar couplings is demonstrated by applying polarization inversion spin exchange at the magic angle and magic angle spinning (PISEMAMAS) to unoriented samples. PMID:19896874

  9. (1)H-(13)C Hetero-nuclear dipole-dipole couplings of methyl groups in stationary and magic angle spinning solid-state NMR experiments of peptides and proteins.

    PubMed

    Wu, Chin H; Das, Bibhuti B; Opella, Stanley J

    2010-02-01

    (13)C NMR of isotopically labeled methyl groups has the potential to combine spectroscopic simplicity with ease of labeling for protein NMR studies. However, in most high resolution separated local field experiments, such as polarization inversion spin exchange at the magic angle (PISEMA), that are used to measure (1)H-(13)C hetero-nuclear dipolar couplings, the four-spin system of the methyl group presents complications. In this study, the properties of the (1)H-(13)C hetero-nuclear dipolar interactions of (13)C-labeled methyl groups are revealed through solid-state NMR experiments on a range of samples, including single crystals, stationary powders, and magic angle spinning of powders, of (13)C(3) labeled alanine alone and incorporated into a protein. The spectral simplifications resulting from proton detected local field (PDLF) experiments are shown to enhance resolution and simplify the interpretation of results on single crystals, magnetically aligned samples, and powders. The complementarity of stationary sample and magic angle spinning (MAS) measurements of dipolar couplings is demonstrated by applying polarization inversion spin exchange at the magic angle and magic angle spinning (PISEMAMAS) to unoriented samples. Copyright 2009 Elsevier Inc. All rights reserved.

  10. Non-Destructive Evaluation of Thermal Spray Coating Interface Quality by Eddy Current Method

    SciTech Connect

    B.Mi; X. Zhao; R. Bayles

    2006-05-26

    Thermal spray coating is usually applied through directing molten or softened particles at very high velocities onto a substrate. An eddy current non-destructive inspection technique is presented here for thermal spray coating interface quality characterization. Several high-velocity-oxy-fuel (HVOF) coated steel plates were produced with different surface preparation conditions before applying the coating, e.g., grit-blasted surface, wire-brush cleaned surface, and a dirty surface. A quad-frequency eddy current probe was used to manually scan over the coating surface to evaluate the bonding quality. Experimental results show that the three surface preparation conditions can be successfully differentiated by looking into the impedance difference observed from the eddy current probe. The measurement is fairly robust and consistent. More specimens are also prepared with variations of process parameters, such as spray angle, stand-off distance, and application of corrosion protective sealant, etc. They are blindly tested to evaluate the reliability of the eddy current system. Quantitative relations between the coating bond strength and the eddy current response are also established with the support of destructive testing. This non-contact, non-destructive, easy to use technique has the potential for evaluating the coating quality immediately after its application so that any defects can be corrected immediately.

  11. Non-destructive Detection for Mold Colonies in Rice Based on Hyperspectra and GWO-SVR.

    PubMed

    Sunli, Cong; Jun, Sun; Hanping, Mao; Xiaohong, Wu; Pei, Wang; Xiaodong, Zhang

    2017-08-08

    Mold contamination of grains not only contributes to unedible food, resulting in economic losses, but also leads to mold in humans and livestock, even can be carcinogenic to them. Rice as one of the main grain varieties, if improper storage, is easily to mildew. In order to detect the total number of mold colonies in rice more accurately, a method based on hyperspectral imaging technology was investigated. In this paper, non-destructive detection for the total number of mold colonies in rice was performed from the angle of spectral analysis. The determination coefficient of 0.9621 for calibration set and 0.9511 for prediction set between the spectral data and number of mold colonies were eventually achieved by establishing the best support vector regression (SVR) model, optimised by gray wolf optimization (GWO) algorithm. The hyperspectral imaging technology combined with the optimal model (GWO-SVR) is feasible for non-destructive detection of the total number of mold colonies in rice, and so hopefully to provide a promising tool for the mold detection of other agricultural products. This article is protected by copyright. All rights reserved.

  12. Magic angle effect on low field magnetic resonance images in the superficial digital flexor tendon in the equine proximal pastern region.

    PubMed

    Sherlock, C E; Mair, T S

    2016-11-01

    Recognition of artefacts is an essential component of the accurate interpretation of diagnostic images. This study aimed to investigate the presence of magic angle effect in the superficial digital flexor tendon (SDFT) in the equine proximal pastern region. The proximal pastern of four cadaver limbs was imaged using a 0.27 Tesla magnet with high-resolution sequences that are commonly utilised in clinical equine practice. The limbs were imaged in a neutral position and positions that simulated the horse 'leaning in', 'leaning out' and having internal and external rotation of the distal limb. Signal intensity changes in the SDFT were described and compared. The simulated 'leaning in' and external rotation positions resulted in increased signal intensity in the axial and middle thirds of the lateral half of the SDFT on sequences with short echo times. The simulated 'leaning out' and internal rotation positions resulted in increased signal intensity in the axial and middle thirds of the medial half of the SDFT on sequences with short echo times. These signal intensity changes did not occur or were only mild and inconsistent on T2 fast spin echo sequences with longer echo times. The increases in signal intensity in the SDFT are consistent with a position-induced magic angle artefact that has been noted in clinical cases. Attention to positioning of the equine distal limb is essential during clinical imaging; radiologists should be aware of position-induced artefacts to ensure accurate image interpretation.

  13. A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins.

    PubMed

    Sharma, Kshama; Madhu, Perunthiruthy K; Mote, Kaustubh R

    2016-08-01

    One of the fundamental challenges in the application of solid-state NMR is its limited sensitivity, yet a majority of experiments do not make efficient use of the limited polarization available. The loss in polarization in a single acquisition experiment is mandated by the need to select out a single coherence pathway. In contrast, sequential acquisition strategies can encode more than one pathway in the same experiment or recover unused polarization to supplement a standard experiment. In this article, we present pulse sequences that implement sequential acquisition strategies on one and two radiofrequency channels with a combination of proton and carbon detection to record multiple experiments under magic-angle spinning. We show that complementary 2D experiments such as [Formula: see text] and [Formula: see text] or DARR and [Formula: see text], and 3D experiments such as [Formula: see text] and [Formula: see text], or [Formula: see text] and [Formula: see text]  can be combined in a single experiment to ensure time savings of at least 40 %. These experiments can be done under fast or slow-moderate magic-angle spinning frequencies aided by windowed [Formula: see text] acquisition and homonulcear decoupling. The pulse sequence suite is further expanded by including pathways that allow the recovery of residual polarization, the so-called 'afterglow' pathways, to encode a number of pulse sequences to aid in assignments and chemical-shift mapping.

  14. Fast magic-angle sample spinning solid-state NMR at 60-100kHz for natural abundance samples.

    PubMed

    Nishiyama, Yusuke

    2016-09-01

    In spite of tremendous progress made in pulse sequence designs and sophisticated hardware developments, methods to improve sensitivity and resolution in solid-state NMR (ssNMR) are still emerging. The rate at which sample is spun at magic angle determines the extent to which sensitivity and resolution of NMR spectra are improved. To this end, the prime objective of this article is to give a comprehensive theoretical and experimental framework of fast magic angle spinning (MAS) technique. The engineering design of fast MAS rotors based on spinning rate, sample volume, and sensitivity is presented in detail. Besides, the benefits of fast MAS citing the recent progress in methodology, especially for natural abundance samples are also highlighted. The effect of the MAS rate on (1)H resolution, which is a key to the success of the (1)H inverse detection methods, is described by a simple mathematical factor named as the homogeneity factor k. A comparison between various (1)H inverse detection methods is also presented. Moreover, methods to reduce the number of spinning sidebands (SSBs) for the systems with huge anisotropies in combination with (1)H inverse detection at fast MAS are discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  15. Orientation of functional groups of soil organic matter on the surface of water repellent soils determined by pulse saturation magic angle spinning (PSTMAS) nuclear magnetic resonance (NMR) spectroscopy

    NASA Astrophysics Data System (ADS)

    Hiradate, Syuntaro; Kawamoto, Ken; Senani Wijewardana, Nadeeka; Müller, Karin; Møldrup, Per; Clothier, Brent; Komatsu, Toshiko

    2014-05-01

    Orientation of functional groups of soil organic matter on soil particles plays a crucial role in the occurrence of soil water repellency. In addition to a general method to characterize soil organic matter using cross polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) technique, we determined the surface orientation of functional groups in water repellent soils by using pulse saturation magic angle spinning (PSTMAS) NMR technique. A preliminary experiment confirmed that the PSTMAS NMR spectrum successfully determined the high mobility of methyl group of octadecylsilylated silica gels when a comparison was made with that of CPMAS NMR. This means that the methyl group oriented towards the outside of the silica gel particle. Similarly, for an experimental system consisting of mixtures of octadecylsilylated silica gel and dimethyl sulfoxide (DMSO), the extremely high mobility of methyl group derived from DMSO was detected using the same methodology. For water repellent soils from Japan and New Zealand, it was found that the methyl and methylene groups were highly mobile. In contrast, the NMR signals of aromatic moiety, another hydrophobic moiety of soil organic matter, were not as intense in PSTMAS compared with CPMAS. From these results, we conclude that alkyl moiety (methyl and methylene groups) would be oriented towards the outside of the soil particle and would play an important role in the appearance of water repellency of soils.

  16. Non-destructive shadowgraph imaging of ultra-cold atoms.

    PubMed

    Wigley, P B; Everitt, P J; Hardman, K S; Hush, M R; Wei, C H; Sooriyabandara, M A; Manju, P; Close, J D; Robins, N P; Kuhn, C C N

    2016-10-15

    An imaging system is presented that is capable of far-detuned non-destructive imaging of a Bose-Einstein condensate with the signal proportional to the second spatial derivative of the density. Whilst demonstrated with application to Rb85, the technique generalizes to other atomic species and is shown to be capable of a signal-to-noise of ∼25 at 1 GHz detuning with 100 in-trap images showing no observable heating or atom loss. The technique is also applied to the observation of individual trajectories of stochastic dynamics inaccessible to single shot imaging. Coupled with a fast optical phase locked loop, the system is capable of dynamically switching to resonant absorption imaging during the experiment.

  17. Non-destructive shadowgraph imaging of ultra-cold atoms

    NASA Astrophysics Data System (ADS)

    Wigley, P. B.; Everitt, P. J.; Hardman, K. S.; Hush, M. R.; Wei, C. H.; Sooriyabandara, M. A.; Manju, P.; Close, J. D.; Robins, N. P.; Kuhn, C. C. N.

    2016-10-01

    An imaging system is presented that is capable of far-detuned non-destructive imaging of a Bose-Einstein condensate with the signal proportional to the second spatial derivative of the density. Whilst demonstrated with application to $^{85}\\text{Rb}$, the technique generalizes to other atomic species and is shown to be capable of a signal to noise of ${\\sim}25$ at $1$GHz detuning with $100$ in-trap images showing no observable heating or atom loss. The technique is also applied to the observation of individual trajectories of stochastic dynamics inaccessible to single shot imaging. Coupled with a fast optical phase lock loop, the system is capable of dynamically switching to resonant absorption imaging during the experiment.

  18. Non-destructive photoacoustic imaging of metal surface defects

    NASA Astrophysics Data System (ADS)

    Jeon, Seungwan; Kim, Jeesu; Yun, Jong Pil; Kim, Chulhong

    2016-11-01

    The detection of metal surface defects is important in achieving the goals of product quality enhancement and manufacturing cost reduction. Identifying the defects with visual inspection is difficult, inaccurate, and time-consuming. Thus, several inspection methods using line cameras, magnetic field, and ultrasound have been proposed. However, identifying small defects on metal surfaces remains a challenge. To deal with this problem, we propose the use of photoacoustic imaging (PAI) as a new non-destructive imaging tool to detect metal surface defects. We successfully visualized two types of cracks (i.e., unclassified and seam cracks) in metal plate samples using PAI. In addition, we successfully extracted cracked edges from height-encoded photoacoustic maximum amplitude projection images using the Laplacian of Gaussian filtering method, and then, quantified the detected edges for a statistical analysis. We concluded that PAI can be useful in detecting metal surface defects reducing the defect rate and manufacturing cost during metal production.

  19. Non-destructive evaluation method employing dielectric electrostatic ultrasonic transducers

    NASA Technical Reports Server (NTRS)

    Yost, William T. (Inventor); Cantrell, Jr., John H. (Inventor)

    2003-01-01

    An acoustic nonlinearity parameter (.beta.) measurement method and system for Non-Destructive Evaluation (NDE) of materials and structural members novelly employs a loosely mounted dielectric electrostatic ultrasonic transducer (DEUT) to receive and convert ultrasonic energy into an electrical signal which can be analyzed to determine the .beta. of the test material. The dielectric material is ferroelectric with a high dielectric constant .di-elect cons.. A computer-controlled measurement system coupled to the DEUT contains an excitation signal generator section and a measurement and analysis section. As a result, the DEUT measures the absolute particle displacement amplitudes in test material, leading to derivation of the nonlinearity parameter (.beta.) without the costly, low field reliability methods of the prior art.

  20. Non-destructive evaluation of water ingress in photovoltaic modules

    DOEpatents

    Bora, Mihail; Kotovsky, Jack

    2017-03-07

    Systems and techniques for non-destructive evaluation of water ingress in photovoltaic modules include and/or are configured to illuminate a photovoltaic module comprising a photovoltaic cell and an encapsulant with at least one beam of light having a wavelength in a range from about 1400 nm to about 2700 nm; capture one or more images of the illuminated photovoltaic module, each image relating to a water content of the photovoltaic module; and determine a water content of the photovoltaic module based on the one or more images. Systems preferably include one or more of a light source, a moving mirror, a focusing lens, a beam splitter, a stationary mirror, an objective lens and an imaging module.

  1. Non-Destructive Classification Approaches for Equilbrated Ordinary Chondrites

    NASA Technical Reports Server (NTRS)

    Righter, K.; Harrington, R.; Schroeder, C.; Morris, R. V.

    2013-01-01

    Classification of meteorites is most effectively carried out by petrographic and mineralogic studies of thin sections, but a rapid and accurate classification technique for the many samples collected in dense collection areas (hot and cold deserts) is of great interest. Oil immersion techniques have been used to classify a large proportion of the US Antarctic meteorite collections since the mid-1980s [1]. This approach has allowed rapid characterization of thousands of samples over time, but nonetheless utilizes a piece of the sample that has been ground to grains or a powder. In order to compare a few non-destructive techniques with the standard approaches, we have characterized a group of chondrites from the Larkman Nunatak region using magnetic susceptibility and Moessbauer spectroscopy.

  2. Non-destructive monitoring of river embankments using GPR

    NASA Astrophysics Data System (ADS)

    di Prinzio, Monica; Bittelli, Marco; Castellarin, Attilio; Rossi Pisa, Paola

    2010-05-01

    Non-destructive investigations and controls of civil structures are improving day by day, however the scientific literature reports only a few documented cases of Ground Penetrating Radar (GPR) applications to the detection of voids and discontinuities in hydraulic defense structures such as river embankments and levee systems. GPR can assist decision making in a number of fields by enhancing our knowledge of subsurface features. We applied successfully GPR to the monitoring of river levees for the detectioning of animal burrows in river levees, which may trigger levee failures by piping. The manageability and the non-invasivity of GPR have resulted to be particularly suitable for this application. First because GPR is an extensive investigation method that enables one to rapidly cover a wide area, locating voids that are difficult and costly to locate using other intrusive methods. Second, GPR returns detailed information about the possible presence of voids and discontinuities within river embankments.

  3. Non-destructive Faraday imaging of dynamically controlled ultracold atoms

    SciTech Connect

    Gajdacz, Miroslav; Pedersen, Poul L.; Mørch, Troels; Hilliard, Andrew J.; Arlt, Jan; Sherson, Jacob F.

    2013-08-15

    We describe an easily implementable method for non-destructive measurements of ultracold atomic clouds based on dark field imaging of spatially resolved Faraday rotation. The signal-to-noise ratio is analyzed theoretically and, in the absence of experimental imperfections, the sensitivity limit is found to be identical to other conventional dispersive imaging techniques. The dependence on laser detuning, atomic density, and temperature is characterized in a detailed comparison with theory. Due to low destructiveness, spatially resolved images of the same cloud can be acquired up to 2000 times. The technique is applied to avoid the effect of shot-to-shot fluctuations in atom number calibration, to demonstrate single-run vector magnetic field imaging and single-run spatial imaging of the system's dynamic behavior. This demonstrates that the method is a useful tool for the characterization of static and dynamically changing properties of ultracold atomic clouds.

  4. Non-destructive diffraction enhanced imaging of seeds.

    PubMed

    Young, Lester W; Parham, Christopher; Zhong, Zhong; Chapman, Dean; Reaney, Martin J T

    2007-01-01

    Techniques that make possible the non-destructive continuous observation of plant anatomy and developmental processes provide novel insights into these phenomena. Non-destructive imaging of seeds was demonstrated using the synchrotron-based X-ray imaging technique, diffraction enhanced imaging (DEI). The seed images obtained had good contrast and definition, allowing anatomical structures and physiological events to be observed. Structures such as hypocotyl-root axes, cotyledons, seed coats, air cavities, and embryo-less Brassica napus L. seeds were readily observed using DEI. Embryo axes, scutella, pericarp furrows, coleoptiles, and roots were observable over a time-course in individual germinating Triticum aestivum L. caryopses. Novel anatomical and physiological observations were also made that would have been difficult to make continuously using other techniques. The physical principles behind DEI make it a unique imaging technique. Contrast in DEI is the result of X-ray refraction at the density differences occurring at tissue boundaries, scatter caused by regions containing ordered molecules such as cellulose fibres, and attenuation. Sectioning of samples and the infusion of stains or other contrast agents are not necessary. Furthermore, as high-energy X-rays are used (30-40 keV), little X-ray absorption occurs, resulting in low levels of radiation damage. Consequently, studies of developmental processes may be performed on individuals. Individual germinating B. napus and T. aestivum seeds were imaged at several time points without incurring any apparent radiation damage. DEI offers a unique way of examining plant anatomy, development, and physiology, and provides images that are complementary to those obtained through other techniques.

  5. Electrical and ionic conductivity effects on magic-angle spinning nuclear magnetic resonance parameters of CuI.

    PubMed

    Yesinowski, James P; Ladouceur, Harold D; Purdy, Andrew P; Miller, Joel B

    2010-12-21

    We investigate experimentally and theoretically the effects of two different types of conductivity, electrical and ionic, upon magic-angle spinning NMR spectra. The experimental demonstration of these effects involves (63)Cu, (65)Cu, and (127)I variable temperature MAS-NMR experiments on samples of γ-CuI, a Cu(+)-ion conductor at elevated temperatures as well as a wide bandgap semiconductor. We extend previous observations that the chemical shifts depend very strongly upon the square of the spinning-speed as well as the particular sample studied and the magnetic field strength. By using the (207)Pb resonance of lead nitrate mixed with the γ-CuI as an internal chemical shift thermometer we show that frictional heating effects of the rotor do not account for the observations. Instead, we find that spinning bulk CuI, a p-type semiconductor due to Cu(+) vacancies in nonstoichiometric samples, in a magnetic field generates induced AC electric currents from the Lorentz force that can resistively heat the sample by over 200 °C. These induced currents oscillate along the rotor spinning axis at the spinning speed. Their associated heating effects are disrupted in samples containing inert filler material, indicating the existence of macroscopic current pathways between micron-sized crystallites. Accurate measurements of the temperature-dependence of the (63)Cu and (127)I chemical shifts in such diluted samples reveal that they are of similar magnitude (ca. 0.27 ppm/K) but opposite sign (being negative for (63)Cu), and appear to depend slightly upon the particular sample. This relationship is identical to the corresponding slopes of the chemical shifts versus square of the spinning speed, again consistent with sample heating as the source of the observed large shift changes. Higher drive-gas pressures are required to spin samples that have higher effective electrical conductivities, indicating the presence of a braking effect arising from the induced currents produced by

  6. Electrical and ionic conductivity effects on magic-angle spinning nuclear magnetic resonance parameters of CuI

    NASA Astrophysics Data System (ADS)

    Yesinowski, James P.; Ladouceur, Harold D.; Purdy, Andrew P.; Miller, Joel B.

    2010-12-01

    We investigate experimentally and theoretically the effects of two different types of conductivity, electrical and ionic, upon magic-angle spinning NMR spectra. The experimental demonstration of these effects involves 63Cu, 65Cu, and 127I variable temperature MAS-NMR experiments on samples of γ-CuI, a Cu+-ion conductor at elevated temperatures as well as a wide bandgap semiconductor. We extend previous observations that the chemical shifts depend very strongly upon the square of the spinning-speed as well as the particular sample studied and the magnetic field strength. By using the 207Pb resonance of lead nitrate mixed with the γ-CuI as an internal chemical shift thermometer we show that frictional heating effects of the rotor do not account for the observations. Instead, we find that spinning bulk CuI, a p-type semiconductor due to Cu+ vacancies in nonstoichiometric samples, in a magnetic field generates induced AC electric currents from the Lorentz force that can resistively heat the sample by over 200 °C. These induced currents oscillate along the rotor spinning axis at the spinning speed. Their associated heating effects are disrupted in samples containing inert filler material, indicating the existence of macroscopic current pathways between micron-sized crystallites. Accurate measurements of the temperature-dependence of the 63Cu and 127I chemical shifts in such diluted samples reveal that they are of similar magnitude (ca. 0.27 ppm/K) but opposite sign (being negative for 63Cu), and appear to depend slightly upon the particular sample. This relationship is identical to the corresponding slopes of the chemical shifts versus square of the spinning speed, again consistent with sample heating as the source of the observed large shift changes. Higher drive-gas pressures are required to spin samples that have higher effective electrical conductivities, indicating the presence of a braking effect arising from the induced currents produced by rotating a

  7. Non-destructive monitoring of curing process in precast concrete

    NASA Astrophysics Data System (ADS)

    Aparicio, S.; Ranz, J.; Fernández, R.; Albert, V.; Fuente, J. V.; Hernández, M. G.

    2012-12-01

    Currently, the use of precast concrete elements has gained importance because it offers many advantages over site-cast concrete. A disadvantage of site-cast concrete is that its properties vary according to the manufacturing method, the environment and even the operator who carried out the mixing, pouring and implementation of the concrete. Precast concrete elements are manufactured in a controlled environment (typically referred to as a precast plant) and this reduces the shrinkage and creep. One of the key properties of precast concrete is the capability to gain compressive strength rapidly under the appropriate conditions. The compressive strength determines if the precast can be stripped from the form or manipulated. This parameter is measured using destructive testing over cylindrical or cubic samples. The quality control of precast is derived from the fracture suffered by these elements, resulting in a "pass or fail" evaluation. In most cases, the solution to this problem is to allow the material to cure for a few hours until it acquires sufficient strength to handle the precast element. The focus of this paper is the description of the research project "CUREND". This project aims to design a non-destructive methodology to monitor the curing process in precast concrete. The monitoring will be performed using wireless sensor networks.

  8. Non-destructive evaluation of mechanical properties of magnetic materials

    SciTech Connect

    Kankolenski, K.P.; Hua, S.Z.; Yang, D.X.; Hicho, G.E.; Swartzendruber, L.J.; Zang, Z.; Chopra, H.D.

    2000-07-01

    A magnetic-based non-destructive evaluation (NDE) method, which employs Barkhausen effect and measurement of the hysteresis loops, is used to correlate the magnetic and mechanical properties of ultra low carbon (ULC) steel. In particular, the NDE method was used to detect small deviations from linearity that occur in the stress-strain curve well below the 0.2% offset strain, and which generally defines the yield point in materials. Results show that three parameters: jumpsum and jumpsum rate (derived from the Barkhausen spectrum), and the relative permeability (derived from the B-H loops) varies sensitively with small permanent strains, and can be related to the plastic deformation in ULC steels. Investigation of micromagnetic structure revealed that plastic deformation leaves a residual stress state in the samples; the associated magneto-elastic energy makes the favorable easy axis of magnetization in a given grain to be the one that lies closest to the tensile axis. The consequence of this realignment of domains is that wall motion becomes intergranular in nature (as opposed to intragranular in unstrained samples). As a result, the more complex grain boundaries instead of dislocations, become the dominant pinning sites for domain walls. These observations provide a microscopic interpretation of the observed changes in the measured magnetic properties.

  9. Biomarkers: Non-destructive Method for Predicting Meat Tenderization.

    PubMed

    Singh, Arashdeep; Ahluwalia, Preeti; Rafiq, Aasima; Sharma, Savita

    2015-07-06

    Meat tenderness is the primary and most important quality attribute for the consumers worldwide. Tenderness is the process of breakdown of collagen tissue in meat to make it palatable. The earlier methods of tenderness evaluation like taste panels and shear force methods are destructive, time consuming and ill suited as they requires removing a piece of steak from the carcass for performing the test. Therefore, a non-destructive method for predicting the tenderness would be more desirable. The development of a meat quality grading and guarantee system through muscle profiling research can help to meet this demand. Biomarkers have the ability to identify if an exposure has occurred. Biomarkers of the meat quality are of prime importance for meat industry, which has ability to satisfy consumers' expectations. The biomarkers so far identified have been then sorted and grouped according to their common biological functions. All of them refer to a series of biological pathways including glycolytic and oxidative energy production, cell detoxification, protease inhibition and production of Heat Shock Proteins. On this basis, a detailed analysis of these metabolic pathways helps in identifying tenderization of meat having some domains of interest. It was, therefore, stressed forward that biomarkers can be used to determine meat tenderness. This review article summarizes the uses of several biomarkers for predicting the meat tenderness.

  10. A non-destructive method for dating human remains

    USGS Publications Warehouse

    Lail, Warren K.; Sammeth, David; Mahan, Shannon; Nevins, Jason

    2013-01-01

    The skeletal remains of several Native Americans were recovered in an eroded state from a creek bank in northeastern New Mexico. Subsequently stored in a nearby museum, the remains became lost for almost 36 years. In a recent effort to repatriate the remains, it was necessary to fit them into a cultural chronology in order to determine the appropriate tribe(s) for consultation pursuant to the Native American Grave Protection and Repatriation Act (NAGPRA). Because the remains were found in an eroded context with no artifacts or funerary objects, their age was unknown. Having been asked to avoid destructive dating methods such as radiocarbon dating, the authors used Optically Stimulated Luminescence (OSL) to date the sediments embedded in the cranium. The OSL analyses yielded reliable dates between A.D. 1415 and A.D. 1495. Accordingly, we conclude that the remains were interred somewhat earlier than A.D. 1415, but no later than A.D. 1495. We believe the remains are from individuals ancestral to the Ute Mouache Band, which is now being contacted for repatriation efforts. Not only do our methods contribute to the immediate repatriation efforts, they provide archaeologists with a versatile, non-destructive, numerical dating method that can be used in many burial contexts.

  11. Non-destructive characterization of archaeological glasses by neutron tomography

    NASA Astrophysics Data System (ADS)

    Fiori, F.; Giunta, G.; Hilger, A.; Kardjilov, N.; Rustichelli, F.

    2006-11-01

    The present work is carried out in the framework of a National Italian Project, whose aim is the assessment of innovative physical non-destructive techniques applied to archaeology. Towards this end, some archaeological artefacts have been studied by our group, in collaboration with the National Museum of Altino (VE) and EniTecnologie S.p.A. The objects come from the excavations in Altino, near Venice, where at least three different historical layers are present, corresponding to ages starting from approximately VII century B.C. In particular, in this work the results of neutron tomography investigations on three I-II century A.D. glass fragments are reported. The experiments were performed at the cold neutron radiography facility CONRAD at HMI (Berlin). For the 3D tomographical reconstruction of the sample, 200 projections were collected while the sample was rotated around a defined axis. The rotation interval was 180 degrees. The results show that the technique is able to reconstruct well the structural features of the investigated objects such as, in particular, highly absorbing zones and the presence of defects in the bulk.

  12. FIRST 100 T NON-DESTRUCTIVE MAGNET OUTER COIL SET

    SciTech Connect

    J. BACON; A. BACA; ET AL

    1999-09-01

    The controlled power outer coil set of the first 100 T non-destructive (100 T ND) magnet is described. This magnet will be installed as part of the user facility research equipment at the National High Magnetic Field laboratory (NHMFL) Pulsed Field Facility at Los Alamos National Laboratory. The 100 T ND controlled power outer coil set consists of seven nested, mechanically independent externally reinforced coils. These coils, in combination, will produce a 47 T platform field in a 225-mm diameter bore. Using inertial energy storage a synchronous motor/generator provides ac power to a set of seven ac-dc converters rated at 64 MW/80 MVA each. These converters energize three independent coil circuits to create 170 MJ of field energy in the outer coil set at the platform field of 47 T. Each coil consists of a multi-layer winding of high strength conductor supported by an external high strength stainless steel shell. Coils with the highest magnetic loads will utilize a reinforcing shell fabricated from highly cold worked 301 stainless steel strip. The autofrettage conditioning method will be used to pre-stress the coils and thereby limit conductor and reinforcement strains to the elastic range. The purpose of pre-stressing the coils is to attain a design life of 10,000 full field pulses. The operation and conditioning of the coil set will be described along with special features of its design, magnetic and structural analyses and construction.

  13. Non-destructive testing of the MEGAPIE target

    NASA Astrophysics Data System (ADS)

    Dai, Y.; Wohlmuther, M.; Boutellier, V.; Hahl, S.; Lagotzki, A.; Leu, H.; Linder, H. P.; Schwarz, R.; Spahr, A.; Zanini, L.; Kuster, D.; Gavillet, D.; Wagner, W.

    2016-01-01

    Non-destructive testing (NDT) is one important part of the post-irradiation examination (PIE) of the MEGAPIE target. It includes visual inspection and ultrasonic measurement of the beam window of the T91 LBE container and gamma mapping of the beam window of the AlMg3 safety-container. The visual inspection showed no visible failure in the proton beam window area of the T91 LBE container. The ultrasonic measurement demonstrated no detectable change in the wall thickness of the T91 beam window, which implies no severe corrosion effect induced by flowing LBE during the four-month irradiation period. The gamma mapping provided the distribution of 22Na, a spallation product, in the proton beam window area of the AlMg3 safety-container. The result was used to evaluate the accumulated proton fluence distribution profile, the input data for determining irradiation parameters. A maximum proton fluence of 1.9 × 1025 p/m2 was deduced. The corresponding displacement damage degree in the T91 beam window was 7.1 dpa.

  14. Non-destructive investigation of thermoplastic reinforced composites

    SciTech Connect

    Hassen, Ahmed; Taheri, Hossein; Vaidya, Uday

    2016-05-09

    This paper studies various manufacturing defects in glass fiber/Polypropylene (PP) composite parts and their methods of detection. Foreign Object Inclusion (FOI) of different shapes, sizes, and materials were placed in a glass fiber/PP panel made by compression molding. The paper aims to characterize the fiber orientation and fiber related defects such as fiber waviness in the composite specimen. Comprehensive investigation for different Non Destructive Evaluation (NDE) techniques, namely X-ray radiography and Ultrasonic Testing (UT) techniques to trace and characterize the embedded defects and the composite texture are presented. Conventional X-ray radiography successfully identified the fiber orientation in two dimension (2-D) plane; however, information for the sample depth was not captured. The radiography techniques showed low relative errors for the defect size measurements (maximum error was below 9.5%) when compared to the ultrasonic techniques. Ultrasonic techniques were able to map all the embedded artificial defects. Phase Array (PA) ultrasonic technique was able to precisely locate the FOI in the glass fiber/PP specimen. Nerveless, the shape and size of the defects were not accurately determined due to the high signal attenuation and distortion characteristics of the E-glass fiber.

  15. Non-Destructive Evaluation (NDE) Applications of THz Radiation

    NASA Astrophysics Data System (ADS)

    Zimdars, David

    2005-03-01

    The technology and applications of time domain terahertz (THz) imaging to non-destructive evaluation (NDE) will be discussed. THz imaging has shown great promise in 2 and 3 dimensional non-contact inspection of non-conductive materials such as plastics, foam, composites, ceramics, paper, wood and glass. THz imaging employs safe low power non-ionizing electromagnetic pulses, with lateral resolution < 200 um, and depth resolution < 50 um. THz pulses can be analyzed spectroscopically to reveal chemical content. Recently, highly integrated turn-key THz imaging systems have been introduced commercially. We will demonstrate the detection of voids and disbonds intentionally incorporated within the sprayed on foam insulation of a space shuttle external tank mock-up segments. An industrially hardened THz scanning system which has been deployed to scan the space shuttle tank with small remote transceiver will be described. Additional terahertz security imaging applications for the detection of weapons and explosives will also be discussed, as well as the application of terahertz sensors for high speed industrial process monitoring and quality control.

  16. Non-destructive sub-THz CW imaging

    NASA Astrophysics Data System (ADS)

    Karpowicz, Nicholas; Zhong, Hua; Xu, Jingzhou; Lin, Kuang-I.; Hwang, Jenn-Shyong; Zhang, Xi-Cheng

    2005-03-01

    A simple, compact CW sub-THz imaging system, utilizing a 0.2 and 0.6 THz Gunn diode source is presented. A silicon beam lead diode detector and a Golay cell are used for the detection. Various results are presented, which show that the CW THz imaging modality is suitable for diverse applications, such as non-destructive testing and security. The key components of the system include the Gunn diode assembly, an optical chopper, a polyethylene lens, a detector, a lock-in amplifier, and two translation stages. The beam from the Gunn diode is focused on the sample being imaged by the polyethylene lens, the transmitted or reflected beam is measured by the detector. The energy transmitted through the sample at each point in the plane of the sample is detected. Since the system has relatively few components compared to pulsed THz imaging systems, it is less expensive and easier to design and operate, although it does not provide depth or spectral information about the sample. Since no time-delay scans take place, scanning can be done quickly compared to a time-domain system, limited by the maximum velocity of the translation stages and response of the detectors. It provides information about the macroscopic features of hidden structures within materials that are transparent to sub THz radiation, such as space shuttle insulating foam, articles of clothing, and luggage.

  17. Non-destructive acoustic defect detection in drug tablets.

    PubMed

    Akseli, Ilgaz; Mani, Girindra N; Cetinkaya, Cetin

    2008-08-06

    For physical defect detection in drug tablets, a non-destructive and non-contact technique based on air coupled excitation and interferometric detection is presented. Physical properties and mechanical integrity of drug tablets can often affect their therapeutic and structural functions. The monitoring for defects and the characterization of tablet mechanical properties therefore have been of practical interest for solid oral dosage forms. The presented monitoring approach is based on the analysis of the transient vibrational responses of an acoustically excited tablet in both in temporal and spectral domains. The pulsed acoustic field exciting the tablet is generated by an air-coupled transducer. Using a laser vibrometer, the out-of-plane vibrational transient response of the tablet is detected and acquired in a non-contact manner. The physical state of the tablet is evaluated based on the spectral properties of these transient responses. In the current study, the effectiveness of three types of simple similarity measures is evaluated for their potential uses as defect detection norms, and for their potential use in quantifying the extent of tablet defect is discussed. It is found that these quantities can not only be used for identification of defective tablets, but could also provide a measure for the extent of the damage.

  18. Non-destructive compositional analysis of historic organ reed pipes

    NASA Astrophysics Data System (ADS)

    Manescu, A.; Fiori, F.; Giuliani, A.; Kardjilov, N.; Kasztovszky, Z.; Rustichelli, F.; Straumal, B.

    2008-03-01

    In order to be able to reproduce historic organ reed pipes, a bulk non-destructive chemical composition analysis was performed on the tongues and shallots, focusing mainly on the ratio between copper and zinc and on the presence of lead. Prompt gamma activation analysis results allowed us to observe for the first time that the ratio between the two main components of the brass alloy changed from Cu:Zn = 3:1 for the old tongues and shallots to Cu:Zn = 2:1 around the middle of the 18th century, which is typical also for the modern alloys offered to the organ builders nowadays. We also discovered that the Pb content in the old historic brass alloy diminished until the middle of 18th century when the brass alloy became mainly Pb free. The non-uniform lead distribution inside one of the shallots obtained from a prompt gamma activation analysis (PGAA) experiment was studied by neutron tomography. It gave us a three-dimensonal (3D) distribution of the lead inclusions inside the shallots. The lead particles are concentrated towards the base of the shallot.

  19. Non-Destructive Assay of Curium Contaminated Transuranic Waste Drums

    SciTech Connect

    Foster, L.A.

    1998-11-01

    At the Plutonium Facility at Los Alamos National Laboratory, a series of non-destructive assays were performed on five transuranic waste (TRU) drums containing non-plutonium scrap metal that was potentially contaminated with weapons grade plutonium and trace quantities of curium. Typically, waste drums containing metal matrices are assayed for plutonium content using passive neutron coincidence counting techniques. The presence of trace quantities of Cm-244 prevents this type of analysis because of the strong coincidence signal created by spontaneous fission of Cm-244. To discriminate between the plutonium and curium materials present, an active neutron measurement technique was used. A Cf shuffler designed for measurement of uranium bearing materials was calibrated for plutonium in the active mode. The waste drums were then assayed for plutonium content in the shuffler using the active-mode calibration. The curium contamination levels were estimated from the difference between the active-mode measurement in the shuffler and a passive assay in a neutron coincidence counter. Far field gamma-ray measurements were made to identify additional radioactive contaminants and to corroborate the plutonium measurement results obtained from the active-mode assay. This report describes in detail the measurement process used for characterization of these waste drums. The measurement results and the estimated uncertainty will be presented.

  20. Non-destructive investigation of thermoplastic reinforced composites

    SciTech Connect

    Hassen, Ahmed; Taheri, Hossein; Vaidya, Uday

    2016-05-09

    This paper studies various manufacturing defects in glass fiber/Polypropylene (PP) composite parts and their methods of detection. Foreign Object Inclusion (FOI) of different shapes, sizes, and materials were placed in a glass fiber/PP panel made by compression molding. The paper aims to characterize the fiber orientation and fiber related defects such as fiber waviness in the composite specimen. Comprehensive investigation for different Non Destructive Evaluation (NDE) techniques, namely X-ray radiography and Ultrasonic Testing (UT) techniques to trace and characterize the embedded defects and the composite texture are presented. Conventional X-ray radiography successfully identified the fiber orientation in two dimension (2-D) plane; however, information for the sample depth was not captured. The radiography techniques showed low relative errors for the defect size measurements (maximum error was below 9.5%) when compared to the ultrasonic techniques. Ultrasonic techniques were able to map all the embedded artificial defects. Phase Array (PA) ultrasonic technique was able to precisely locate the FOI in the glass fiber/PP specimen. Nerveless, the shape and size of the defects were not accurately determined due to the high signal attenuation and distortion characteristics of the E-glass fiber.

  1. Evaluation of Transportation Options for Intermediate Non-destructive Examinations

    SciTech Connect

    Case, Susan; Hoggard, Gary

    2013-11-01

    Idaho National Laboratory (INL) shipments of irradiated experiments from the Advanced Test Reactor (ATR) to the Hot Fuels Examination Facility (HFEF) have historically been accomplished using the General Electric Model 2000 (GE 2000) Type B shipping container. Battelle Energy Alliance (BEA) concerns regarding the future availability and leasing and handling costs associated with the GE 2000 cask have warranted an evaluation of alternative shipping options. One or more of these shipping options may be utilized to perform non-destructive examinations (NDE) such as neutron radiography and precision gamma scans of irradiated experiments at HFEF and then return the experiments to ATR for further irradiation, hereafter referred to as “intermediate NDE.” This evaluation includes transportation options for intermediate NDE using the GE 2000 cask, BEA Research Reactor (BRR) package, Dry Transfer Cubicle (DTC) insert, and the General Electric Model 100 (GE 100) cask. The GE 2000 cask is the only Type B shipping container currently in use for shipments of irradiated material (exceeding Type A quantities) from ATR to HFEF; therefore it is included as one of the four shipping options in this evaluation. Cost and schedule estimates are provided for performing neutron radiography and precision gamma scans of a five-capsule drop-in-type ATR experiment for each transportation option. All costs provided in this evaluation are rough order-of-magnitude costs based on input from knowledgeable vendor employees and individuals at INL facilities.

  2. A novel thermosonic imaging system for non-destructive testing

    NASA Astrophysics Data System (ADS)

    Willey, C. L.; Xiang, D.; Long, M.

    2017-02-01

    Thermosonic infrared (Sonic IR) imaging is a new non-destructive testing (NDT) technique that uses high-frequency sonic excitation together with infrared (IR) detection to image surface and subsurface defects. A conventional Sonic IR imaging system employs an ultrasonic welder, which is designed to operate at a single frequency. This single frequency ultrasonic source has been found to yield a "blind zone" for NDT due to the formation of standing waves inside the test piece. To overcome this limitation, a spring loaded ultrasonic transducer was used to generate the desired multi-frequency acoustic chaos in the test object [1]. The limitation of the spring loaded ultrasonic transducer is its repeatability and reproducibility for field applications. In this work, we present the development of a novel thermosonic imaging system, which is capable of exciting the ultrasonic transducer at difflerent frequencies for thermosonic NDT to overcome the limitations associated with a single frequency power source as well as the spring loaded transducer design. A comparison of experimental results will be made between the single frequency and the developed multi-frequency thermosonic NDT systems.

  3. Non-destructive investigation of thermoplastic reinforced composites

    DOE PAGES

    Hassen, Ahmed; Taheri, Hossein; Vaidya, Uday

    2016-05-09

    This paper studies various manufacturing defects in glass fiber/Polypropylene (PP) composite parts and their methods of detection. Foreign Object Inclusion (FOI) of different shapes, sizes, and materials were placed in a glass fiber/PP panel made by compression molding. The paper aims to characterize the fiber orientation and fiber related defects such as fiber waviness in the composite specimen. Comprehensive investigation for different Non Destructive Evaluation (NDE) techniques, namely X-ray radiography and Ultrasonic Testing (UT) techniques to trace and characterize the embedded defects and the composite texture are presented. Conventional X-ray radiography successfully identified the fiber orientation in two dimension (2-D)more » plane; however, information for the sample depth was not captured. The radiography techniques showed low relative errors for the defect size measurements (maximum error was below 9.5%) when compared to the ultrasonic techniques. Ultrasonic techniques were able to map all the embedded artificial defects. Phase Array (PA) ultrasonic technique was able to precisely locate the FOI in the glass fiber/PP specimen. Nerveless, the shape and size of the defects were not accurately determined due to the high signal attenuation and distortion characteristics of the E-glass fiber.« less

  4. Non-Destructive Evaluation of Materials via Ultraviolet Spectroscopy

    NASA Technical Reports Server (NTRS)

    Pugel, Betsy

    2008-01-01

    A document discusses the use of ultraviolet spectroscopy and imaging for the non-destructive evaluation of the degree of cure, aging, and other properties of resin-based composite materials. This method can be used in air, and is portable for field use. This method operates in reflectance, absorbance, and luminescence modes. The ultraviolet source is used to illuminate a composite surface of interest. In reflectance mode, the reflected response is acquired via the imaging system or via the spectrometer. The spectra are analyzed for organic compounds (conjugated organics) and inorganic compounds (semiconducting band-edge states; luminescing defect states such as silicates, used as adhesives for composite aerospace applications; and metal oxides commonly used as thermal coating paints on a wide range of spacecraft). The spectra are compared with a database for variation in conjugation, substitution, or length of molecule (in the case of organics) or band edge position (in the case of inorganics). This approach is useful in the understanding of material quality. It lacks the precision in defining the exact chemical structure that is found in other materials analysis techniques, but it is advantageous over methods such as nuclear magnetic resonance, infrared spectroscopy, and chromatography in that it can be used in the field to assess significant changes in chemical structure that may be linked to concerns associated with weaknesses or variations in structural integrity, without disassembly of or destruction to the structure of interest.

  5. Non-destructive evaluation of anchorage zones by ultrasonics techniques.

    PubMed

    Kharrat, M; Gaillet, L

    2015-08-01

    This work aims to evaluate the efficiency and reliability of two Non-Destructive Testing (NDT) methods for damage assessment in bridges' anchorages. The Acousto-Ultrasonic (AU) technique is compared to classical Ultrasonic Testing (UT) in terms of defect detection and structural health classification. The AU technique is firstly used on single seven-wire strands damaged by artificial defects. The effect of growing defects on the waves traveling through the strands is evaluated. Thereafter, three specimens of anchorages with unknown defects are inspected by the AU and UT techniques. Damage assessment results from both techniques are then compared. The structural health conditions of the specimens can be then classified by a damage severity criterion. Finally, a damaged anchorage socket with mastered defects is controlled by the same techniques. The UT allows the detection and localization of damaged wires. The AU technique is used to bring out the effect of defects on acoustic features by comparing a healthy and damaged anchorage sockets. It is concluded that the UT method is suitable for local and crack-like defects, whereas the AU technique enables the assessment of the global structural health of the anchorage zones.

  6. Data fusion for automated non-destructive inspection

    PubMed Central

    Brierley, N.; Tippetts, T.; Cawley, P.

    2014-01-01

    In industrial non-destructive evaluation (NDE), it is increasingly common for data acquisition to be automated, driving a recent substantial increase in the availability of data. The collected data need to be analysed, typically necessitating the painstaking manual labour of a skilled operator. Moreover, in automated NDE a region of an inspected component is typically interrogated several times, be it within a single data channel due to multiple probe passes, across several channels acquired simultaneously or over the course of repeated inspections. The systematic combination of these diverse readings is recognized to offer an opportunity to improve the reliability of the inspection, but is not achievable in a manual analysis. This paper describes a data-fusion-based software framework providing a partial automation capability, allowing component regions to be declared defect-free to a very high probability while readily identifying defect indications, thereby optimizing the use of the operator's time. The system is designed to applicable to a wide range of automated NDE scenarios, but the processing is exemplified using the industrial ultrasonic immersion inspection of aerospace turbine discs. Results obtained for industrial datasets demonstrate an orders-of-magnitude reduction in false-call rates, for a given probability of detection, achievable using the developed software system. PMID:25002828

  7. 1H-detected 1H- 1H correlation spectroscopy of a stereo-array isotope labeled amino acid under fast magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Takahashi, Hiroki; Kainosho, Masatsune; Akutsu, Hideo; Fujiwara, Toshimichi

    2010-04-01

    The combined use of selective deuteration, stereo-array isotope labeling (SAIL), and fast magic-angle spinning effectively suppresses the 1H-1H dipolar couplings in organic solids. This method provided the high-field 1H NMR linewidths comparable to those achieved by combined rotation and multiple-pulse spectroscopy. This technique was applied to two-dimensional 1H-detected 1H-1H polarization transfer CHH experiments of valine. The signal sensitivity for the 1H-detected CHH experiments was greater than that for the 13C-detected 1H-1H polarization transfer experiments by a factor of 2-4. We obtained the 1H-1H distances in SAIL valine by CHH experiments with an accuracy of about 0.2 Å by using a theory developed for 1H-1H polarization transfer in 13C-labeled organic compounds.

  8. High resolution magic angle spinning NMR spectroscopy reveals that pectoralis muscle dystrophy in chicken is associated with reduced muscle content of anserine and carnosine.

    PubMed

    Sundekilde, Ulrik K; Rasmussen, Martin K; Young, Jette F; Bertram, Hanne Christine

    2017-02-15

    Increased incidences of pectoralis muscle dystrophy are observed in commercial chicken products, but the muscle physiological causes for the condition remain to be identified. In the present study a high-resolution magic angle spinning (HR-MAS) proton ((1)H) NMR spectroscopic examination of intact pectoralis muscle samples (n=77) were conducted to explore metabolite perturbations associated with the muscle dystrophy condition for the very first time. Both in chicken with an age of 21 and 31days, respectively, pectoralis muscle dystrophy was associated with a significantly lower content of anserine (p=0.034), carnosine (p=0.019) and creatine (p=0.049). These findings must be considered intriguing as they corroborate that characteristic muscle di-peptides composed of β-alanine and histidine derivatives such as anserine are extremely important in homeostasis of contractile muscles as a results of their role as buffering, anti-oxidative, and anti-glycation capacities.

  9. An NMR thermometer for cryogenic magic-angle spinning NMR: the spin-lattice relaxation of (127)I in cesium iodide.

    PubMed

    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 (79)Br in KBr powder can be useful for measuring sample temperature under MAS over a wide temperature range (20-296 K). However the value of T(1) exceeds 3 min at temperatures below 20K, which is inconveniently long. In this communication, we show that the spin-lattice relaxation time constant of (127)I in CsI powder can be used to accurately measure sample temperature under MAS within a reasonable experimental time down to 10 K.

  10. Characterization of cromolyn sodium hydrates and its formulation by (23) Na-multiquantum and magic-angle spinning nuclear magnetic resonance spectroscopy.

    PubMed

    Umino, Makoto; Higashi, Kenjirou; Masu, Hyuma; Limwikrant, Waree; Yamamoto, Keiji; Moribe, Kunikazu

    2013-08-01

    We characterized cromolyn sodium (CS) hydrates and evaluated their molecular states in low-dose formulations using Na-multiquantum magic-angle spinning (MQMAS) nuclear magnetic resonance (NMR) analysis. Two CS hydrates, low-water-content hydrated form and high-water-content hydrated form containing 2-3 and 5-6 hydrates, respectively, were prepared by humidification. Single-crystal X-ray diffraction and powder X-ray diffraction analysis revealed that these CS hydrates contained sodium channel structures and that water molecules were adsorbed on the sodium nucleus. (13) C-cross-polarization/MAS NMR spectra of these hydrates revealed similar results, confirming that the water molecules were adsorbed not on the cromolyn skeletons but mainly on the sodium nucleus. In contrast, (23) Na-MQMAS NMR analysis allowed us to clearly distinguish these hydrates without discernible effects from quadrupolar interaction. Thus, MQMAS NMR analysis is a valuable tool for evaluating salt drugs and their formulations.

  11. Crocus sativus Petals: Waste or Valuable Resource? The Answer of High-Resolution and High-Resolution Magic Angle Spinning Nuclear Magnetic Resonance.

    PubMed

    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.

  12. Direct observation of cell wall glucans in whole cells of Saccharomyces cerevisiae by magic-angle spinning 13C-NMR.

    PubMed

    Krainer, E; Stark, R E; Naider, F; Alagramam, K; Becker, J M

    1994-12-01

    Intact cells of Saccharomyces cerevisiae were examined as an aqueous paste by 13C-nmr spectroscopy with direct polarization and magic-angle spinning. The spectra obtained were highly resolved, showing numerous resonances in the 60-105 ppm range that were assigned to carbons of a liquid-like domain of the cell wall glucan. Assignments were confirmed by running the spectrum of S. cerevisiae in which the cell wall glucans were labeled with [13C] by feeding the cell [13C]galactose. The spectra indicate that the glucan in the cell wall of intact S. cerevisiae assumes a helical conformation and suggest that strain 17A fed with galactose preferentially incorporates the resulting glucose into beta (1-->3)-linkages.

  13. Low-power broadband homonuclear dipolar recoupling without decoupling: Double-quantum 13C NMR correlations at very fast magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Teymoori, Gholamhasan; Pahari, Bholanath; Stevensson, Baltzar; Edén, Mattias

    2012-09-01

    We report novel symmetry-based radio-frequency (rf) pulse sequences for efficient excitation of double-quantum (2Q) coherences under very fast (>60 kHz) magic-angle spinning (MAS) conditions. The recursively generated pulse-scheme series, R22p1R22p-1(p=1,2,3,…), offers broadband 13C-13C recoupling in organic solids at a very low rf power. No proton decoupling is required. A high-order average Hamiltonian theory analysis reveals a progressively enhanced resonance-offset compensation for increasing p, as verified both by numerical simulations and 2Q filtration NMR experiments on 13C2-glycine, [2,3-13C2]alanine, and [U-13C]tyrosine at 14.1 T and 66 kHz MAS, where the pulse schemes with p⩾3 compare favorably to current state-of-the-art recoupling options.

  14. Proton-nitrogen-14 overtone two-dimensional correlation NMR spectroscopy of solid-sample at very fast magic angle sample spinning.

    PubMed

    Nishiyama, Yusuke; Malon, Michal; Gan, Zhehong; Endo, Yuki; Nemoto, Takahiro

    2013-05-01

    (1)H-(14)N overtone (OT) heteronuclear multiple quantum coherence (HMQC) experiment at very fast magic angle spinning (MAS) is reported. The (14)N OT coherence is excited and reconverted by (14)N OT pulses at twice the (14)N Larmor frequency. The OT coherence is free from the first order quadrupolar broadening. MAS further removes the broadening due to chemical shift anisotropy (CSA). With a small 0.75 mm MAS rotor and coil system, very fast MAS up to 90 kHz and very strong rf field are achieved, enhancing the sensitivity of indirect (14)N OT observation via protons. In comparison with (1)H-(14)N double-quantum HMQC, an enhancement factor of 1.8 is obtained for glycine with the (14)N OT irradiation. The bandwidth in the (14)N OT dimension is limited due to long (14)N OT pulses. Copyright © 2013 Elsevier Inc. All rights reserved.

  15. Decoupling and recoupling using continuous-wave irradiation in magic-angle-spinning solid-state NMR: A unified description using bimodal Floquet theory

    SciTech Connect

    Ernst, Matthias; Samoson, Ago; Meier, Beat H.

    2005-08-08

    The application of two or more different time-dependent coherent perturbations with, in general, incommensurable frequencies occurs quite commonly in NMR experiments. Here we develop a unified description of the entire class of experiments using bimodal Floquet theory and van Vleck-Primas perturbation theory. This treatment leads to a time-independent effective Hamiltonian in Hilbert space and can be looked at as a generalization of average Hamiltonian theory to several incommensurate time dependencies. As a prototype experiment we treat the application of continuous-wave (cw) radio-frequency irradiation in combination with magic-angle sample spinning. Practically relevant examples of this type of experiments are heteronuclear spin decoupling and recoupling experiments using cw irradiation, e.g., rotary-resonance recoupling. Perturbations up to the third order must be taken into account to explain all experimentally observed resonance conditions.

  16. A High-Resolution Magic Angle Spinning NMR Study of the Enantiodiscrimination of 3,4-Methylenedioxymethamphetamine (MDMA) by an Immobilized Polysaccharide-Based Chiral Phase

    PubMed Central

    Paixão, Márcio W.; Lourenço, Tiago C.

    2016-01-01

    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. PMID:27668862

  17. 1H High Resolution Magic-Angle Coil Spinning (HR-MACS) - NMR Metabolic Profiling of whole Saccharomyces cervisiae cells: A Demonstrative Study

    NASA Astrophysics Data System (ADS)

    Wong, Alan; Boutin, Celine; Aguiar, Pedro

    2014-06-01

    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.

  18. Geophysical Methods for Non-Destructive Testing in Civil Engineering

    NASA Astrophysics Data System (ADS)

    Niederleithinger, E.

    2013-12-01

    Many non-destructive testing (NDT) methods for civil engineering (e. g. ultrasonics, radar) are similar to geophysical techniques. They just differ in scale, material under investigation and vocabulary used. In spite of the fact that the same principles of physics and mathematics apply to both fields, exchange has been limited in the past. But since a few years more and more geophysical knowledge is used in civil engineering. One of the focal points in research is to improve ultrasonic testing of concrete to be able to image the inside even of large, complex structures and to detect any deterioration as early as possible. One of the main issues is the heterogeneity of concrete, including aggregates, reinforcement, cracks and many other features. Our current research focuses on three points. One is the application of state of the art geophysical migration techniques as Reverse Time Migration (RTM) to image vertical faces or the backside of voids and ducts in thick concrete structures, which isn't possible with conventional techniques used in NDT. Second, we have started to use seismic interferometric techniques to interpolate ultrasonic traces, which can't be measured directly for technical reasons. Third, we are using coda wave interferometry to detect concrete degradation due to load, fatigue, temperature or other influences as early as possible. Practical examples of the application of these techniques are given and potential future research directions will be discussed. It will be shown, how a subset of these techniques can be used for innovative monitoring systems for civil infrastructure. Imaging the interior of a concrete body by ultrasonics and reverse time migration(simulated data).

  19. Non Destructive Analysis of Fsw Welds using Ultrasonic Signal Analysis

    NASA Astrophysics Data System (ADS)

    Pavan Kumar, T.; Prabhakar Reddy, P.

    2017-08-01

    Friction Stir Welding is an evolving metal joining technique and is mostly used in joining materials which cannot be easily joined by other available welding techniques. It is a technique which can be used for welding dissimilar materials also. The strength of the weld joint is determined by the way in which these material are mixing with each other, since we are not using any filler material for the welding process the intermixing has a significant importance. The complication with the friction stir welding process is that there are many process parameters which effect this intermixing process such as tool geometry, rotating speed of the tool, transverse speed etc., In this study an attempt is made to compare the material flow and weld quality of various weldments by changing the parameters. Ultrasonic signal Analysis is used to characterize the microstructure of the weldments. use of ultrasonic waves is a non destructive, accurate and fast way of characterization of microstructure. In this method the relationship between the ultrasonic measured parameters and microstructures are evaluated using background echo and backscattered signal process techniques. The ultrasonic velocity and attenuation measurements are dependent on the elastic modulus and any change in the microstructure is reflected in the ultrasonic velocity. An insight into material flow is essential to determine the quality of the weld. Hence an attempt is made in this study to know the relationship between tool geometry and the pattern of material flow and resulting weld quality the experiments are conducted to weld dissimilar aluminum alloys and the weldments are characterized using and ultra Sonic signal processing. Characterization is also done using Scanning Electron Microscopy. It is observed that there is a good correlation between the ultrasonic signal processing results and Scanning Electron Microscopy on the observed precipitates. Tensile tests and hardness tests are conducted on the

  20. Non-destructive detection of corrosion for life management

    NASA Astrophysics Data System (ADS)

    Bruce, David A.

    1995-01-01

    In recent years, aircraft operators have been driven to increased use of Non-Destructive Evaluation (NDE) to ensure airworthiness during life extensions for ageing aircraft or as an integral part of a damage tolerant lifting philosophy. Major airframe static and fatigue tests are routinely used to highlight problem areas on airframes where design limitations or changes of usage may lead to early failures. The results of such tests become progressively less reliable as the age of the airframe increases and the operating conditions diverge from those under which the tests were conducted. Increased inspection, whether by visual or other means is usually the only alternative to wholesale refurbishment or replacement of aircraft or components. Almost all of the development to date of NDE techniques for corrosion detection and characterization has been concentrated on existing airframe materials, principally Aluminum alloys and steels. The current capabilities of corrosion detection techniques will be reviewed and current research aimed at areas where there is a requirement for improved detection capability will be described. New materials, such as Polymer Matrix Composites, will experience different types of 'corrosive' deterioration. The capability of NDE methods to detect material degradation in new composite materials will be discussed. Finally, reliance on NDE, choice of NDE technique and optimal scheduling of inspections all require an assessment of the reliability of NDE methods. It will be shown that a range of NDE techniques with differing capabilities and characteristics will be required to ensure compatibility with maintenance schedules if full use is to be made of NDE for life management of structures which may be subject to corrosion.

  1. Rapid, non-destructive coral paleothermometry by synchrotron XR

    NASA Astrophysics Data System (ADS)

    Tangri, N.; Mehta, A.; Marks, R.; Dunbar, R. B.

    2016-12-01

    We present advances in the use of synchrotron x-ray fluorescence (XRF) to recover climate signals from coral exoskeleton. Corals record sea surface temperature (SST), salinity, and other environmental conditions in the density and composition of their exoskeletons; in particular, SST is reflected in both the Sr/Ca ratio and the annual density banding. Synchrotron XRF has previously been used to examine the fine-scaled variability of Sr concentrations in the exoskeleton structure, but has not yet yielded any long-term SST reconstructions. Modern XRF techniques allow the detection of sub-ppm trace element concentrations and appear ideally suited to long climate reconstructions, as they are non-destructive, high-resolution (250 um) and potentially quite rapid ( 40 years of sample in 24 hours of instrument time). The low Sr content of the coral and its low change in concentration require a high brightness synchrotron source to generate a high signal-to-background ratio. However, difficulties arise from the local heterogeneity of Sr that is unrelated to environmental conditions. These variations of biological origin in Sr concentrations often mask the smaller-amplitude, annual and interannual SST signals. The challenge is to normalize the local variability in order to extract the climate signal. Other techniques have normalized against Ca, but in XRF the Ca signal is sensitive to only the surface 50 um of material, whereas the Sr signal comes from 1mm, so the values are not comparable. Instead, we normalize against density as calculated from beam transmission. We also explore the use of Rb normalization to filter out collection artifacts. Both Sr and Rb show strong annual signals and interesting departures from the density signal. Finally, we pair the XRF results with δ18O measurements to recover a convincing record of SST variation. Although challenges remain, we believe that synchrotron XRF techniques hold considerable promise to rapidly and accurately recover

  2. Magic Physics?

    ERIC Educational Resources Information Center

    Featonby, David

    2010-01-01

    This article examines several readily available "magic tricks" which base their "trickery" on physics principles, and questions the use of the word "magic" in the 21st century, both in popular children's science and in everyday language. (Contains 18 figures.)

  3. Magic Physics?

    ERIC Educational Resources Information Center

    Featonby, David

    2010-01-01

    This article examines several readily available "magic tricks" which base their "trickery" on physics principles, and questions the use of the word "magic" in the 21st century, both in popular children's science and in everyday language. (Contains 18 figures.)

  4. Accuracy of Non-Destructive Testing of PBRs to Estimate Fragilities

    NASA Astrophysics Data System (ADS)

    Brune, J. N.; Brune, R.; Biasi, G. P.; Anooshehpoor, R.; Purvance, M.

    2011-12-01

    Prior studies of Precariously Balanced Rocks (PBRs) have involved various methods of documenting rock shapes and fragilities. These have included non-destructive testing (NDT) methods such as photomodeling, and potentially destructive testing (PDT) such as forced tilt tests. PDT methods usually have the potential of damaging or disturbing the rock or its pedestal so that the PBR usefulness for future generations is compromised. To date we have force-tilt tested approximately 28 PBRs, and of these we believe 7 have been compromised. We suggest here that given other inherent uncertainties in the current methodologies, NDT methods are now sufficiently advanced as to be adequate for the current state of the art use for comparison with Ground Motion Prediction Equations (GMPEs) and seismic hazard maps (SHMs). Here we compare tilt-test static toppling estimates to three non-destructive methods: (1) 3-D photographic modeling (2) profile analysis assuming the rock is 2-D, and (3) expert judgments from photographs. 3-D modeling uses the commercial Photomodeler program and photographs in the field taken from numerous directions around the rock. The output polyhedral shape is analyzed in Matlab determine the center of mass and in Autocad to estimate the static overturning angle alpha. For the 2-D method we chose the photograph in profile looking perpendicular to the estimated direction of toppling. The rock is outlined as a 2-D object in Matlab. Rock dimensions, rocking points, and a vertical reference are supplied by the photo analyst to estimate the center of gravity and static force overturning angles. For the expert opinion method we used additional photographs taken from different directions to improve the estimates of the center of mass and the rocking points. We used 7 rocks for comparisons. The error in estimating tan alpha from 3-D modeling is about 0.05. For 2-D estimates an average error is about 0.1 (?). For expert opinion estimates the error is about 0.06. For

  5. Non-Destructive Damping Measurement for Wafer-Level Packaged Microelectromechanical System (MEMS) Acceleration Switches

    DTIC Science & Technology

    2014-09-01

    logarithmic decrement of those amplitudes.7,8 Experiments that did not rely on resonant frequencies used capacitance measurements or pressure sensors to relate...Non-destructive Damping Measurement for Wafer- level Packaged Microelectromechanical System (MEMS) Acceleration Switches by Ryan Knight and...Laboratory Adelphi, MD 20783-1138 ARL-TR-7094 September 2014 Non-destructive Damping Measurement for Wafer- level Packaged

  6. Recent advances in the use of non-destructive near infrared spectroscopy on intact olive fruits

    USDA-ARS?s Scientific Manuscript database

    The objective of this review is to illustrate the state of the art in the use of non-destructive near infrared (NIR) spectroscopy for quality evaluation of intact fruit in the olive industry. First, the most recent studies regarding the application of non-destructive NIR spectroscopy methods to asse...

  7. Non-destructive determination of maize leaf and canopy chlorophyll content

    USDA-ARS?s Scientific Manuscript database

    The objective of this study was to develop a rapid non-destructive technique to estimate total chlorophyll (Chl) content in a maize canopy using Chl content in a single leaf. The approach was (1) to calibrate and validate a reflectance-based non-destructive technique to estimate leaf Chl in maize; (...

  8. Non-destructive hyperspectral imaging of quarantined Mars Returned Samples

    NASA Astrophysics Data System (ADS)

    Simionovici, Alexandre; Viso, Michel; Beck, Pierre; Lemelle, Laurence; Westphal, Andrew; Vincze, Laszlo; Schoonjans, Tom; Fihman, Francois; Chazalnoel, Pascale; Ferroir, Tristan; Solé, Vicente Armando; Tucoulou, R.

    Introduction: In preparation for the upcoming International Mars Sample Return mission (MSR), returning samples containing potential biohazards, we have implemented a hyperspec-tral method of in-situ analysis of grains performed in BSL4 quarantine conditions, by combining several non-destructive imaging diagnostics. This allows sample transportation on optimized experimental setups, while monitoring the sample quarantine conditions. Our hyperspectral methodology was tested during analyses of meteorites [1-2] and cometary and interstellar grains from the recent NASA Stardust mission [3-6]. Synchrotron Radiation protocols: X-ray analysis methods are widely accepted as the least destructive probes of fragile, unique samples. Diffraction, X-ray fluorescence and ab-sorption micro/nano-spectroscopies were performed on chondritic test samples using focused monochromatic beams at the ESRF synchrotron in Grenoble, France. 2D maps of grain com-position down to ppm concentrations and polycrystalline structure have simultaneously been acquired, followed by X-ray absorption performed on elements of Z 26. Ideally, absorption micro-tomography can later be performed in full-beam mode to record the 3D morphology of the grain followed by fluorescence-tomography in focus-beam mode which complements this picture with a 3D elemental image of the grain. Lab-based protocols: Raman and IR-based spectroscopies have been performed in reflection mode for mineralogical imaging of the grains in the laboratory using commercial microscopes. The spatial resolution varied in the 1-10 m range. Laser limited penetration of opaque samples permits only 2D imaging of the few nanometer-thick outer layers of the grains. Mineralogical maps are now routinely acquired using Raman spectroscopy at sub-micron scales through the 3 container walls of the Martian sample holder, followed by IR few-micrometer spot measurements recording C-based and potential aqueous alteration distributions. Sample Holder: A

  9. Plane Wave Imaging for ultrasonic non-destructive testing: Generalization to multimodal imaging.

    PubMed

    Le Jeune, Léonard; Robert, Sébastien; Lopez Villaverde, Eduardo; Prada, Claire

    2016-01-01

    This paper describes a new ultrasonic array imaging method for Non-Destructive Testing (NDT) which is derived from the medical Plane Wave Imaging (PWI) technique. The objective is to perform fast ultrasound imaging with high image quality. The approach is to transmit plane waves at several angles and to record the back-scattered signals with all the array elements. Focusing in receive is then achieved by coherent summations of the signals in every point of a region of interest. The medical PWI is generalized to immersion setups where water acts as a coupling medium and to multimodal (direct, half-skip modes) imaging in order to detect different types of defects (inclusions, porosities, cracks). This method is compared to the Total Focusing Method (TFM) which is the reference imaging technique in NDT. First, the two post-processing algorithms are described. Then experimental results with the array probe either in contact or in immersion are presented. A good agreement between the TFM and the PWI is observed, with three to ten times less transmissions required for the PWI. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Non-destructive evaluation of spiral-welded pipes using flexural guided waves

    NASA Astrophysics Data System (ADS)

    Zhang, Xiaowei; Tang, Zhifeng; Lü, Fuzai; Pan, Xiaohong

    2016-02-01

    Millions of miles of pipes are being used in both civil and industrial fields. Spiral-welded pipes, which are widely applied in fields such as drainage, architecture as well as oil and gas storage and transportation, are difficult to inspect due to their complex geometry. Guided waves have shown a great potential in Non-Destructive Evaluation (NDE) and Structural Health Monitoring (SHM) for such cases. Flexural guided waves that propagate at a helix angle relative to the axial direction of pipe, are the most appropriate modes for inspecting spiral-welded pipes. The classical Normal Mode Expansion method (NME) is adopted to disseminate the forced response and perturbation analysis of a steel pipe with respect to a time delay circular loading. A time delay circular array transducer (TDCAT) is proposed for the purpose of exciting pure flexural mode in pipes. Pure flexural mode can be excited when the time delay parameter is specifically designed. The theoretical prediction is verified by finite element numerical evaluation and spiral-welded pipe inspection experiment.

  11. Routes for GMR-Sensor Design in Non-Destructive Testing

    PubMed Central

    Pelkner, Matthias; Neubauer, Andreas; Reimund, Verena; Kreutzbruck, Marc; Schütze, Andreas

    2012-01-01

    GMR sensors are widely used in many industrial segments such as information technology, automotive, automation and production, and safety applications. Each area requires an adaption of the sensor arrangement in terms of size adaption and alignment with respect to the field source involved. This paper deals with an analysis of geometric sensor parameters and the arrangement of GMR sensors providing a design roadmap for non-destructive testing (NDT) applications. For this purpose we use an analytical model simulating the magnetic flux leakage (MFL) distribution of surface breaking defects and investigate the flux leakage signal as a function of various sensor parameters. Our calculations show both the influence of sensor length and height and that when detecting the magnetic flux leakage of μm sized defects a gradiometer base line of 250 μm leads to a signal strength loss of less than 10% in comparison with a magnetometer response. To validate the simulation results we finally performed measurements with a GMR magnetometer sensor on a test plate with artificial μm-range cracks. The differences between simulation and measurement are below 6%. We report on the routes for a GMR gradiometer design as a basis for the fabrication of NDT-adapted sensor arrays. The results are also helpful for the use of GMR in other application when it comes to measure positions, lengths, angles or electrical currents.

  12. Numerical study of light propagation in agricultural products for non-destructive assessment of food quality

    NASA Astrophysics Data System (ADS)

    Hattori, Kiyohito; Fujii, Hiroyuki; Tatekura, Yuki; Kobayashi, Kazumichi; Watanabe, Masao

    2015-12-01

    An accurate determination of optical properties of agricultural products is crucial for non-destructive assessment of food quality. For the determination, light intensity is measured at the surface of the product; then, inverse analysis is employed based on a light propagation model such as the radiative transfer equation (RTE). The inverse analysis requires high computational loads because the light intensity is numerically calculated using the model every time the optical properties are changed. For the calculation, we propose an efficient technique by combining a numerical solution with an analytical solution of the RTE, and investigate the validity of the technique in a two-dimensional homogeneous circular medium which is regarded as a light propagation model with optical properties of kiwifruit. The proposed technique can provide accurate results of the light intensity in change of the optical properties, and the accuracy is less dependent on the boundary conditions and source-detector angles. In addition, the technique can reduce computation time compared with that for numerical calculation of the RTE. These results indicate usefulness of the proposed technique for the inverse analysis.

  13. Theory for cross effect dynamic nuclear polarization under magic-angle spinning in solid state nuclear magnetic resonance: The importance of level crossings

    PubMed Central

    Thurber, Kent R.; Tycko, Robert

    2012-01-01

    We present theoretical calculations of dynamic nuclear polarization (DNP) due to the cross effect in nuclear magnetic resonance under magic-angle spinning (MAS). Using a three-spin model (two electrons and one nucleus), cross effect DNP with MAS for electron spins with a large g-anisotropy can be seen as a series of spin transitions at avoided crossings of the energy levels, with varying degrees of adiabaticity. If the electron spin-lattice relaxation time T1e is large relative to the MAS rotation period, the cross effect can happen as two separate events: (i) partial saturation of one electron spin by the applied microwaves as one electron spin resonance (ESR) frequency crosses the microwave frequency and (ii) flip of all three spins, when the difference of the two ESR frequencies crosses the nuclear frequency, which transfers polarization to the nuclear spin if the two electron spins have different polarizations. In addition, adiabatic level crossings at which the two ESR frequencies become equal serve to maintain non-uniform saturation across the ESR line. We present analytical results based on the Landau-Zener theory of adiabatic transitions, as well as numerical quantum mechanical calculations for the evolution of the time-dependent three-spin system. These calculations provide insight into the dependence of cross effect DNP on various experimental parameters, including MAS frequency, microwave field strength, spin relaxation rates, hyperfine and electron-electron dipole coupling strengths, and the nature of the biradical dopants. PMID:22938251

  14. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves.

    PubMed

    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.

  15. Theory for cross effect dynamic nuclear polarization under magic-angle spinning in solid state nuclear magnetic resonance: the importance of level crossings.

    PubMed

    Thurber, Kent R; Tycko, Robert

    2012-08-28

    We present theoretical calculations of dynamic nuclear polarization (DNP) due to the cross effect in nuclear magnetic resonance under magic-angle spinning (MAS). Using a three-spin model (two electrons and one nucleus), cross effect DNP with MAS for electron spins with a large g-anisotropy can be seen as a series of spin transitions at avoided crossings of the energy levels, with varying degrees of adiabaticity. If the electron spin-lattice relaxation time T(1e) is large relative to the MAS rotation period, the cross effect can happen as two separate events: (i) partial saturation of one electron spin by the applied microwaves as one electron spin resonance (ESR) frequency crosses the microwave frequency and (ii) flip of all three spins, when the difference of the two ESR frequencies crosses the nuclear frequency, which transfers polarization to the nuclear spin if the two electron spins have different polarizations. In addition, adiabatic level crossings at which the two ESR frequencies become equal serve to maintain non-uniform saturation across the ESR line. We present analytical results based on the Landau-Zener theory of adiabatic transitions, as well as numerical quantum mechanical calculations for the evolution of the time-dependent three-spin system. These calculations provide insight into the dependence of cross effect DNP on various experimental parameters, including MAS frequency, microwave field strength, spin relaxation rates, hyperfine and electron-electron dipole coupling strengths, and the nature of the biradical dopants.

  16. Microanisotropy imaging: quantification of microscopic diffusion anisotropy and orientational order parameter by diffusion MRI with magic-angle spinning of the q-vector

    NASA Astrophysics Data System (ADS)

    Lasič, Samo; Szczepankiewicz, Filip; Eriksson, Stefanie; Nilsson, Markus; Topgaard, Daniel

    2014-02-01

    Diffusion tensor imaging (DTI) is the method of choice for non-invasive investigations of the structure of human brain white matter. The results are conventionally reported as maps of the fractional anisotropy (FA), which is a parameter related to microstructural features such as axon density, diameter, and myelination. The interpretation of FA in terms of microstructure becomes ambiguous when there is a distribution of axon orientations within the image voxel. In this paper, we propose a procedure for resolving this ambiguity by determining a new parameter, the microscopic fractional anisotropy (µFA), which corresponds to the FA without the confounding influence of orientation dispersion. In addition, we suggest a method for measuring the orientational order parameter (OP) for the anisotropic objects. The experimental protocol is capitalizing on a recently developed diffusion NMR pulse sequence based on magic-angle spinning of the q-vector. Proof-of-principle experiments are carried out on microimaging and clinical MRI equipment using lyotropic liquid crystals and plant tissues as model materials with high µFA and low FA on account of orientation dispersion. We expect the presented method to be especially fruitful in combination with DTI and high angular resolution acquisition protocols for neuroimaging studies of grey and white matter.

  17. High-speed magic angle spinning solid-state 1H nuclear magnetic resonance study of the conformation of gramicidin A in lipid bilayers.

    PubMed Central

    Bouchard, M; Davis, J H; Auger, M

    1995-01-01

    One- and two-dimensional solid-state 1H nuclear magnetic resonance spectra of gramicidin A incorporated in a dimyristoylphosphatidylcholine membrane have been obtained with use of high-speed magic angle spinning. By rotating the sample at 13 kHz, it is possible to observe signals in the 1H spectra between 6.0 and 9.0 ppm attributable to the aromatic protons of the tryptophan residues and the formyl group proton of gramicidin A. Two-dimensional solid-state COSY spectra provided information for the peak assignments. Moreover, changes in the 1H spectra have been observed as a function of the co-solubilization solvent initially used to prepare the samples and therefore as a function of the conformation adopted by gramicidin A. Three organic solvents have been used: trifluoroethanol, a mixture of methanol/chloroform (1:1 v/v), and ethanol. The conformational interconversion of gramicidin A from the double helix conformation to the channel structure for the sample prepared from ethanol was confirmed by following the time evolution of the proton spectra. PMID:8580336

  18. Magic angle Lee-Goldburg frequency offset irradiation improves the efficiency and selectivity of SPECIFIC-CP in triple-resonance MAS solid-state NMR

    NASA Astrophysics Data System (ADS)

    Wu, Chin H.; De Angelis, Anna A.; Opella, Stanley J.

    2014-09-01

    The efficiency and selectivity of SPECIFIC-CP, a widely used method for selective double cross-polarization in triple-resonance magic angle spinning solid-state NMR, is improved by performing the tangential-shaped 13C irradiation at an offset frequency that meets the Lee-Goldburg condition (LG-SPECIFIC-CP). This is demonstrated on polycrystalline samples of uniformly 13C, 15N labeled N-acetyl-leucine and N-formyl-Met-Leu-Phe-OH (MLF) at 700 MHz and 900 MHz 1H resonance frequencies, respectively. For the single 13Cα of N-acetyl-leucine, relative to conventional broad band cross-polarization, the SPECIFIC-CP signal has 47% of the intensity. Notably, the LG-SPECIFIC-CP signal has 72% of the intensity, essentially the theoretical maximum. There were no other changes in the experimental parameters. The three 13Cα signals in MLF show some variation in intensities, reflecting the relatively narrow bandwidth of a frequency-offset procedure, and pointing to future developments for this class of experiment.

  19. A nuclear magnetic resonance spectrometer concept for hermetically sealed magic angle spinning investigations on highly toxic, radiotoxic, or air sensitive materials

    NASA Astrophysics Data System (ADS)

    Martel, L.; Somers, J.; Berkmann, C.; Koepp, F.; Rothermel, A.; Pauvert, O.; Selfslag, C.; Farnan, I.

    2013-05-01

    A concept to integrate a commercial high-resolution, magic angle spinning nuclear magnetic resonance (MAS-NMR) probe capable of very rapid rotation rates (70 kHz) in a hermetically sealed enclosure for the study of highly radiotoxic materials has been developed and successfully demonstrated. The concept centres on a conventional wide bore (89 mm) solid-state NMR magnet operating with industry standard 54 mm diameter probes designed for narrow bore magnets. Rotor insertion and probe tuning take place within a hermetically enclosed glovebox, which extends into the bore of the magnet, in the space between the probe and the magnet shim system. Oxygen-17 MAS-NMR measurements demonstrate the possibility of obtaining high quality spectra from small sample masses (˜10 mg) of highly radiotoxic material and the need for high spinning speeds to improve the spectral resolution when working with actinides. The large paramagnetic susceptibility arising from actinide paramagnetism in (Th1-xUx)O2 solid solutions gives rise to extensive spinning sidebands and poor resolution at 15 kHz, which is dramatically improved at 55 kHz. The first 17O MAS-NMR measurements on NpO2+x samples spinning at 55 kHz are also reported. The glovebox approach developed here for radiotoxic materials can be easily adapted to work with other hazardous or even air sensitive materials.

  20. Elucidating connectivity and metal-binding structures of unlabeled paramagnetic complexes by 13C and 1H solid-state NMR under fast magic angle spinning.

    PubMed

    Wickramasinghe, Nalinda P; Shaibat, Medhat A; Ishii, Yoshitaka

    2007-08-23

    Characterizing paramagnetic complexes in solids is an essential step toward understanding their molecular functions. However, methodologies to characterize chemical and electronic structures of paramagnetic systems at the molecular level have been notably limited, particularly for noncrystalline solids. We present an approach to obtain connectivities of chemical groups and metal-binding structures for unlabeled paramagnetic complexes by 13C and 1H high-resolution solid-state NMR (SSNMR) using very fast magic angle spinning (VFMAS, spinning speed >or=20 kHz). It is experimentally shown for unlabeled Cu(II)(Ala-Thr) that 2D 13C/1H correlation SSNMR under VFMAS provides the connectivity of chemical groups and assignments for the characterization of unlabeled paramagnetic systems in solids. We demonstrate that on the basis of the assignments provided by the VFMAS approach multiple 13C-metal distances can be simultaneously elucidated by a combination of measurements of 13C anisotropic hyperfine shifts and 13C T1 relaxation due to hyperfine interactions for this peptide-Cu(II) complex. It is also shown that an analysis of 1H anisotropic hyperfine shifts allows for the determination of electron-spin states in Fe(III)-chloroprotoporphyin-IX in solid states.

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

    PubMed

    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.

  2. Vibrational 13C-cross-polarization/magic angle spinning NMR spectroscopic and thermal characterization of poly(alanine-glycine) as model for silk I Bombyx mori fibroin.

    PubMed

    Monti, Patrizia; Taddei, Paola; Freddi, Giuliano; Ohgo, Kosuke; Asakura, Tetsuo

    2003-01-01

    This study focuses on the conformational characterization of poly(alanine-glycine) II (pAG II) as a model for a Bombyx mori fibroin silk I structure. Raman, IR, and 13C-cross-polarization/magic angle spinning NMR spectra of pAG II are discussed in comparison with those of the crystalline fraction of B. mori silk fibroin (chymotryptic precipitate, Cp) with a silk I (silk I-Cp) structure. The spectral data give evidence that silk I-Cp and the synthetic copolypeptide pAG II have similar conformations. Moreover, the spectral findings reveal that silk I-Cp is more crystalline than pAG II; consequently, the latter contains a larger amount of the random coil conformation. Differential scanning calorimetry measurements confirm this result. N-Deuteration experiments on pAG II allow us to attribute the Raman component at 1320 cm(-1) to the amide III mode of a beta-turn type II conformation, thus confirming the results of those who propose a repeated beta-turn type II structure for silk I. The analysis of the Raman spectra in the nuNH region confirms that the silk I structure is characterized by the presence of different types of H-bonding arrangements, in agreement with the above model. Copyright 2003 Wiley Periodicals, Inc.

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

    PubMed

    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.

  4. Magic angle Lee-Goldburg frequency offset irradiation improves the efficiency and selectivity of SPECIFIC-CP in triple-resonance MAS solid-state NMR

    PubMed Central

    Wu, C.H.; De Angelis, Anna A.; Opella, Stanley J.

    2014-01-01

    The efficiency and selectivity of SPECIFIC-CP, a widely used method for selective double cross-polarization in triple-resonance magic angle spinning solid-state NMR, is improved by performing the tangential-shaped 13C irradiation at an offset frequency that meets the Lee-Goldburg condition (LG-SPECIFIC-CP). This is demonstrated on polycrystalline samples of uniformly 13C, 15N labeled N-acetyl-leucine and N-formyl-Met-Leu-Phe-OH (MLF) at 700 MHz and 900 MHz 1H resonance frequencies, respectively. For the single 13Cα of N-acetyl-leucine, relative to conventional broad band cross-polarization, the SPECIFIC-CP signal has 47% of the intensity. Notably, the LG-SPECIFIC-CP signal has 72% of the intensity, essentially the theoretical maximum. There were no other changes in the experimental parameters. The three 13Cα signals in MLF show some variation in intensities, reflecting the relatively narrow bandwidth of a frequency-offset procedure, and pointing to future developments for this class of experiment. PMID:25051542

  5. Solid-state NMR adiabatic TOBSY sequences provide enhanced sensitivity for multidimensional high-resolution magic-angle-spinning 1H MR spectroscopy

    NASA Astrophysics Data System (ADS)

    Andronesi, Ovidiu C.; Mintzopoulos, Dionyssios; Struppe, Jochem; Black, Peter M.; Tzika, A. Aria

    2008-08-01

    We propose a solid-state NMR method that maximizes the advantages of high-resolution magic-angle-spinning (HRMAS) applied to intact biopsies when compared to more conventional liquid-state NMR approaches. Theoretical treatment, numerical simulations and experimental results on intact human brain biopsies are presented. Experimentally, it is proven that an optimized adiabatic TOBSY (TOtal through Bond correlation SpectroscopY) solid-state NMR pulse sequence for two-dimensional 1H- 1H homonuclear scalar-coupling longitudinal isotropic mixing provides a 20%-50% improvement in signal-to-noise ratio relative to its liquid-state analogue TOCSY (TOtal Correlation SpectroscopY). For this purpose we have refined the C9151 symmetry-based 13C TOBSY pulse sequence for 1H MRS use and compared it to MLEV-16 TOCSY sequence. Both sequences were rotor-synchronized and implemented using WURST-8 adiabatic inversion pulses. As discussed theoretically and shown in simulations, the improved magnetization-transfer comes from actively removing residual dipolar couplings from the average Hamiltonian. Importantly, the solid-state NMR techniques are tailored to perform measurements at low temperatures where sample degradation is reduced. This is the first demonstration of such a concept for HRMAS metabolic profiling of disease processes, including cancer, from biopsies requiring reduced sample degradation for further genomic analysis.

  6. Magic Angle Spinning NMR Reveals Sequence-Dependent Structural Plasticity, Dynamics, and the Spacer Peptide 1 Conformation in HIV-1 Capsid Protein Assemblies

    SciTech Connect

    Han, Yun; Hou, Guangjin; Suiter, Christopher L.; Ahn, Jinwoo; Byeon, In-Ja L.; Lipton, Andrew S.; Burton, Sarah D.; Hung, Ivan; Gorkov, Peter L.; Gan, Zhehong; Brey, William W.; Rice, David M.; Gronenborn, Angela M.; Polenova, Tatyana E.

    2013-11-27

    Maturation of HIV-1 virus into an infectious virion requires cleavage of the Gag polyprotein into its constituent domains and formation of a conical capsid core that encloses viral RNA and a small complement of proteins for replication. The final step of this process is the cleavage of the SP1 peptide from the CA-SP1 maturation intermediate, which triggers the condensation of the CA protein into a conical capsid. The mechanism of this step, including the conformation of the SP1 peptide in CA-SP1, is under intense debate. In this report, we examine the tubular assemblies of CA and the CA-SP1 maturation intermediate using Magic Angle Spinning NMR spectroscopy. At the magnetic fields of 19.9 T and above, tubular CA and CA-SP1 assemblies yield outstanding-quality 2D and 3D MAS NMR spectra, which are amenable to resonance assignments and detailed structural characterization. Dipolar- and scalar-based correlation experiments unequivocally indicate that SP1 peptide is in a random coil conformation and mobile in the assembled CA-SP1. Analysis of two sequence variants reveals that remarkably, the conformation of SP1 tail, of the functionally important CypA loop, and of the loop preceding helix 8 are sequence dependent and modulated by the residue variations at distal sites. These findings challenge the role of SP1 as a conformational switch in the maturation process and establish sequence-dependent conformational plasticity in CA.

  7. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

    SciTech Connect

    Thurber, Kent R. Tycko, Robert

    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.

  8. The effects of high concentrations of ionic liquid on GB1 protein structure and dynamics probed by high-resolution magic-angle-spinning NMR spectroscopy.

    PubMed

    Warner, Lisa; Gjersing, Erica; Follett, Shelby E; Elliott, K Wade; Dzyuba, Sergei V; Varga, Krisztina

    2016-12-01

    Ionic liquids have great potential in biological applications and biocatalysis, as some ionic liquids can stabilize proteins and enhance enzyme activity, while others have the opposite effect. However, on the molecular level, probing ionic liquid interactions with proteins, especially in solutions containing high concentration of ionic liquids, has been challenging. In the present work the (13)C, (15)N-enriched GB1 model protein was used to demonstrate applicability of high-resolution magic-angle-spinning (HR-MAS) NMR spectroscopy to investigate ionic liquid - protein interactions. Effect of an ionic liquid (1-butyl-3-methylimidazolium bromide, [C4-mim]Br) on GB1was studied over a wide range of the ionic liquid concentrations (0.6 to 3.5 M, which corresponds to 10%-60% v/v). Interactions between GB1 and [C4-mim]Br were observed from changes in the chemical shifts of the protein backbone as well as the changes in (15)N ps-ns dynamics and rotational correlation times. Site-specific interactions between the protein and [C4-mim]Br were assigned using 3D methods under HR-MAS conditions. Thus, HR-MAS NMR is a viable tool that could aid in elucidation of the molecular mechanism of ionic liquid - protein interactions.

  9. The use of a selective saturation pulse to suppress t1 noise in two-dimensional 1H fast magic angle spinning solid-state NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Robertson, Aiden J.; Pandey, Manoj Kumar; Marsh, Andrew; Nishiyama, Yusuke; Brown, Steven P.

    2015-11-01

    A selective saturation pulse at fast magic angle spinning (MAS) frequencies (60+ kHz) suppresses t1 noise in the indirect dimension of two-dimensional 1H MAS NMR spectra. The method is applied to a synthetic nucleoside with an intense methyl 1H signal due to triisopropylsilyl (TIPS) protecting groups. Enhanced performance in terms of suppressing the methyl signal while minimising the loss of signal intensity of nearby resonances of interest relies on reducing spin diffusion - this is quantified by comparing two-dimensional 1H NOESY-like spin diffusion spectra recorded at 30-70 kHz MAS. For a saturation pulse centred at the methyl resonance, the effect of changing the nutation frequency at different MAS frequencies as well as the effect of changing the pulse duration is investigated. By applying a pulse of duration 30 ms and nutation frequency 725 Hz at 70 kHz MAS, a good compromise of significant suppression of the methyl resonance combined with the signal intensity of resonances greater than 5 ppm away from the methyl resonance being largely unaffected is achieved. The effectiveness of using a selective saturation pulse is demonstrated for both homonuclear 1H-1H double quantum (DQ)/single quantum (SQ) MAS and 14N-1H heteronuclear multiple quantum coherence (HMQC) two-dimensional solid-state NMR experiments.

  10. Strong-coupling induced damping of spin-echo modulations in magic-angle-spinning NMR: Implications for J coupling measurements in disordered solids.

    PubMed

    Guerry, Paul; Brown, Steven P; Smith, Mark E

    2017-08-19

    In the context of improving J coupling measurements in disordered solids, strong coupling effects have been investigated in the spin-echo and refocused INADEQUATE spin-echo (REINE) modulations of three- and four-spin systems under magic-angle-spinning (MAS), using density matrix simulations and solid-state NMR experiments on a cadmium phosphate glass. Analytical models are developed for the different modulation regimes, which are shown to be distinguishable in practice using Akaike's information criterion. REINE modulations are shown to be free of the damping that occurs for spin-echo modulations when the observed spin has the same isotropic chemical shift as its neighbour. Damping also occurs when the observed spin is bonded to a strongly-coupled pair. For mid-chain units, the presence of both direct and relayed damping makes both REINE and spin-echo modulations impossible to interpret quantitatively. We nonetheless outline how a qualitative comparison of the modulation curves can provide valuable information on disordered networks, possibly also pertaining to dynamic effects therein. Copyright © 2017 Elsevier Inc. All rights reserved.

  11. High-resolution magic angle spinning (1)H magnetic resonance spectroscopy detects choline as a biomarker in a swine obstructive chronic pancreatitis model at an early stage.

    PubMed

    Sun, Gaofeng; Wang, Jianhua; Zhang, Jian; Ma, Chao; Shao, Chengwei; Hao, Jun; Zheng, Jianming; Feng, Xiaoyuan; Zuo, Changjing

    2014-03-04

    Chronic pancreatitis (CP) is a progressive inflammatory and fibrotic disease of the pancreas which encompasses a variety of clinical syndromes ranging from mild to life-threatening complications. Metabolomics has increasingly been applied to identify biomarkers for disease diagnosis with particular interest in diseases at an early stage. In this study, we tested a swine obstructive CP model by subtotal ligation of the main pancreatic duct, and the metabolic profiles of the Bama miniature swine pancreas were investigated using high-resolution magic angle spinning proton magnetic resonance spectroscopy (HR MAS (1)H MRS) combined with principal components analysis (PCA). Increases in lactate and choline for mild CP and decreases in glycerophosphocholine, phosphocholine, betaine and glycine were observed from normal pancreas to mild, moderate and severe CP. PCA results showed visual separations among the groups. The increase of choline at an early stage of CP and the decrease of glycerophosphocholine, phosphocholine, betaine and glycine reveal the pathogenesis of CP at a molecular level. The MRS results presented here demonstrate the potential of metabolic profiles in discriminating a normal pancreas from different stages of CP, which may be used to achieve CP early diagnosis and timely intervention to prevent irreversible destruction of the pancreas.

  12. Magic-angle spinning NMR studies of cell wall bound aromatic-aliphatic biopolyesters associated with strengthening of intercellular adhesion in potato (Solanum tuberosum L.) tuber parenchyma.

    PubMed

    Yu, Bingwu; Vengadesan, G; Wang, Hsin; Jashi, Liana; Yefremov, Tatiana; Tian, Shiying; Gaba, Victor; Shomer, Ilan; Stark, Ruth E

    2006-03-01

    Intercellular adhesion strengthening, a phenomenon that compromises the texture and the edible quality of potatoes (Solanum tuberosum L.), has been induced reproducibly by exposure to low-pH acetic acid solutions under tissue culture conditions. The resulting parenchyma tissues have been examined by solid-state nuclear magnetic resonance (NMR) in order to characterize the biopolymer(s) thought to be associated with this syndrome. Cross polarization-magic angle spinning (CPMAS) (13)C NMR has been used to establish the presence of a polyphenol-suberin-like aromatic-aliphatic polyester within an abundant cell wall polysaccharide matrix in potato tubers that exhibit hardening due to strengthened intercellular adhesion. Dipolar dephasing and CP chemical shift anisotropy experiments suggest that the aromatic domain is composed primarily of guaiacyl and sinapyl groups. Two-dimensional wide-line separation experiments show that the biopolymer associated with parenchyma hardening contains rigid polysaccharide cell walls and mobile aliphatic long-chain fatty acids; (1)H spin diffusion experiments show that these flexible aliphatic chains are proximal to both the phenolics and a subpopulation of the cell wall polysaccharides. Finally, high-resolution MAS NMR of parenchyma samples swelled in DMSO in conjunction with two-dimensional through-bond and through-space NMR spectroscopy provides evidence for covalent linkages among the polysaccharide, phenolic, and aliphatic domains of the intercellular adhesion-strengthening biopolymer in potato parenchyma tissue.

  13. Assessing the Detection Limit of a Minority Solid-State Form of a Pharmaceutical by (1)H Double-Quantum Magic-Angle Spinning Nuclear Magnetic Resonance Spectroscopy.

    PubMed

    Maruyoshi, Keisuke; Iuga, Dinu; Watts, Abigail E; Hughes, Colan E; Harris, Kenneth D M; Brown, Steven P

    2017-07-25

    The lower detection limit for 2 distinct crystalline phases by (1)H magic-angle spinning (MAS) solid-state nuclear magnetic resonance (NMR) is investigated for a minority amount of cimetidine (anhydrous polymorph A) in a physical mixture with the anhydrous HCl salt of cimetidine. Specifically, 2-dimensional (1)H double-quantum (DQ) MAS NMR spectra of polymorph A and the anhydrous HCl salt constitute fingerprints for the presence of each of these solid forms. For solid-state NMR data recorded at a (1)H Larmor frequency of 850 MHz and a MAS frequency of 30 kHz on ∼10 mg of sample, it is shown that, by following the pair of cross-peaks at a (1)H DQ frequency of 7.4 + 11.6 = 19.0 ppm that are unique to polymorph A, the level of detection for polymorph A in a physical mixture with the anhydrous HCl salt is a concentration of 1% w/w. Copyright © 2017 The Authors. Published by Elsevier Inc. All rights reserved.

  14. Taurine detected using high-resolution magic angle spinning 1H nuclear magnetic resonance: A potential indicator of early myocardial infarction

    PubMed Central

    YANG, YUNLONG; YANG, LIN; ZHANG, YUE; GU, XINGHUA; XU, DANLING; FANG, FANG; SUN, AIJUN; WANG, KEQIANG; YU, YIHUA; ZUO, JI; GE, JUNBO

    2013-01-01

    Magnetic resonance spectroscopy (MRS) is a unique non-invasive method for detecting cardiac metabolic changes. However, MRS in cardiac diagnosis is limited due to insensitivity and low efficiency. Taurine (Tau) is the most abundant free amino acid in the myocardium. We hypothesized that Tau levels may indicate myocardial ischemia and early infarction. Sprague-Dawley rats were divided into seven groups according to different time points during the course of myocardial ischemia, which was induced by left anterior descending coronary artery ligation. Infarcted myocardial tissue was obtained for high-resolution magic angle spinning 1H nuclear magnetic resonance (NMR) analysis. Results were validated via high-performance liquid chromatography. The Tau levels in the ischemic myocardial tissue were reduced significantly within 5 min compared with those in the control group (relative ratio from 20.27±6.48 to 8.81±0.04, P<0.05) and were maintained for 6 h post-ischemia. Tau levels declined more markedly (56.5%) than creatine levels (48.5%) at 5 min after ligation. This suggests that Tau may have potential as an indicator in the early detection of myocardial ischemia by 1H MRS. PMID:23408155

  15. Carbon-thirteen cross-polarization magic angle spinning nuclear magnetic resonance and Fourier transform infrared studies of thermally modified wood exposed to brown and soft rot fungi.

    PubMed

    Sivonen, Hanne; Nuopponen, Mari; Maunu, Sirkka L; Sundholm, Franciska; Vuorinen, Tapani

    2003-03-01

    Thermally modified wood has many technically interesting properties, such as increased dimensional stability, low equilibrium moisture content, and enhanced biological and weather resistance. This paper describes solid-state nuclear magnetic resonance (NMR) and Fourier transform infrared (FT-IR) spectroscopic studies on the decay of heat-treated and untreated pine (Pinus sylvestris) by brown (Poria placenta) and soft rot fungi. Both techniques combined with multivariate data analysis proved to be powerful tools for the study of wood degradation by fungi. When untreated pine was exposed to brown or soft rot fungi, a drastic decay of the cell wall polysaccharides was observed. Brown rot fungus degraded mainly hemicelluloses while soft rot fungus attacked cellulose more extensively. The aromatic region of 13C cross-polarization magic angle spinning (CPMAS) NMR spectra revealed that the structure of lignin was also altered. New carboxylic structures were formed as a consequence of the decay. The increased biological resistance of pine wood heat-treated at >220 degrees C was observed in the 13C CPMAS NMR and IR spectra.

  16. A Solid-State Study of a Novel 31P Spin Pair Using Magic-Angle-Spinning Nuclear Magnetic Resonance Spectroscopy

    NASA Astrophysics Data System (ADS)

    Challoner, R.; Mcdowell, C. A.; Yoshifuji, M.; Toyota, K.; Tossell, J. A.

    The present investigation concerns the solid-state nuclear magnetic resonance spectroscopy of the 31P spin pair in the novel three-membered heterocyclic compound 3-(dichloromethylene)- trans-1,2-bis( 2,4,6-tri- tert-butylphenyl)- 1,2-diphosphirane using the magic-angle-spinning (MAS) technique. The homogeneous 31P lineshapes are analyzed to extract the principal components of the shielding tensors using the Maricq and Waugh description of homonuclear spin-pair systems by average-Hamiltonian theory, modified to encompass the n = 0 rotational resonance situation. The experimental values of the shielding-tensor components are compared with those obtained from ab initio calculations performed on the model molecule P 2C 2H 4 to aid further the interpretation of the 31P MAS NMR spectrum of the chloromethylene-diphosphirane. The magnitudes and orientations of calculated shielding-tensor components of the model compound methylene-diphosphirane P 2C 2H 4 are compared with those for the phosphorus spin pair in the molecular environments of P 2, P 2H 2, and P 2H 4. The electronic structures and bonding in all of those molecular species are discussed.

  17. A Monte Carlo/simulated annealing algorithm for sequential resonance assignment in solid state NMR of uniformly labeled proteins with magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Tycko, Robert; Hu, Kan-Nian

    2010-08-01

    We describe a computational approach to sequential resonance assignment in solid state NMR studies of uniformly 15N, 13C-labeled proteins with magic-angle spinning. As input, the algorithm uses only the protein sequence and lists of 15N/ 13C α crosspeaks from 2D NCACX and NCOCX spectra that include possible residue-type assignments of each crosspeak. Assignment of crosspeaks to specific residues is carried out by a Monte Carlo/simulated annealing algorithm, implemented in the program MC_ASSIGN1. The algorithm tolerates substantial ambiguity in residue-type assignments and coexistence of visible and invisible segments in the protein sequence. We use MC_ASSIGN1 and our own 2D spectra to replicate and extend the sequential assignments for uniformly-labeled HET-s(218-289) fibrils previously determined manually by Siemer et al. (J. Biomol. NMR, 34 (2006) 75-87) from a more extensive set of 2D and 3D spectra. Accurate assignments by MC_ASSIGN1 do not require data that are of exceptionally high quality. Use of MC_ASSIGN1 (and its extensions to other types of 2D and 3D data) is likely to alleviate many of the difficulties and uncertainties associated with manual resonance assignments in solid state NMR studies of uniformly labeled proteins, where spectral resolution and signal-to-noise are often sub-optimal.

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

    PubMed Central

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

    2015-01-01

    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. PMID:26604305

  19. Probing molecular dynamics in chromatographic systems using high-resolution 1H magic-angle-spinning NMR spectroscopy: interaction between p-Xylene and C18-bonded silica.

    PubMed

    Coen, Muireann; Wilson, Ian D; Nicholson, Jeremy K; Tang, Huiru; Lindon, John C

    2004-06-01

    The exact nature of the interaction between small molecules and chromatographic solid phases has been the subject of much research, but detailed understanding of the molecular dynamics in such systems remains elusive. High-resolution (1)H magic-angle-spinning (MAS) NMR spectroscopy has been applied to the investigation of C18-bonded silica material as used in chromatographic separation techniques together with an adsorbed model analyte, p-xylene. Two distinct p-xylene and water environments were identified within the C18-bonded silica through the measurement of (1)H NMR chemical shifts, T(1) and T(2) relaxation times and diffusion coefficients, including their temperature dependence. The results have been analyzed in terms of two environments, p-xylene within the C18 chains, in slow exchange on the NMR time scale with p-xylene in a more mobile state adsorbed as a layer in close proximity to the C18 particles, but which is distinct from free liquid p-xylene. The techniques used here could have more general applications, including the study of drug molecules bound into phospholipid membranes in micelles or vesicles.

  20. A nuclear magnetic resonance spectrometer concept for hermetically sealed magic angle spinning investigations on highly toxic, radiotoxic, or air sensitive materials.

    PubMed

    Martel, L; Somers, J; Berkmann, C; Koepp, F; Rothermel, A; Pauvert, O; Selfslag, C; Farnan, I

    2013-05-01

    A concept to integrate a commercial high-resolution, magic angle spinning nuclear magnetic resonance (MAS-NMR) probe capable of very rapid rotation rates (70 kHz) in a hermetically sealed enclosure for the study of highly radiotoxic materials has been developed and successfully demonstrated. The concept centres on a conventional wide bore (89 mm) solid-state NMR magnet operating with industry standard 54 mm diameter probes designed for narrow bore magnets. Rotor insertion and probe tuning take place within a hermetically enclosed glovebox, which extends into the bore of the magnet, in the space between the probe and the magnet shim system. Oxygen-17 MAS-NMR measurements demonstrate the possibility of obtaining high quality spectra from small sample masses (~10 mg) of highly radiotoxic material and the need for high spinning speeds to improve the spectral resolution when working with actinides. The large paramagnetic susceptibility arising from actinide paramagnetism in (Th(1-x)U(x))O2 solid solutions gives rise to extensive spinning sidebands and poor resolution at 15 kHz, which is dramatically improved at 55 kHz. The first (17)O MAS-NMR measurements on NpO(2+x) samples spinning at 55 kHz are also reported. The glovebox approach developed here for radiotoxic materials can be easily adapted to work with other hazardous or even air sensitive materials.

  1. Multidimensional High-Resolution Magic Angle Spinning and Solution-State NMR Characterization of 13C-labeled Plant Metabolites and Lignocellulose

    PubMed Central

    Mori, Tetsuya; Tsuboi, Yuuri; Ishida, Nobuhiro; Nishikubo, Nobuyuki; Demura, Taku; Kikuchi, Jun

    2015-01-01

    Lignocellulose, which includes mainly cellulose, hemicellulose, and lignin, is a potential resource for the production of chemicals and for other applications. For effective production of materials derived from biomass, it is important to characterize the metabolites and polymeric components of the biomass. Nuclear magnetic resonance (NMR) spectroscopy has been used to identify biomass components; however, the NMR spectra of metabolites and lignocellulose components are ambiguously assigned in many cases due to overlapping chemical shift peaks. Using our 13C-labeling technique in higher plants such as poplar samples, we demonstrated that overlapping peaks could be resolved by three-dimensional NMR experiments to more accurately assign chemical shifts compared with two-dimensional NMR measurements. Metabolites of the 13C-poplar were measured by high-resolution magic angle spinning NMR spectroscopy, which allows sample analysis without solvent extraction, while lignocellulose components of the 13C-poplar dissolved in dimethylsulfoxide/pyridine solvent were analyzed by solution-state NMR techniques. Using these methods, we were able to unambiguously assign chemical shifts of small and macromolecular components in 13C-poplar samples. Furthermore, using samples of less than 5 mg, we could differentiate between two kinds of genes that were overexpressed in poplar samples, which produced clearly modified plant cell wall components. PMID:26143886

  2. Field-cycling NMR with high-resolution detection under magic-angle spinning: determination of field-window for nuclear hyperpolarization in a photosynthetic reaction center.

    PubMed

    Gräsing, Daniel; Bielytskyi, Pavlo; Céspedes-Camacho, Isaac F; Alia, A; Marquardsen, Thorsten; Engelke, Frank; Matysik, Jörg

    2017-09-21

    Several parameters in NMR depend on the magnetic field strength. Field-cycling NMR is an elegant way to explore the field dependence of these properties. The technique is well developed for solution state and in relaxometry. Here, a shuttle system with magic-angle spinning (MAS) detection is presented to allow for field-dependent studies on solids. The function of this system is demonstrated by exploring the magnetic field dependence of the solid-state photochemically induced nuclear polarization (photo-CIDNP) effect. The effect allows for strong nuclear spin-hyperpolarization in light-induced spin-correlated radical pairs (SCRPs) under solid-state conditions. To this end, (13)C MAS NMR is applied to a photosynthetic reaction center (RC) of the purple bacterium Rhodobacter (R.) sphaeroides wildtype (WT). For induction of the effect in the stray field of the magnet and its subsequent observation at 9.4 T under MAS NMR conditions, the sample is shuttled by the use of an aerodynamically driven sample transfer technique. In the RC, we observe the effect down to 0.25 T allowing to determine the window for the occurrence of the effect to be between about 0.2 and 20 T.

  3. Characterization of metabolic profile of intact non-tumor and tumor breast cells by high-resolution magic angle spinning nuclear magnetic resonance spectroscopy.

    PubMed

    Maria, Roberta M; Altei, Wanessa F; Andricopulo, Adriano D; Becceneri, Amanda B; Cominetti, Márcia R; Venâncio, Tiago; Colnago, Luiz A

    2015-11-01

    (1)H high-resolution magic angle spinning nuclear magnetic resonance ((1)H HR-MAS NMR) spectroscopy was used to analyze the metabolic profile of an intact non-tumor breast cell line (MCF-10A) and intact breast tumor cell lines (MCF-7 and MDA-MB-231). In the spectra of MCF-10A cells, six metabolites were assigned, with glucose and ethanol in higher concentrations. Fifteen metabolites were assigned in MCF-7 and MDA-MB-231 (1)H HR-MAS NMR spectra. They did not show glucose and ethanol, and the major component in both tumor cells was phosphocholine (higher in MDA-MB-231 than in MCF-7), which can be considered as a tumor biomarker of breast cancer malignant transformation. These tumor cells also show acetone signal that was higher in MDA-MB-231 cells than in MCF-7 cells. The high acetone level may be an indication of high demand for energy in MDA-MB-231 to maintain cell proliferation. The higher acetone and phosphocholine levels in MDA-MB-231 cells indicate the higher malignance of the cell line. Therefore, HR-MAS is a rapid reproducible method to study the metabolic profile of intact breast cells, with minimal sample preparation and contamination, which are critical in the analyses of slow-growth cells. Copyright © 2015 Elsevier Inc. All rights reserved.

  4. Self-diffusion of electrolyte species in model battery electrodes using Magic Angle Spinning and Pulsed Field Gradient Nuclear Magnetic Resonance

    NASA Astrophysics Data System (ADS)

    Tambio, Sacris Jeru; Deschamps, Michaël; Sarou-Kanian, Vincent; Etiemble, Aurélien; Douillard, Thierry; Maire, Eric; Lestriez, Bernard

    2017-09-01

    Lithium-ion batteries are electrochemical storage devices using the electrochemical activity of the lithium ion in relation to intercalation compounds owing to mass transport phenomena through diffusion. Diffusion of the lithium ion in the electrode pores has been poorly understood due to the lack of experimental techniques for measuring its self-diffusion coefficient in porous media. Magic-Angle Spinning, Pulsed Field Gradient, Stimulated-Echo Nuclear Magnetic Resonance (MAS-PFG-STE NMR) was used here for the first time to measure the self-diffusion coefficients of the electrolyte species in the LP30 battery electrolyte (i.e. a 1 M solution of LiPF6 dissolved in 1:1 Ethylene Carbonate - Dimethyl Carbonate) in model composites. These composite electrodes were made of alumina, carbon black and PVdF-HFP. Alumina's magnetic susceptibility is close to the measured magnetic susceptibility of the LP30 electrolyte thereby limiting undesirable internal field gradients. Interestingly, the self-diffusion coefficient of lithium ions decreases with increasing carbon content. FIB-SEM was used to describe the 3D geometry of the samples. The comparison between the reduction of self-diffusion coefficients as measured by PFG-NMR and as geometrically derived from FIB/SEM tortuosity values highlights the contribution of specific interactions at the material/electrolyte interface on the lithium transport properties.

  5. Systematic evaluation of heteronuclear spin decoupling in solid-state NMR at the rotary-resonance conditions in the regime of fast magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Sharma, Kshama; Madhu, P. K.; Agarwal, Vipin

    2016-09-01

    The performance of heteronuclear spin decoupling sequences in solid-state NMR severely degrades when the proton radiofrequency (RF) nutation frequencies (ν1) are close to or at multiples of magic-angle spinning (MAS) frequency (νr) that are referred to as rotary-resonance recoupling conditions (ν1 = n · νr). Recently, two schemes, namely, PISSARRO and rCWApA, have been shown to be less affected by the problem of MAS and RF interference, specifically at the n = 2 rotary-resonance recoupling condition, especially in the fast MAS regime. Here, we systematically evaluate the loss in intensity of several heteronuclear spin decoupling sequences at the n = 1, 2 conditions compared to high-power decoupling in the fast-MAS regime. We propose that in the fast-MAS regime (above 40 kHz) the entire discussion about RF and MAS interference can be avoided by using appropriate low-power decoupling sequences which give comparable performance to decoupling sequences with high-power 1H irradiation of ca.195 kHz.

  6. High-resolution magic angle spinning 1H NMR spectroscopy of metabolic changes in rabbit lens after treatment with dexamethasone combined with UVB exposure.

    PubMed

    Saether, Oddbjørn; Risa, Oystein; Cejková, Jitka; Krane, Jostein; Midelfart, Anna

    2004-12-01

    Long-term steroid treatment and UVB exposure are well-known cataractogenic factors. The purpose of this study was to investigate metabolic changes in the rabbit lens after long-term dexamethasone treatment in combination with UVB exposure, using high-resolution magic angle spinning proton nuclear magnetic resonance (HR-MAS (1)H NMR) spectroscopy to analyse intact lens tissues. Rabbits received topical doses of 0.1% dexamethasone or 0.9% saline (50 microl) four times daily for 36 days. On day 37, the eyes were exposed to UVB radiation (2.05 J/cm(2)). Twenty-four hours later the animals were killed, and HR-MAS (1)H NMR spectra of lens tissues were obtained. More than 15 major metabolites were assigned in NMR spectra of rabbit lenses. The combined treatment with dexamethasone and UVB induced large reductions in the concentration of reduced glutathione, inositols, taurine and lactate compared with normal lenses. Concurrently, the levels of glucose, sorbitol and sorbitol-3-phosphate were increased. After exposure to UVB radiation only, the most significant finding was a decrease in the concentration of lactate. No lens opacities were detected. HR-MAS (1)H NMR spectroscopy was found to be an efficient tool for analysis of intact lens tissues. High-resolution NMR spectra of intact lens tissue enabled metabolic changes to be quantified. Long-term treatment with dexamethasone combined with UVB exposure induced substantial metabolic changes, dominated by osmolytic regulation processes and loss of glutathione.

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

    NASA Astrophysics Data System (ADS)

    Thurber, Kent R.; Tycko, Robert

    2009-01-01

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

  8. Perturbation of nuclear spin polarizations in solid state NMR of nitroxide-doped samples by magic-angle spinning without microwaves

    PubMed Central

    Thurber, Kent R.; Tycko, Robert

    2014-01-01

    We report solid state 13C and 1H 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, 1H and cross-polarized 13C NMR signals from 15N,13C-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. PMID:24832263

  9. The use of a selective saturation pulse to suppress t1 noise in two-dimensional (1)H fast magic angle spinning solid-state NMR spectroscopy.

    PubMed

    Robertson, Aiden J; Pandey, Manoj Kumar; Marsh, Andrew; Nishiyama, Yusuke; Brown, Steven P

    2015-11-01

    A selective saturation pulse at fast magic angle spinning (MAS) frequencies (60+kHz) suppresses t1 noise in the indirect dimension of two-dimensional (1)H MAS NMR spectra. The method is applied to a synthetic nucleoside with an intense methyl (1)H signal due to triisopropylsilyl (TIPS) protecting groups. Enhanced performance in terms of suppressing the methyl signal while minimising the loss of signal intensity of nearby resonances of interest relies on reducing spin diffusion--this is quantified by comparing two-dimensional (1)H NOESY-like spin diffusion spectra recorded at 30-70 kHz MAS. For a saturation pulse centred at the methyl resonance, the effect of changing the nutation frequency at different MAS frequencies as well as the effect of changing the pulse duration is investigated. By applying a pulse of duration 30 ms and nutation frequency 725 Hz at 70 kHz MAS, a good compromise of significant suppression of the methyl resonance combined with the signal intensity of resonances greater than 5 ppm away from the methyl resonance being largely unaffected is achieved. The effectiveness of using a selective saturation pulse is demonstrated for both homonuclear (1)H-(1)H double quantum (DQ)/single quantum (SQ) MAS and (14)N-(1)H heteronuclear multiple quantum coherence (HMQC) two-dimensional solid-state NMR experiments.

  10. Magic angle Lee-Goldburg frequency offset irradiation improves the efficiency and selectivity of SPECIFIC-CP in triple-resonance MAS solid-state NMR.

    PubMed

    Wu, Chin H; De Angelis, Anna A; Opella, Stanley J

    2014-09-01

    The efficiency and selectivity of SPECIFIC-CP, a widely used method for selective double cross-polarization in triple-resonance magic angle spinning solid-state NMR, is improved by performing the tangential-shaped (13)C irradiation at an offset frequency that meets the Lee-Goldburg condition (LG-SPECIFIC-CP). This is demonstrated on polycrystalline samples of uniformly (13)C, (15)N labeled N-acetyl-leucine and N-formyl-Met-Leu-Phe-OH (MLF) at 700MHz and 900MHz (1)H resonance frequencies, respectively. For the single (13)Cα of N-acetyl-leucine, relative to conventional broad band cross-polarization, the SPECIFIC-CP signal has 47% of the intensity. Notably, the LG-SPECIFIC-CP signal has 72% of the intensity, essentially the theoretical maximum. There were no other changes in the experimental parameters. The three (13)Cα signals in MLF show some variation in intensities, reflecting the relatively narrow bandwidth of a frequency-offset procedure, and pointing to future developments for this class of experiment. Copyright © 2014 Elsevier Inc. All rights reserved.

  11. Characterization of fungal-degraded lime wood by X-ray diffraction and cross-polarization magic-angle-spinning 13C-nuclear magnetic resonance spectroscopy.

    PubMed

    Popescu, Carmen-Mihaela; Larsson, Per Tomas; Tibirna, Carmen Mihaela; Vasile, Cornelia

    2010-09-01

    X-ray diffraction, scanning electron microscopy (SEM), and solid-state cross-polarization magic-angle-spinning (CP/MAS) (13)C-NMR spectroscopy were applied to determine changes over time in the morphology and crystallinity of lime wood (Tilia cordata Miller) generated by the soft-rot fungi. Wood samples were inoculated with Trichoderma viride Pers for various durations up to 84 days. Structural and morphological modifications were assessed by comparing the structural features of decayed lime wood samples with references. Significant morphology changes such as defibration or small cavities were clearly observed on the SEM micrographs of lime wood samples exposed to fungi. Following the deconvolution process of the diffraction patterns, the degree of crystallinity, apparent lateral crystallite size, the proportion of crystallite interior chains, and the cellulose fraction have been determined. It was found that all crystallographic data vary with the duration of exposure to fungi. The degree of crystallinity and cellulose fraction tend to decrease, whereas the apparent lateral crystallite size and the proportion of crystallite interior chains increase with prolonged biodegradation processes. The most relevant signals in CP/MAS (13)C-NMR spectra were assigned according to literature data. The differences observed were discussed in terms of lignin and cellulose composition: by fixing the lignin reference signal intensity, the cellulose and hemicelluloses moieties showed a relative decrease compared to the lignin signals in decayed wood.

  12. NON-DESTRUCTIVE METHOD AND MEANS FOR FLAW DETECTION

    DOEpatents

    Hochschild, R.

    1959-03-10

    BS>An improved method is presented for the nondestructive detection of flaws in olectrictilly conductivc articles using magnetic field. According to thc method a homogoneous mignetic field is established in the test article;it right angle" to the artyicle. A probe is aligned with its axis transverse to the translates so hat th4 probe scans the surface of the test article while the axis of the robe is transverse to the direction of translation of the article. In this manner any output current obtained in thc probe is an indication of the size and location of a flaw in the article under test, with a miiiimum of signal pick- up in the probe from the established magnetic field.

  13. Cs/CsPbX3 (X = Br, Cl) epitaxial heteronanocrystals with magic-angle stable/metastable grain boundary

    NASA Astrophysics Data System (ADS)

    Zhang, Yumeng; Fan, Baolu; Wu, Wenhui; Fan, Jiyang

    2017-05-01

    Metal-semiconductor heteronanostructures are crucial building blocks of nanoscale electronic and optoelectronic devices. However, the lattice misfit remains a challenge in constructing heteronanostructures. Perovskite nanocrystals are superior candidates for constructing nanodevices owing to excellent optical, ferroelectric, and superconducting properties. We report the epitaxial growth of lattice-matched Cs/CsPbBr3 metal-semiconductor heteronanocrystals in a liquid medium. The well-crystallized ultrathin Cs layers grow epitaxially on the surfaces of colloidal CsPbBr3 nanocrystals, forming heteronanocrystals with interface diameters of several nanometers. Most of them are pseudomorphic with coherent interfaces free from dislocations, and the others exhibit discrete high-angle grain boundaries. The model based on the calculation of the elastic potential energy of the epilayer and analysis of the near-coincidence sites explains well the experimental result. The analysis shows that the excellent lattice match between the metal and the semiconductor ensures the ideal epitaxial-growth of both Cs/CsPbBr3 and Cs/CsPbCl3 heteronanocrystals. Such metal/semiconductor heteronanocrystals pave the way for developing perovskite-based nanodevices.

  14. Non-Destructive Evaluation of Wire Insulation and Coatings

    NASA Technical Reports Server (NTRS)

    Madaras, Eric I (Inventor); Anastasi, Robert F. (Inventor)

    2004-01-01

    The present invention uses the generation and detection of acoustic guided waves to evaluate the condition of the insulation on electrical wiring. Low order axisymmetric and flexural acoustic modes are generated in the insulated wire and travel partially in the center conductor and partially in the outer insulation. The stiffness of the insulation and the insulation's condition affect the overall wave speed and amplitude of the guided wave. Analysis of the received signal provides information about the age or useful life of the wire insulation. In accordance with the present invention, signal transmission occurs at one location on the electrical wire to be evaluated, and detection occurs at one or more locations along the electrical wire. Additional receivers can be used to improve measurement accuracy. Either the transmission transducer or one or more receiver transducers may be angled at other than 90 degrees to the wire. Generation of the guided waves can be accomplished by imparting a pressure pulse on the wire. Alternative embodiments include generation via a laser, such as a Q-switched laser or a laser diode.

  15. Selective excitation enables assignment of proton resonances and (1)H-(1)H distance measurement in ultrafast magic angle spinning solid state NMR spectroscopy.

    PubMed

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy

    2015-07-21

    Remarkable developments in ultrafast magic angle spinning (MAS) solid-state NMR spectroscopy enabled proton-based high-resolution multidimensional experiments on solids. To fully utilize the benefits rendered by proton-based ultrafast MAS experiments, assignment of (1)H resonances becomes absolutely necessary. Herein, we propose an approach to identify different proton peaks by using dipolar-coupled heteronuclei such as (13)C or (15)N. In this method, after the initial preparation of proton magnetization and cross-polarization to (13)C nuclei, transverse magnetization of desired (13)C nuclei is selectively prepared by using DANTE (Delays Alternating with Nutations for Tailored Excitation) sequence and then, it is transferred to bonded protons with a short-contact-time cross polarization. Our experimental results demonstrate that protons bonded to specific (13)C atoms can be identified and overlapping proton peaks can also be assigned. In contrast to the regular 2D HETCOR experiment, only a few 1D experiments are required for the complete assignment of peaks in the proton spectrum. Furthermore, the finite-pulse radio frequency driven recoupling sequence could be incorporated right after the selection of specific proton signals to monitor the intensity buildup for other proton signals. This enables the extraction of (1)H-(1)H distances between different pairs of protons. Therefore, we believe that the proposed method will greatly aid in fast assignment of peaks in proton spectra and will be useful in the development of proton-based multi-dimensional solid-state NMR experiments to study atomic-level resolution structure and dynamics of solids.

  16. Selective excitation enables assignment of proton resonances and {sup 1}H-{sup 1}H distance measurement in ultrafast magic angle spinning solid state NMR spectroscopy

    SciTech Connect

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy

    2015-07-21

    Remarkable developments in ultrafast magic angle spinning (MAS) solid-state NMR spectroscopy enabled proton-based high-resolution multidimensional experiments on solids. To fully utilize the benefits rendered by proton-based ultrafast MAS experiments, assignment of {sup 1}H resonances becomes absolutely necessary. Herein, we propose an approach to identify different proton peaks by using dipolar-coupled heteronuclei such as {sup 13}C or {sup 15}N. In this method, after the initial preparation of proton magnetization and cross-polarization to {sup 13}C nuclei, transverse magnetization of desired {sup 13}C nuclei is selectively prepared by using DANTE (Delays Alternating with Nutations for Tailored Excitation) sequence and then, it is transferred to bonded protons with a short-contact-time cross polarization. Our experimental results demonstrate that protons bonded to specific {sup 13}C atoms can be identified and overlapping proton peaks can also be assigned. In contrast to the regular 2D HETCOR experiment, only a few 1D experiments are required for the complete assignment of peaks in the proton spectrum. Furthermore, the finite-pulse radio frequency driven recoupling sequence could be incorporated right after the selection of specific proton signals to monitor the intensity buildup for other proton signals. This enables the extraction of {sup 1}H-{sup 1}H distances between different pairs of protons. Therefore, we believe that the proposed method will greatly aid in fast assignment of peaks in proton spectra and will be useful in the development of proton-based multi-dimensional solid-state NMR experiments to study atomic-level resolution structure and dynamics of solids.

  17. Selective excitation enables assignment of proton resonances and 1H-1H distance measurement in ultrafast magic angle spinning solid state NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Zhang, Rongchun; Ramamoorthy, Ayyalusamy

    2015-07-01

    Remarkable developments in ultrafast magic angle spinning (MAS) solid-state NMR spectroscopy enabled proton-based high-resolution multidimensional experiments on solids. To fully utilize the benefits rendered by proton-based ultrafast MAS experiments, assignment of 1H resonances becomes absolutely necessary. Herein, we propose an approach to identify different proton peaks by using dipolar-coupled heteronuclei such as 13C or 15N. In this method, after the initial preparation of proton magnetization and cross-polarization to 13C nuclei, transverse magnetization of desired 13C nuclei is selectively prepared by using DANTE (Delays Alternating with Nutations for Tailored Excitation) sequence and then, it is transferred to bonded protons with a short-contact-time cross polarization. Our experimental results demonstrate that protons bonded to specific 13C atoms can be identified and overlapping proton peaks can also be assigned. In contrast to the regular 2D HETCOR experiment, only a few 1D experiments are required for the complete assignment of peaks in the proton spectrum. Furthermore, the finite-pulse radio frequency driven recoupling sequence could be incorporated right after the selection of specific proton signals to monitor the intensity buildup for other proton signals. This enables the extraction of 1H-1H distances between different pairs of protons. Therefore, we believe that the proposed method will greatly aid in fast assignment of peaks in proton spectra and will be useful in the development of proton-based multi-dimensional solid-state NMR experiments to study atomic-level resolution structure and dynamics of solids.

  18. Insights into atomic-level interaction between mefenamic acid and eudragit EPO in a supersaturated solution by high-resolution magic-angle spinning NMR spectroscopy.

    PubMed

    Higashi, Kenjirou; Yamamoto, Kazutoshi; Pandey, Manoj Kumar; Mroue, Kamal H; Moribe, Kunikazu; Yamamoto, Keiji; Ramamoorthy, Ayyalusamy

    2014-01-06

    The intermolecular interaction between mefenamic acid (MFA), a poorly water-soluble nonsteroidal anti-inflammatory drug, and Eudragit EPO (EPO), a water-soluble polymer, is investigated in their supersaturated solution using high-resolution magic-angle spinning (HRMAS) nuclear magnetic resonance (NMR) spectroscopy. The stable supersaturated solution with a high MFA concentration of 3.0 mg/mL is prepared by dispersing the amorphous solid dispersion into a d-acetate buffer at pH 5.5 and 37 °C. By virtue of MAS at 2.7 kHz, the extremely broad and unresolved (1)H resonances of MFA in one-dimensional (1)H NMR spectrum of the supersaturated solution are well-resolved, thus enabling the complete assignment of MFA (1)H resonances in the aqueous solution. Two-dimensional (2D) (1)H/(1)H nuclear Overhauser effect spectroscopy (NOESY) and radio frequency-driven recoupling (RFDR) under MAS conditions reveal the interaction of MFA with EPO in the supersaturated solution at an atomic level. The strong cross-correlations observed in the 2D (1)H/(1)H NMR spectra indicate a hydrophobic interaction between the aromatic group of MFA and the backbone of EPO. Furthermore, the aminoalkyl group in the side chain of EPO forms a hydrophilic interaction, which can be either electrostatic or hydrogen bonding, with the carboxyl group of MFA. We believe these hydrophobic and hydrophilic interactions between MFA and EPO molecules play a key role in the formation of this extremely stable supersaturated solution. In addition, 2D (1)H/(1)H RFDR demonstrates that the molecular MFA-EPO interaction is quite flexible and dynamic.

  19. High-Resolution Magic-Angle Spinning-(1)H NMR Spectroscopy-Based Metabolic Profiling of Hippocampal Tissue in Rats with Depression-Like Symptoms.

    PubMed

    Akimoto, Hayato; Oshima, Shinji; Ohara, Kousuke; Negishi, Akio; Hiroyama, Hanako; Nemoto, Tadashi; Kobayashi, Daisuke

    2017-03-04

    Depressive disorders cause large socioeconomic effects influencing not only the patients themselves but also their family and broader community as well. To better understand the physiologic factors underlying depression, in this study, we performed metabolomics analysis, an omics technique that comprehensively analyzes small molecule metabolites in biological samples. Specifically, we utilized high-resolution magic-angle spinning-(1)H NMR (HRMAS-(1)H NMR) spectroscopy to comprehensively analyze the changes in metabolites in the hippocampal tissue of rats exposed to chronic stress (CS) via multi-step principal component analysis (multi-step PCA). The rats subjected to CS exhibited obvious depression-like behaviors. High correlations were observed between the first principal component (PC1) score in the score plot obtained using multi-step PCA and measurements from depression-like behavioral testing (body weight, sucrose preference test, and open field test). Alanine, glutamate, glutamine, and aspartate levels in the hippocampal tissue were significantly lower, whereas N-acetylaspartate, myo-inositol, and creatine were significantly higher in the CS group compared to the control (non-CS) group. As alanine, glutamate, and glutamine are known to be involved in energy metabolism, especially in the TCA cycle, chronic exogenous stress may have induced abnormalities in energy metabolism in the brains of the rats. The results suggest that N-acetylaspartate and creatine levels may have increased in order to complement the loss of energy-producing activity resulting from the development of the depression-like disorder. Multi-step PCA therefore allowed an exploration of the degree of depression-like symptoms as represented by changes in intrinsic metabolites.

  20. The combined effect of quadrupolar and dipolar interactions on the excitation and evolution of triple quantum coherences in ⁷Li solid state magic angle spinning NMR.

    PubMed

    Eliav, Uzi; Goldbourt, Amir

    2013-05-01

    Magic-angle spinning triple-quantum NMR spectra of lithium-7 provide enhanced spectral dispersion for the inherent low chemical shift range of this nucleus, while maintaining linewidths, which are free of any quadrupolar broadening to first order. Since the quadrupolar interaction of (7)Li is very small, in the order of the radio frequency nutation frequencies and only moderately larger than the spinning rates, such spectra are also only marginally affected by the second order quadrupolar interaction under large magnetic fields. In the current study we demonstrate that the existence of two and more proximate (7)Li spins, as encountered in many materials, affects both excitation and evolution of triple-quantum coherences due to the combined effect of quadrupolar and homonuclear dipolar interactions. We show that the generation of (7)Li triple-quantum coherences using two π/2 pulses separated by one-half rotor period is superior in such cases to a single pulse excitation since the excitation time is shorter; thus the maximum signal is only marginally affected by the homonuclear dipolar couplings. When the quadrupolar-dipolar cross terms dominate the spectra, single- and triple-quantum lineshapes are very similar and therefore a true gain in dispersion is maintained in the latter spectrum. The effects of quadrupolar-dipolar cross terms are experimentally demonstrated by comparing a natural abundance and a (6)Li-diluted samples of lithium acetate, resulting in the possibility of efficient excitation of triple quantum coherences over longer periods of time, and in longer life times of triple-quantum coherences. Copyright © 2013 Elsevier Inc. All rights reserved.

  1. Fast Magic-Angle Spinning Three-Dimensional NMR Experiment for Simultaneously Probing H-H and N-H Proximities in Solids.

    PubMed

    Reddy, G N Manjunatha; Malon, Michal; Marsh, Andrew; Nishiyama, Yusuke; Brown, Steven P

    2016-12-06

    A fast magic-angle spinning (MAS, 70 kHz) solid-state NMR experiment is presented that combines (1)H Double-Quantum (DQ) and (14)N-(1)H HMQC (Heteronuclear Multiple-Quantum Coherence) pulse-sequence elements, so as to simultaneously probe H-H and N-H proximities in molecular solids. The proposed experiment can be employed in both two-dimensional (2D) and three-dimensional (3D) versions: first, a 2D (14)N HMQC-filtered (1)H-DQ experiment provides specific DQ-SQ correlation peaks for proton pairs that are in close proximities to the nitrogen sites, thereby achieving spectral filtration. Second, a proton-detected three-dimensional (3D) (1)H(DQ)-(14)N(SQ)-(1)H(SQ) experiment correlates (1)H(DQ)-(1)H(SQ) chemical shifts with (14)N shifts such that longer range N···H-H correlations are observed between protons and nitrogen atoms with internuclear NH distances exceeding 3 Å. Both 2D and 3D versions of the proposed experiment are demonstrated for an amino acid hydrochloride salt, l-histidine·HCl·H2O, and a DNA nucleoside, guanosine·2H2O. In the latter case, the achieved spectral filtration ensures that DQ cross peaks are only observed for guanine NH and CH8 (1)H resonances and not ribose and water (1)H resonances, thus providing insight into the changes in the solid-state structure of this hydrate that occur over time; significant changes are observed in the NH and NH2(1)H chemical shifts as compared to the freshly recrystallized sample previously studied by Reddy et al., Cryst. Growth Des. 2015, 15, 5945.

  2. Analysis of metabolic characteristics in a rat model of chronic pancreatitis using high-resolution magic-angle spinning nuclear magnetic resonance spectroscopy.

    PubMed

    Tian, Bing; Ma, Chao; Wang, Jian; Pan, Chun-Shu; Yang, Gen-Jin; Lu, Jian-Ping

    2015-01-01

    Pathological and metabolic alterations co-exist and co-develop in the progression of chronic pancreatitis (CP). The aim of the present study was to investigate the metabolic characteristics and disease severity of a rat model of CP in order to determine associations in the observed pathology and the metabolites of CP using high-resolution magic-angle spinning nuclear magnetic resonance spectroscopy (HR-MAS NMR). Wistar rats (n=36) were randomly assigned into 6 groups (n=6 per group). CP was established by administering dibutyltin dichloride solution into the tail vein. After 0, 7, 14, 21, 28 and 35 days, the pancreatic tissues were collected for pathological scoring or for HR-MAS NMR. Correlation analyses between the major pathological scores and the integral areas of the major metabolites were determined. The most representative metabolites, aspartate, betaine and fatty acids, were identified as possessing the greatest discriminatory significance. The Spearman's rank correlation coefficients between the pathology and metabolites of the pancreatic tissues were as follows: Betaine and fibrosis, 0.454 (P=0.044); betaine and inflammatory cell infiltration, 0.716 (P=0.0001); aspartate and fibrosis, -0.768 (P=0.0001); aspartate and inflammatory cell infiltration, -0.394 (P=0.085); fatty acid and fibrosis, -0.764 (P=0.0001); and fatty acid and inflammatory cell infiltration, -0.619 (P=0.004). The metabolite betaine positively correlated with fibrosis and inflammatory cell infiltration in CP. In addition, aspartate negatively correlated with fibrosis, but exhibited no significant correlation with inflammatory cell infiltration. Furthermore, the presence of fatty acids negatively correlated with fibrosis and inflammatory cell infiltration in CP. HR-MAS NMR may be used to analyze metabolic characteristics in a rat model of different degrees of chronic pancreatitis.

  3. Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies.

    PubMed

    Mote, Kaustubh R; Madhu, Perunthiruthy K

    2015-12-01

    (1)H-detection offers a substitute to the sensitivity-starved experiments often used to characterize biomolecular samples using magic-angle spinning solid-state NMR spectroscopy (MAS-ssNMR). To mitigate the effects of the strong (1)H-(1)H dipolar coupled network that would otherwise severely broaden resonances, high MAS frequencies (>40kHz) are often employed. Here, we have explored the alternative of stroboscopic (1)H-detection at moderate MAS frequencies of 5-30kHz using windowed version of supercycled-phase-modulated Lee-Goldburg homonuclear decoupling. We show that improved resolution in the (1)H dimension, comparable to that obtainable at high spinning frequencies of 40-60kHz without homonuclear decoupling, can be obtained in these experiments for fully protonated proteins. Along with detailed analysis of the performance of the method on the standard tri-peptide f-MLF, experiments on micro-crystalline GB1 and amyloid-β aggregates are used to demonstrate the applicability of these pulse-sequences to challenging biomolecular systems. With only two parameters to optimize, broadbanded performance of the homonuclear decoupling sequence, linear dependence of the chemical-shift scaling factor on resonance offset and a straightforward implementation under experimental conditions currently used for many biomolecular studies (viz. spinning frequencies and radio-frequency amplitudes), we expect these experiments to complement the current (13)C-detection based methods in assignments and characterization through chemical-shift mapping. Copyright © 2015 Elsevier Inc. All rights reserved.

  4. High-Resolution Magic Angle Spinning Nuclear Magnetic Resonance Spectroscopy for the Metabolic Assessment of Acute Rejection After Cardiac Transplantation in Rats.

    PubMed

    Lee, C W; Lee, J S; Woo, C W; Kim, S

    2017-10-01

    To evaluate the potential of high-resolution magic angle spinning (HR-MAS) (1)H nuclear magnetic resonance (NMR) spectroscopy for metabolite characterization and the differentiation of acute rejection after heart transplantation in rat models. We transplanted syngeneic heart grafts from Lewis rats (n = 4) and allogeneic heart grafts from F344 rats (n = 4) heterotopically into Lewis recipients. On day 7 postoperatively, the transplanted hearts were harvested for ex vivo (1)H NMR spectroscopy and HR-MAS (1)H NMR spectroscopy. (1)H NMR spectroscopy and HR-MAS (1)H NMR spectroscopy were performed at 4.7 T and 11.7 T, respectively. Metabolomic profiles contributing to the differentiation of allogeneic and syngeneic graft groups were statistically assessed by orthogonal partial least squares discriminant analysis (OPLS/O2PLS-DA). Metabolite concentrations were normalized by total spectral intensities and were compared using Mann-Whitney U tests. One allogeneic graft that showed extensive necrotic change suggesting graft failure was excluded from the statistical analysis of the NMR spectroscopy. In the 4.7-T (1)H NMR spectroscopy, the creatine peak was decreased in the allogeneic group. The PLS-DA and OPLS/O2PLS-DA score plot demonstrated good discrimination of the allogeneic graft group from syngeneic graft group. The concentrations of creatine, myo-inositol, glucose, niacinamide, hypoxanthine, inosine, and glutamine were significantly decreased in the allogeneic graft group, whereas the concentrations of glycine, phosphoethanolamine, xanthine, sn-glycero-3-phosphocholine, leucine, valine, and tyrosine were significantly increased (P < .05). HR-MAS (1)H NMR spectroscopy can metabolically characterize the acute rejection of heart transplantation. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. A Large Sample Volume Magic Angle Spinning Nuclear Magnetic Resonance Probe for In-Situ Investigations with Constant Flow of Reactants

    SciTech Connect

    Hu, Jian Z.; Sears, Jesse A.; Mehta, Hardeep S.; Ford, Joseph J.; Kwak, Ja Hun; Zhu, Kake; Wang, Yong; Liu, Jun; Hoyt, David W.; Peden, Charles HF

    2012-02-21

    A large-sample-volume constant-flow magic angle sample spinning (CF-MAS) NMR probe is reported for in-situ studies of the reaction dynamics, stable intermediates/transition states, and mechanisms of catalytic reactions. In our approach, the reactants are introduced into the catalyst bed using a fixed tube at one end of the MAS rotor while a second fixed tube, linked to a vacuum pump, is attached at the other end of the rotor. The pressure difference between both ends of the catalyst bed inside the sample cell space forces the reactants flowing through the catalyst bed, which improves the diffusion of the reactants and products. This design allows the use of a large sample volume for enhanced sensitivity and thus permitting in-situ 13C CF-MAS studies at natural abundance. As an example of application, we show that reactants, products and reaction transition states associated with the 2-butanol dehydration reaction over a mesoporous silicalite supported heteropoly acid catalyst (HPA/meso-silicalite-1) can all be detected in a single 13C CF-MAS NMR spectrum at natural abundance. Coke products can also be detected at natural 13C abundance and under the stopped flow condition. Furthermore, 1H CF-MAS NMR is used to identify the surface functional groups of HPA/meso-silicalite-1 under the condition of in-situ drying . We also show that the reaction dynamics of 2-butanol dehydration using HPA/meso-silicalite-1 as a catalyst can be explored using 1H CF-MAS NMR.

  6. Nanostructures of Mg0.65Ti0.35Dx studied with x-ray diffraction, neutron diffraction, and magic-angle-spinning H2 NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Srinivasan, S.; Magusin, P. C. M. M.; Kalisvaart, W. P.; Notten, P. H. L.; Cuevas, F.; Latroche, M.; van Santen, R. A.

    2010-02-01

    Magnesium transition-metal alloys have a high hydrogen-storage capacity and show improved hydrogen-uptake and -release kinetics compared to magnesium alone. In the present study we have investigated the structure of bulk magnesium-titanium deuteride Mg0.65Ti0.35Dx prepared via mechanical alloying and gas-phase deuterium absorption by combined use of x-ray diffraction (XRD), neutron diffraction, and magic-angle-spinning H2 nuclear magnetic resonance (NMR). The initial ball-milled alloy has two XRD-distinct Mg and Ti fcc phases. Even after prolonged exposure to deuterium gas at 75 bar and 175°C the materials with and without palladium catalyst are only partly deuterated. Deuterium loading causes the formation of, on the one hand, bct (rutile) MgD2 nanodomains with interdispersed TiDy layers and, on the other hand, a separate fcc (fluorite) TiDz phase. The TiDy phase is XRD invisible, but shows clearly up at a H2 NMR shift of -43ppm between the shift of MgD2 (3 ppm) and the Knight shift of the TiDz phase (-143ppm) . Exchange NMR indicates complete deuterium exchange at 25°C between the MgD2 and TiDy phase within 1 s, as consistent with intimate contacts between these phases. Combined analysis of the XRD and NMR peak areas suggests that the deuterium concentrations y and z in the TiDy and TiDz domains are about 1.5 and 2.0, respectively. Comparing the intrinsic cell parameters of rutile MgH2 and fluorite TiH2 , we propose that stabilization of the mixed nanocomposite may arise from a coherent coupling between the crystal structures of the rutile MgD2 nanodomains and the thin layers of fcc TiDy .

  7. High-Resolution Magic Angle Spinning Nuclear Magnetic Resonance of Intact Zebrafish Embryos Detects Metabolic Changes Following Exposure to Teratogenic Polymethoxyalkenes from Algae.

    PubMed

    Berry, John P; Roy, Upasana; Jaja-Chimedza, Asha; Sanchez, Kristel; Matysik, Joerg; Alia, A

    2016-10-01

    Techniques based on nuclear magnetic resonance (NMR) for imaging and chemical analyses of in vivo, or otherwise intact, biological systems are rapidly emerging and finding diverse applications within a wide range of fields. Very recently, several NMR-based techniques have been developed for the zebrafish as a model animal system. In the current study, the novel application of high-resolution magic angle spinning (HR-MAS) NMR is presented as a means of metabolic profiling of intact zebrafish embryos. Toward investigating the utility of HR-MAS NMR as a toxicological tool, these studies specifically examined metabolic changes of embryos exposed to polymethoxy-1-alkenes (PMAs)-a recently identified family of teratogenic compounds from freshwater algae-as emerging environmental contaminants. One-dimensional and two-dimensional HR-MAS NMR analyses were able to effectively identify and quantify diverse metabolites in early-stage (≤36 h postfertilization) embryos. Subsequent comparison of the metabolic profiles between PMA-exposed and control embryos identified several statistically significant metabolic changes associated with subacute exposure to the teratogen, including (1) elevated inositol as a recognized component of signaling pathways involved in embryo development; (2) increases in several metabolites, including inositol, phosphoryl choline, fatty acids, and cholesterol, which are associated with lipid composition of cell membranes; (3) concomitant increase in glucose and decrease in lactate; and (4) decreases in several biochemically related metabolites associated with central nervous system development and function, including γ-aminobutyric acid, glycine, glutamate, and glutamine. A potentially unifying model/hypothesis of PMA teratogenicity based on the data is presented. These findings, taken together, demonstrate that HR-MAS NMR is a promising tool for metabolic profiling in the zebrafish embryo, including toxicological applications.

  8. Magic Angle Spinning Nuclear Magnetic Resonance Characterization of Voltage-Dependent Anion Channel Gating in Two-Dimensional Lipid Crystalline Bilayers

    PubMed Central

    2015-01-01

    The N-terminus of the voltage-dependent anion channel (VDAC) has been proposed to contain the mechanistically important gating helices that modulate channel opening and closing. In this study, we utilize magic angle spinning nuclear magnetic resonance (MAS NMR) to determine the location and structure of the N-terminus for functional channels in lipid bilayers by measuring long-range 13C–13C distances between residues in the N-terminus and other domains of VDAC reconstituted into DMPC lipid bilayers. Our structural studies show that the distance between A14 Cβ in the N-terminal helix and S193 Cβ is ∼4–6 Å. Furthermore, VDAC phosphorylation by a mitochondrial kinase at residue S193 has been claimed to delay mitochondrial cell death by causing a conformational change that closes the channel, and a VDAC-Ser193Glu mutant has been reported to show properties very similar to those of phosphorylated VDAC in a cellular context. We expressed VDAC-S193E and reconstituted it into DMPC lipid bilayers. Two-dimensional 13C–13C correlation experiments showed chemical shift perturbations for residues located in the N-terminus, indicating possible structural perturbations to that region. However, electrophysiological data recorded on VDAC-S193E showed that channel characteristics were identical to those of wild type samples, indicating that phosphorylation of S193 does not directly affect channel gating. The combination of NMR and electrophysiological results allows us to discuss the validity of proposed gating models. PMID:25545271

  9. Assignment strategies for large proteins by magic-angle spinning NMR: the 21-kDa disulfide bond forming enzyme DsbA

    PubMed Central

    Sperling, Lindsay J.; Berthold, Deborah A.; Sasser, Terry L.; Jeisy-Scott, Victoria; Rienstra, Chad M.

    2010-01-01

    Summary We present strategies for chemical shift assignments of large proteins by magic-angle spinning (MAS) solid-state NMR (SSNMR), using the 21-kDa disulfide bond forming enzyme DsbA as a prototype. Previous studies have demonstrated that complete de novo assignments are possible for proteins up to ~17 kDa, and partial assignments have been performed for several larger proteins. Here we show that combinations of isotopic labeling strategies, high field correlation spectroscopy and 3D and 4D backbone correlation experiments yield highly confident assignments for more than 90% of the backbone resonances in DsbA. Samples were prepared as nanocrystalline precipitates by a dialysis procedure, resulting in heterogeneous linewidths under 0.2 ppm. Thus, high magnetic fields, selective decoupling pulse sequences, and sparse isotopic labeling all improved spectral resolution. Assignments by amino acid type were facilitated by particular combinations of pulse sequences and isotopic labeling; for example, TEDOR experiments enhanced sensitivity for Pro and Gly residues, 2-13C-glycerol labeling clarified Val, Ile and Leu assignments, IPAP correlation spectra enabled interpretation of otherwise crowded Glx/Asx sidechain regions, and 3D NCACX experiments on 2-13C-glycerol samples provided unique sets of aromatic (Phe, Tyr, Trp) correlations. Together with high sensitivity CANCOCA 4D and CANCOCX 3D experiments, unambiguous backbone walks could be performed throughout the majority of the sequence. At 189 residues, DsbA represents the largest monomeric unit for which essentially complete solid-state NMR assignments have so far been achieved. These results will facilitate studies of nanocrystalline DsbA structure and dynamics and enable analysis of its 41-kDa covalent complex with the membrane protein DsbB, for which we demonstrate a high-resolution 2D 13C-13C spectrum. PMID:20394752

  10. Quantification of amounts and (13)C content of metabolites in brain tissue using high- resolution magic angle spinning (13)C NMR spectroscopy.

    PubMed

    Risa, Oystein; Melø, Torun Margareta; Sonnewald, Ursula

    2009-04-01

    Metabolic pathway mapping using (13)C NMR spectroscopy has been used extensively to study interactions between neurons and glia in the brain. Established extraction procedures of brain tissue are time consuming and may result in degradation of labile substances. We examined the potential of mapping (13)C-enriched compounds in intact brain tissue using high-resolution magic angle spinning (HR-MAS) NMR spectroscopy. Sprague-Dawley rats received an intraperitoneal injection of [1,6-(13)C]glucose, and 15 min later the animals were subjected to microwave fixation of the brain. Quantification of concentration and (13)C labelling of metabolites in intact rat thalamus were carried out based on exogenous ethylene glycol concentrations measured from (1)H NMR spectra using an ERETIC (Electronic REference To access In vivo Concentrations) signal. The results from intact tissue were compared with those from perchloric acid-extracted brain tissue. Amounts of (13)C labelling at different positions (C2, C3 and C4) in glutamate, glutamine, gamma-aminobutyric acid and aspartate measured in either intact tissue or perchloric acid extracts were not significantly different. Proton NMR spectra were used for quantification of six different amino acids plus lactate, inositol, N-acetylaspartate, creatine and phosphocreatine. Again, results were very similar when comparing the methods. To our knowledge, this is the first time quantitative (13)C NMR spectroscopy measurements have been carried out on intact brain tissue ex vivo using the HR-MAS technique. The results show that HR-MAS (13)C NMR spectroscopy in combination with (1)H NMR spectroscopy and the ERETIC method is useful for metabolic studies of intact brain tissue ex vivo.

  11. Carbon-13 cross-polarization magic-angle-spinning nuclear magnetic resonance investigation of the interactions between maleic anhydride grafted polypropylene and wood polymers.

    PubMed

    Rude, Erica; Laborie, Marie-Pierre G

    2008-05-01

    The chemical interactions between maleic anhydride grafted polypropylene (MAPP) and wood were studied with solid-state carbon-13 cross-polarization magic-angle-spinning nuclear magnetic resonance ((13)C CPMAS NMR) spectroscopy. MAPP was synthesized with 100% (13)C enrichment at the C(1) and C(4) carbons to allow detection of the [1,4-(13)C(2)]MAPP functional groups and was melt blended with cellulose, lignin, and maple wood. In the cellulose/MAPP blend, changes in (13)C CPMAS NMR corrected signal intensities for the anhydride and dicarboxylic maleic acid functionalities suggested that esterification may have occurred predominantly from the more numerous diacid carbons. A single proton longitudinal relaxation in the rotating frame, (H)T(1rho), for the MAPP and the cellulose carbons in the blend suggested that they were spin coupled, i.e., homogeneous on a 10-200 Angstrom scale. Esterification was also suggested in the lignin/MAPP blend. Furthermore, the more significant changes in the intensities of the carbonyl signals and (H)T(1rho) values suggested that lignin may be more reactive to MAPP than cellulose. Finally, when maple was melt blended with MAPP, the same trends in the (13)C CP-MAS NMR spectra and (H)T(1rho) behavior were observed as when MAPP was blended with cellulose or lignin. This study therefore clarifies that during melt compounding of wood with MAPP, esterification occurs with wood polymers, preferentially with lignin. Understanding the interactions of MAPP with wood is of significance for the development of natural-fiber-reinforced thermoplastic composites.

  12. Prediction of Eggshell Ultrastructure via Some Non-destructive and Destructive Measurements in Fayoumi Breed

    PubMed Central

    Radwan, Lamiaa M.; Galal, A.; Shemeis, A. R.

    2015-01-01

    Possibilities of predicting eggshell ultrastructure from direct non-destructive and destructive measurements were examined using 120 Fayoumi eggs collected from the flock at 45 weeks of age. The non-destructive measurements included weight, length and width of the egg. The destructive measurements were breaking strength and shell thickness. The eggshell ultrastructure traits involved the total thickness of eggshell layer, thickness of palisade layer, cone layer and total score. Prediction of total thickness of eggshell layer based on non-destructive measurements individually or simultaneously was not possible (R2 = 0.01 to 0.16). The destructive measurements were far more accurate than the non-destructive in predicting total thickness of eggshell layer. Prediction based on breaking strength alone was more accurate (R2 = 0.85) than that based on shell thickness alone (R2 = 0.72). Adding shell thickness to breaking strength (the best predictor) increased the accuracy of prediction by 5%. The results obtained indicated that both non-destructive and destructive measurements were not useful in predicting the cone layer (R2 not exceeded 18%). The maximum accuracy of prediction of total score (R2 = 0.48) was obtained from prediction based on breaking strength alone. Combining shell thicknesses and breaking strength into one equation was no help in improving the accuracy of prediction. PMID:26104404

  13. Prediction of Eggshell Ultrastructure via Some Non-destructive and Destructive Measurements in Fayoumi Breed.

    PubMed

    Radwan, Lamiaa M; Galal, A; Shemeis, A R

    2015-07-01

    Possibilities of predicting eggshell ultrastructure from direct non-destructive and destructive measurements were examined using 120 Fayoumi eggs collected from the flock at 45 weeks of age. The non-destructive measurements included weight, length and width of the egg. The destructive measurements were breaking strength and shell thickness. The eggshell ultrastructure traits involved the total thickness of eggshell layer, thickness of palisade layer, cone layer and total score. Prediction of total thickness of eggshell layer based on non-destructive measurements individually or simultaneously was not possible (R(2) = 0.01 to 0.16). The destructive measurements were far more accurate than the non-destructive in predicting total thickness of eggshell layer. Prediction based on breaking strength alone was more accurate (R(2) = 0.85) than that based on shell thickness alone (R(2) = 0.72). Adding shell thickness to breaking strength (the best predictor) increased the accuracy of prediction by 5%. The results obtained indicated that both non-destructive and destructive measurements were not useful in predicting the cone layer (R(2) not exceeded 18%). The maximum accuracy of prediction of total score (R(2) = 0.48) was obtained from prediction based on breaking strength alone. Combining shell thicknesses and breaking strength into one equation was no help in improving the accuracy of prediction.

  14. Non-destructive monitoring of layered infrastructure using GPR data

    NASA Astrophysics Data System (ADS)

    Slob, Evert

    2013-04-01

    In most societies infrastructure is a high-value asset that requires secure and safe accessibility for all users. Security and safety can be guaranteed up to a certain extent and monitoring the fate of these infrastructures is important to allow emergency situations and the occurrence of damage to be detected in near real time. This can be done by analyzing images of the state of the infrastructure in question. These images must be obtained in a non-destrcutive way. Electromagnetic methods are among the most viable technologies for providing the required information at sufficient level of detail and ground-penetrating radar is one of the best candidates to be part of such a tool. Current sensing technologies allow ground-penetrating radar antennas and radar equipment to acquire high-quality, multi-offset, and multi-component data very fast. For such data I present a novel imaging technique that requires the subsurface ground-penetrating radar reflection response of a layered lossless medium that can be used on some of the mentioned infrastructures. Multi-component, multi-offset GPR data is necessary to decompose the electromagnetic wavefield into upgoing and downgoing waves. In a layered medium plane wave decomposition simplifies the imaging scheme and for each angle of incidence the subsurface image can be constructed without additional knowledge of the subsurface properties. The subsurface image does not contain effects from multiple reflections present in the data. The image is constructed in an iterative procedure that converges very fast allowing for the development of a near real time processing and imaging tool. Depending on the available bandwidth a very high-resolution image can be obtained at several times in a time-lapse monitoring set up or almost continuously in a permanent monitoring system. I will show the theoretical basis for this scheme and illustrate it with some numerical examples high-lighting the advantages and drawbacks of the method

  15. Non-Destructive Testing A Developing Tool in Science and Engineering

    SciTech Connect

    Lin, Lianshan

    2013-01-01

    Non-destructive testing (NDT), sometimes also known as non-destructive inspection (NDI) or non-destructive examination (NDE), has been applied to solve a wide range of science and industry problems including construction, aerospace, nuclear engineering, manufacturing, space exploration, art objects, forensic studies, biological and medical fields, etc. Without any permanent changing or alteration of testing objects, NDT methods provide great advantages such as increased testing reliability, efficiency, and safety, as well as reduced time and cost. Since the second half of the 20th century, NDT technology has seen significant growth. Depending on the physical properties being measured, NDT techniques can be classified into several branches. This article will provide a brief overview of commonly used NDT methods and their up-to-date progresses including optical examination, radiography, acoustic emission, ultrasonic testing and eddy current testing. For extended reviews on many presently used NDT methods, please refer to articles by Mullins [1, 2].

  16. Non-destructive testing of composite materials using terahertz time-domain spectroscopy

    NASA Astrophysics Data System (ADS)

    Yakovlev, Egor V.; Zaytsev, Kirill I.; Chernomyrdin, Nikita V.; Gavdush, Arsenii A.; Zotov, Arsen K.; Nikonovich, Maxim Y.; Yurchenko, Stanislav O.

    2016-04-01

    Development of novel methods for non-destructive evaluation of composite materials (CMs) at manufacturing and operational stages remains challenging problem of applied physics, optics and material science. In this paper, we have considered the ability to use the terahertz (THz) time-domain spectroscopy (TDS) for non-destructive evaluation of CMs. By combining the TDS technique with appropriate methods of solving the inverse ill-posed problems, we have shown that TDS could be applied for CM testing. At first, we have demonstrated that TDS could be used to control the polymerization process and, as a consequence, the CM binder curing. Secondary, we have shown the ability to detect the internal defects (non-impregnated voids) inside the CMs via the TDS-based THz time-of-flight tomography. Thereby, the results of our study allow highlighting the prospective of non-destructive evaluation of CMs using the TDS.

  17. Comparative analysis of non-destructive methods to control fissile materials in large-size containers

    NASA Astrophysics Data System (ADS)

    Batyaev, V. F.; Sklyarov, S. V.

    2017-09-01

    The analysis of various non-destructive methods to control fissile materials (FM) in large-size containers filled with radioactive waste (RAW) has been carried out. The difficulty of applying passive gamma-neutron monitoring FM in large containers filled with concreted RAW is shown. Selection of an active non-destructive assay technique depends on the container contents; and in case of a concrete or iron matrix with very low activity and low activity RAW the neutron radiation method appears to be more preferable as compared with the photonuclear one. Note to the reader: the pdf file has been changed on September 22, 2017.

  18. Edward's sword? - A non-destructive study of a medieval king's sword

    SciTech Connect

    Segebade, Chr.

    2013-04-19

    Non-destructive and instrumental methods including photon activation analysis were applied in an examination of an ancient sword. It was tried to find indication of forgery or, if authentic, any later processing and alteration. Metal components of the hilt and the blade were analysed by instrumental photon activation. Non-destructive metallurgical studies (hardness measurements, microscopic microstructure analysis) are briefly described, too. The results of these investigations did not yield indication of non-authenticity. This stood in agreement with the results of stylistic and scientific studies by weapon experts.

  19. "Non-destructive" dimensional metrology of EUV resist gratings (Conference Presentation)

    NASA Astrophysics Data System (ADS)

    Kline, R. Joseph; Sunday, Daniel F.; Windover, Donald; Kulmala, Tero S.; Ekinci, Yasin

    2017-03-01

    New critical dimension metrology methods such as critical dimension small angle X-ray scattering (CDSAXS) are being developed to meet the measurement challenges of next generation devices. Two key requirements for any new CD metrology method are non-destructiveness and the measurement speed. We will report on a study of beam damage and scattering strength of two model photoresist systems, HSQ and PMMA. We also will report on the status and initial results from NIST's upgraded lab CDSAXS system. 50 nm pitch line gratings were fabricated in HSQ and PMMA films using EUV interference lithography at the Swiss Light Source. The lines were about 30 nm tall and 20-30 nm wide. The 17 keV CDSAXS exposure time was varied from 0.1 s to 60 s to determine the minimum X-ray exposure required to obtain a satisfactory fit. Normal incident measurements separated by a blanket X-ray exposure were repeated to measure the decrease in scattering intensity with X-ray dose. The PMMA scattering signal was found to decrease by about 80 % before stabilizing at around 15 % of the original scattering intensity. The HSQ scattering signal decreased much less and stabilized at about 80 % of the original scattering intensity. We also conducted a series of variable-angle CDSAXS measurements as a function of blanket X-ray exposure to determine how the shape of the photoresist lines changed during X-ray exposure. For PMMA, we found the line width to remain constant and the line height to decrease from 25 nm to 10 nm during the exposure series. The exposures that damaged the samples corresponded to several hours of exposure to the synchrotron beam in a 100 µm spot and were much longer than what was required to characterize the line gratings. Smaller targets result in a larger dose and could potentially damage the resist in the time required to make a CDSAXS measurement. The large differences in beam damage between PMMA and HSQ show that resist damage from CDSAXS will depend on the particular resist

  20. Magic-angle spinning NMR studies of molecular organization in multibilayers formed by 1-octadecanoyl-2-decanoyl-sn-glycero-3-phosphocholine.

    PubMed Central

    Halladay, H N; Stark, R E; Ali, S; Bittman, R

    1990-01-01

    Magic-angle spinning 1H and 13C nuclear magnetic resonance (NMR) have been employed to study 50%-by-weight aqueous dispersions of 1-octadecanoyl-2-decanoyl-sn-glycero-3-phosphocholine (C[18]:C[10]PC) and 1-octadecanoyl-2-d19-decanoyl-PC (C[18]:C[10]PC-d19), mixed-chain phospholipids which can form interdigitated multibilayers. The 1H NMR linewidth for methyl protons of the choline headgroup has been used to monitor the liquid crystalline-to-gel (LC-to-G) phase transition and confirm variations between freezing and melting temperatures. Both 1H and 13C spin-lattice relaxation times indicate unusual restrictions on segmental reorientation at megahertz frequencies for C(18):C(10)PC as compared with symmetric-chain species in the LC state; nevertheless each chemical moiety of the mixed-chain phospholipid exhibits motional behavior that may be classified as liquidlike. Two-dimensional nuclear Overhauser spectroscopy (NOESY) on C(18):C(10)PC and C(18):C(10)PC-d19 reveals cross-peaks between the omega-methyl protons of the C18 chain and the N-methyl protons of the phosphocholine headgroup, and several experimental and theoretical considerations argue against an interpretation based on spin diffusion. Using NMR relaxation times and NOESY connectivities along with a computational formalism for four-spin systems (Keepers, J. W., and T. L. James. 1984. J. Magn. Reson. 57:404-426), an estimate of 3.5 A is obtained for the average distance between the omega-methyl protons of the C18 chain and the N-methyl protons of the phosphocholine headgroup. This finding is consistent with a degree of interdigitation similar to that proposed for organized assemblies of gel-state phosphatidylcholine molecules with widely disparate acyl-chain lengths (Hui, S. W., and C.-H. Huang. 1986. Biochemistry. 25:1330-1335); however, acyl-chain bendback or other intermolecular interactions may also contribute to the NOESY results. For multibilayers of C(18):C(10)PC in the gel phase, 13C chemical

  1. High-resolution mono- and multidimensional magic angle spinning 1H nuclear magnetic resonance of membrane peptides in nondeuterated lipid membranes and H2O.

    PubMed Central

    Le Guernevé, C; Seigneuret, M

    1996-01-01

    High-speed (14 kHz) solid-state magic angle spinning (MAS) 1H NMR has been applied to several membrane peptides incorporated into nondeuterated dilauroyl or dimyristoylphosphatidylcholine membranes suspended in H2O. It is shown that solvent suppression methods derived from solution NMR, such as presaturation or jump-return, can be used to reduce water resonance, even at relatively high water content. In addition, regioselective excitation of 1H peptide resonances promotes an efficient suppression of lipid resonances, even in cases where these are initially two orders of magnitude more intense. As a consequence, 1H MAS spectra of the peptide low-field region are obtained without interference from water and lipid signals. These display resonances from amide and other exchangeable 1H as well as from aromatic nonexchangeable 1H. The spectral resolution depends on the specific types of resonance and membrane peptide. For small amphiphilic or hydrophobic oligopeptides, resolution of most individual amide resonance is achieved, whereas for the transmembrane peptide gramicidin A, an unresolved amide spectrum is obtained. Partial resolution of aromatic 1H occurs in all cases. Multidimensional 1H-MAS spectra of membrane peptides can also be obtained by using water suppression and regioselective excitation. For gramicidin A, F2-regioselective 2D nuclear Overhauser effect spectroscopy (NOESY) spectra are dominated by intermolecular through-space connectivities between peptide aromatic or formyl 1H and lipid 1H. These appear to be compatible with the known structure and topography of the gramicidin pore. On the other hand, for the amphiphilic peptide leucine-enkephalin, F2-regioselective NOESY spectra mostly display cross-peaks originating from though-space proximities of amide or aromatic 1H with themselves and with aliphatic 1H. F3-regioselective 3D NOESY-NOESY spectra can be used to obtain through-space correlations within aliphatic 1H. Such intrapeptide proximities should

  2. Unsaturation level decreased in bone marrow fat of postmenopausal women with low bone density using high resolution magic angle spinning (HRMAS) (1)H NMR spectroscopy.

    PubMed

    Li, Xiaojuan; Shet, Keerthi; Xu, Kaipin; Rodríguez, Juan Pablo; Pino, Ana María; Kurhanewicz, John; Schwartz, Ann; Rosen, Clifford J

    2017-08-18

    There are increasing evidences suggesting bone marrow adiposity tissue (MAT) plays a critical role in affecting both bone quantity and quality. However, very limited studies that have investigated the association between the composition of MAT and bone mineral density (BMD). The goal of this study was to quantify MAT unsaturation profile of marrow samples from post-menopausal women using ex vivo high-resolution magic angle spinning (HRMAS) proton nuclear magnetic resonance ((1)H NMR) spectroscopy, and to investigate the relationship between MAT composition and BMD. Bone marrow samples were obtained by iliac crest aspiration during surgical procedures from 24 postmenopausal women (65-89years) who had hip surgery due to bone fracture or arthroplasty. Marrow fat composition parameters, in particular, unsaturation level (UL), mono-unsaturation level (MUL) and saturation level (SL), were quantified using HRMAS (1)H NMR spectroscopy. The patients were classified into three groups based on the DXA BMD T-scores: controls, osteopenia and osteoporosis. Marrow fat composition was compared between these three groups as well as between subjects with and without factures using ANOCOVA, adjusted for age. Subjects with lower BMD (n=17) had significantly lower MUL (P=0.003) and UL (P=0.039), and significantly higher SL (P=0.039) compared to controls (n=7). When separating lower BMD into osteopenia (n=9) and osteoporosis (n=8) groups, subjects with osteopenia had significantly lower MUL (P=0.002) and UL (P=0.010), and significantly higher SL (P=0.010) compared to healthy controls. No significant difference was observed between subjects with osteopenia and osteoporosis. Using HRMAS (1)H NMR, significantly lower unsaturation and significantly higher saturation levels were observed in the marrow fat of subjects with lower BMD. HRMAS (1)H NMR was shown to be a powerful tool for identifying novel MR markers of marrow fat composition that are associated with bone quality and potentially

  3. Site-resolved multiple-quantum filtered correlations and distance measurements by magic-angle spinning NMR: Theory and applications to spins with weak to vanishing quadrupolar couplings

    SciTech Connect

    Eliav, U. E-mail: eliav@tau.ac.il; Haimovich, A.; Goldbourt, A. E-mail: eliav@tau.ac.il

    2016-01-14

    We discuss and analyze four magic-angle spinning solid-state NMR methods that can be used to measure internuclear distances and to obtain correlation spectra between a spin I = 1/2 and a half-integer spin S > 1/2 having a small quadrupolar coupling constant. Three of the methods are based on the heteronuclear multiple-quantum and single-quantum correlation experiments, that is, high rank tensors that involve the half spin and the quadrupolar spin are generated. Here, both zero and single-quantum coherence of the half spins are allowed and various coherence orders of the quadrupolar spin are generated, and filtered, via active recoupling of the dipolar interaction. As a result of generating coherence orders larger than one, the spectral resolution for the quadrupolar nucleus increases linearly with the coherence order. Since the formation of high rank tensors is independent of the existence of a finite quadrupolar interaction, these experiments are also suitable to materials in which there is high symmetry around the quadrupolar spin. A fourth experiment is based on the initial quadrupolar-driven excitation of symmetric high order coherences (up to p = 2S, where S is the spin number) and subsequently generating by the heteronuclear dipolar interaction higher rank (l + 1 or higher) tensors that involve also the half spins. Due to the nature of this technique, it also provides information on the relative orientations of the quadrupolar and dipolar interaction tensors. For the ideal case in which the pulses are sufficiently strong with respect to other interactions, we derive analytical expressions for all experiments as well as for the transferred echo double resonance experiment involving a quadrupolar spin. We show by comparison of the fitting of simulations and the analytical expressions to experimental data that the analytical expressions are sufficiently accurate to provide experimental {sup 7}Li–{sup 13}C distances in a complex of lithium, glycine, and water

  4. Dynamic High-Resolution H-1 and P-31 NMR Spectroscopy and H-1 T-2 Measurements in Postmortem Rabbit Muscles Using Slow Magic Angle Spinning

    SciTech Connect

    Bertram, Hanne Christine; Hu, Jian Zhi; Rommereim, Donald N.; Wind, Robert A.; Andersen, Henrik J.

    2004-05-05

    Postmortem changes in rabbit muscle tissue with different glycogen status (normal vs low) were followed continuously from 13 min postmortem until 8 h postmortem and again 20 h postmortem using simultaneous magic angle spinning 1H and 31P NMR spectroscopy together with measurement of the transverse relaxation time, T2, of the muscle water. The 1H metabolite spectra were measured using the phase-altered spinning sidebands (PASS) technique at a spinning rate of 40 Hz. pH values calculated from the 31P NMR spectra using the chemical shifts of the C-6 line of histidine in the 1H spectra and the chemical shifts of inorganic phosphate in the 31P spectra confirmed the different muscle glycogen status in the tissues. High-resolution 1H spectra obtained from the PASS technique revealed the presence of a new resonance line at 6.8 ppm during the postmortem period, which were absent in muscles with low muscle glycogen content. This new resonance line may originate from the aminoprotons in creatine, and its appearance may be a result of a pH effect on the exchange rate between the amino and the water protons and thereby the NMR visibility. Alternatively, the new resonance line may originate from the aromatic protons in tyrosine, and its appearance may be a result of a pH-induced protein unfolding exposing hydrophobic amino acid residues to the aqueous environment. Further studies are needed to evaluate these hypotheses. Finally, distributed analysis of the water T2 relaxation data revealed three relaxation populations and an increase in the population believed to reflect extramyofibrillar water through the postmortem period. This increase was significantly reduced (p < 0.0001) in samples from animals with low muscle glycogen content, indicating that the pH is controlling the extent of postmortem expulsion of water from myofibrillar structures. The significance of the postmortem increase in the amount extramyofibrillar water on the water-holding capacity was verified by

  5. 13C high-resolution-magic angle spinning MRS reveals differences in glucose metabolism between two breast cancer xenograft models with different gene expression patterns.

    PubMed

    Grinde, Maria T; Moestue, Siver A; Borgan, Eldrid; Risa, Øystein; Engebraaten, Olav; Gribbestad, Ingrid S

    2011-12-01

    Tumor cells have increased glycolytic activity, and glucose is mainly used to form lactate and alanine, even when high concentrations of oxygen are present (Warburg effect). The purpose of the present study was to investigate glucose metabolism in two xenograft models representing basal-like and luminal-like breast cancer using (13) C high-resolution-magic angle spinning (HR-MAS) MRS and gene expression analysis. Tumor tissue was collected from two groups for each model: untreated mice (n=19) and a group of mice (n=16) that received an injection of [1-(13) C]-glucose 10 or 15 min before harvesting the tissue. (13) C HR-MAS MRS was performed on the tumor samples and differences in the glucose/alanine (Glc/Ala), glucose/lactate (Glc/Lac) and alanine/lactate (Ala/Lac) ratios between the models were studied. The expression of glycolytic genes was studied using tumor tissue from the same models. In the natural abundance MR spectra, a significantly lower Glc/Ala and Glc/Lac ratio (p<0.001) was observed in the luminal-like model compared with the basal-like model. In the labeled samples, the predominant glucose metabolites were lactate and alanine. Significantly lower Glc/Ala and Glc/Lac ratios were observed in the luminal-like model (p<0.05). Most genes contributing to glycolysis were expressed at higher levels in the luminal-like model (fdr<0.001). The lower Glc/Ala and Glc/Lac ratios and higher glycolytic gene expression observed in the luminal-like model indicates that the transformation of glucose to lactate and alanine occurred faster in this model than in the basal-like model, which has a growth rate several times faster than that of the luminal-like model. The results from the present study suggest that the tumor growth rate is not necessarily a determinant of glycolytic activity. Copyright © 2011 John Wiley & Sons, Ltd.

  6. A spatially offset Raman spectroscopy method for non-destructive detection of gelatin-encapsulated powders

    USDA-ARS?s Scientific Manuscript database

    Non-destructive subsurface detection of encapsulated, coated, or seal-packaged foods and pharmaceuticals can help prevent distribution and consumption of counterfeit or hazardous products. This study used a Spatially Offset Raman Spectroscopy (SORS) method to detect and identify urea, ibuprofen, and...

  7. Non-destructive method for inward leakage detection of a plate evaporator

    NASA Astrophysics Data System (ADS)

    Hribernik, Ales

    2007-05-01

    A new non-destructive method was developed for the detection of refrigerant leakage at an evaporator's inflow. Nitrogen and oxygen gas were successively blown through the evaporator. A gas analyser was applied at the outflow of the evaporator and the oxygen concentration measured. It was possible to detect any leakage by investigating the oxygen concentration-time history diagram.

  8. Using magnetic levitation for non-destructive quality control of plastic parts.

    PubMed

    Hennek, Jonathan W; Nemiroski, Alex; Subramaniam, Anand Bala; Bwambok, David K; Yang, Dian; Harburg, Daniel V; Tricard, Simon; Ellerbee, Audrey K; Whitesides, George M

    2015-03-04

    Magnetic levitation (MagLev) enables rapid and non-destructive quality control of plastic parts. The feasibility of MagLev as a method to: i) rapidly assess injection-molded plastic parts for defects during process optimization, ii) monitor the degradation of plastics after exposure to harsh environmental conditions, and iii) detect counterfeit polymers by density is demonstrated.

  9. Non-destructive digital imaging in poplar allows detailed analysis of adventitious rooting dynamics

    Treesearch

    R.J. Kodrzycki; R.B. Michaels; A.L. Friend; R.S. Zalesny; Ch.P. Mawata; D.W. McDonald

    2008-01-01

    The dynamics of root formation are difficult to observe directly over time without disturbing the rooting environment. A novel system for a non-destructive, non-invasive root analysis (RootViz FS, Phenotype Screening Corp.) was evaluated for its ability to analyze root formation from cuttings over a 32 day period in three poplar genotypes (DN70, P. Deltoides x...

  10. Research on non-destructive testing method of silkworm cocoons based on image processing technology

    NASA Astrophysics Data System (ADS)

    Gan, Yong; Kong, Qing-hua; Wei, Li-fu

    2008-03-01

    The major studied in this dissertation is the non-destructive testing method of silkworm cocoon's quality, based on the digital image processing and photoelectricity technology. Through the images collection and the data analysis, procession and calculation of the tested silkworm cocoons with the non-destructive testing technology, internet applications automatically reckon all items of the classification indexes. Finally we can conclude the classification result and the purchase price of the silkworm cocoons. According to the domestic classification standard of the silkworm cocoons, the author investigates various testing methods of silkworm cocoons which are used or have been explored at present, and devices a non-destructive testing scheme of the silkworm cocoons based on the digital image processing and photoelectricity technology. They are dissertated about the project design of the experiment. The precisions of all the implements are demonstrated. I establish Manifold mathematic models, compare them with each other and analyze the precision with technology of databank to get the best mathematic model to figure out the weight of the dried silkworm cocoon shells. The classification methods of all the complementary items are designed well and truly. The testing method has less error and reaches an advanced level of the present domestic non-destructive testing technology of the silkworm cocoons.

  11. Measuring low-level porosity structures by using a non-destructive terahertz inspection system

    NASA Astrophysics Data System (ADS)

    Liu, Hongwei; Ke, Lin

    2017-09-01

    It is demanded a non-contact, non-destructive and reliable system and method of porosity measurement because conventional techniques are contact and cubersome. We have developed a method by using THz inspection system, which allows measuring the porosity rapidly and non-invasively, by introducing an external perturbation. The embodiments of the external perturbation can be mechanical or pulsed laser.

  12. Non-destructive assessment of human ribs mechanical properties using quantitative ultrasound.

    PubMed

    Mitton, David; Minonzio, Jean-Gabriel; Talmant, Maryline; Ellouz, Rafaa; Rongieras, Frédéric; Laugier, Pascal; Bruyère-Garnier, Karine

    2014-04-11

    Advanced finite element models of the thorax have been developed to study, for example, the effects of car crashes. While there is a need for material properties to parameterize such models, specific properties are largely missing. Non-destructive techniques applicable in vivo would, therefore, be of interest to support further development of thorax models. The only non-destructive technique available today to derive rib bone properties would be based on quantitative computed tomography that measures bone mineral density. However, this approach is limited by the radiation dose. Bidirectional ultrasound axial transmission was developed on long bones ex vivo and used to assess in vivo health status of the radius. However, it is currently unknown if the ribs are good candidates for such a measurement. Therefore, the goal of this study is to evaluate the relationship between ex vivo ultrasonic measurements (axial transmission) and the mechanical properties of human ribs to determine if the mechanical properties of the ribs can be quantified non-destructively. The results show statistically significant relationships between the ultrasonic measurements and mechanical properties of the ribs. These results are promising with respect to a non-destructive and non-ionizing assessment of rib mechanical properties. This ex vivo study is a first step toward in vivo studies to derive subject-specific rib properties.

  13. Magical Boxes

    ERIC Educational Resources Information Center

    Costello, Judith

    2005-01-01

    Students get excited when they realize that they can transform a flat sheet of paper into a box. By using different sizes of paper, they can make different sizes of boxes and put a box inside a box, inside a box. These magical boxes within boxes can contain unwanted emotions or special treasures. The project described in this article incorporates…

  14. Matisse Magic.

    ERIC Educational Resources Information Center

    Gibson, Marcia

    2002-01-01

    Presents an art lesson in which kindergarten and first-grade students learn about Henri Matisse and his art work. Explains that the students use "Model Magic" to create Matisse style face refrigerator magnets. Discusses in detail how to create the magnets. (CMK)

  15. MAGIC clarifications

    NASA Astrophysics Data System (ADS)

    Ellis, John; Mavromatos, Nikolaos

    2008-02-01

    We are disappointed that your news story on the recent gamma-ray observations we made with the MAGIC telescope November 2007 p12) does not do justice to the caveats included in our paper. It chooses instead (like many blogs) to focus on theoretical speculations that were not made in the paper.

  16. Magical Boxes

    ERIC Educational Resources Information Center

    Costello, Judith

    2005-01-01

    Students get excited when they realize that they can transform a flat sheet of paper into a box. By using different sizes of paper, they can make different sizes of boxes and put a box inside a box, inside a box. These magical boxes within boxes can contain unwanted emotions or special treasures. The project described in this article incorporates…

  17. Mummies & Magic.

    ERIC Educational Resources Information Center

    Casey, Jeanne E.

    1989-01-01

    Covers the cultural and aesthetic significance of Egyptian mummies, as explained in an exhibition at Boston's Museum of Fine Arts. The display, "Mummies & Magic: The Funerary Arts of Ancient Egypt," allowed for restoration work which did much to advance modern knowledge of Egyptian culture and funerary art. (LS)

  18. Magic Mirrors

    ERIC Educational Resources Information Center

    Mills, Allan

    2011-01-01

    "Magic mirrors" were so named because, when they were positioned to throw a reflected patch of sunlight on a nearby wall, this area contained an outline of a design cast on the back of the (bronze) mirror. Investigations begun in the 19th century showed that this was a response to heavy localized pressures exerted on the face of the thin mirror…

  19. Mummies & Magic.

    ERIC Educational Resources Information Center

    Casey, Jeanne E.

    1989-01-01

    Covers the cultural and aesthetic significance of Egyptian mummies, as explained in an exhibition at Boston's Museum of Fine Arts. The display, "Mummies & Magic: The Funerary Arts of Ancient Egypt," allowed for restoration work which did much to advance modern knowledge of Egyptian culture and funerary art. (LS)

  20. Magic Mirrors

    ERIC Educational Resources Information Center

    Mills, Allan

    2011-01-01

    "Magic mirrors" were so named because, when they were positioned to throw a reflected patch of sunlight on a nearby wall, this area contained an outline of a design cast on the back of the (bronze) mirror. Investigations begun in the 19th century showed that this was a response to heavy localized pressures exerted on the face of the thin mirror…

  1. Progress in 13C and 1H solid-state nuclear magnetic resonance for paramagnetic systems under very fast magic angle spinning

    NASA Astrophysics Data System (ADS)

    Wickramasinghe, Nalinda P.; Shaibat, Medhat A.; Jones, Christopher R.; Casabianca, Leah B.; de Dios, Angel C.; Harwood, John S.; Ishii, Yoshitaka

    2008-02-01

    High-resolution solid-state NMR (SSNMR) of paramagnetic systems has been largely unexplored because of various technical difficulties due to large hyperfine shifts, which have limited the success of previous studies through depressed sensitivity/resolution and lack of suitable assignment methods. Our group recently introduced an approach using "very fast" magic angle spinning (VFMAS) for SSNMR of paramagnetic systems, which opened an avenue toward routine analyses of small paramagnetic systems by C13 and H1 SSNMR [Y. Ishii et al., J. Am. Chem. Soc. 125, 3438 (2003); N. P. Wickramasinghe et al., ibid. 127, 5796 (2005)]. In this review, we discuss our recent progress in establishing this approach, which offers solutions to a series of problems associated with large hyperfine shifts. First, we demonstrate that MAS at a spinning speed of 20kHz or higher greatly improves sensitivity and resolution in both H1 and C13 SSNMR for paramagnetic systems such as Cu(II)(L-alanine)2ṡH2O (Cu( L-Ala )2) and Mn(acac)3, for which the spectral dispersions due to H1 hyperfine shifts reach 200 and 700ppm, respectively. Then, we introduce polarization transfer methods from H1 spins to C13 spins with high-power cross polarization and dipolar insensitive nuclei enhanced by polarization transfer (INEPT) in order to attain further sensitivity enhancement and to correlate H1 and C13 spins in two-dimensional (2D) SSNMR for the paramagnetic systems. Comparison of C13 VFMAS SSNMR spectra with C13 solution NMR spectra revealed superior sensitivity in SSNMR for Cu( L-Ala )2, Cu(Gly)2, and V(acac)3. We discuss signal assignment methods using one-dimensional (1D) C13 SSNMR C13-H1 rotational echo double resonance (REDOR) and dipolar INEPT methods and 2D C13/H1 correlation SSNMR under VFMAS, which yield reliable assignments of H1 and C13 resonances for Cu(Ala-Thr). Based on the excellent sensitivity/resolution and signal assignments attained in the VFMAS approach, we discuss methods of elucidating

  2. Post-Irradiation Non-Destructive Analyses of the AFIP-7 Experiment

    NASA Astrophysics Data System (ADS)

    Williams, W. J.; Robinson, A. B.; Rabin, B. H.

    2017-08-01

    This article reports the results and interpretation of post-irradiation non-destructive examinations performed on four curved full-size fuel plates that comprise the AFIP-7 experiment. These fuel plates, having a U-10 wt.%Mo monolithic design, were irradiated under moderate operating conditions in the Advanced Test Reactor to assess fuel performance for geometries that are prototypic of research reactor fuel assemblies. Non-destructive examinations include visual examination, neutron radiography, profilometry, and precision gamma scanning. This article evaluates the qualitative and quantitative data taken for each plate, compares corresponding data sets, and presents the results of swelling analyses. These characterization results demonstrate that the fuel meets established irradiation performance requirements for mechanical integrity, geometric stability, and stable and predictable behavior.

  3. Photoacoustic Spectroscopy as a Non-destructive Tool for Quantification of Pesticide Residue in Apple Cuticle

    NASA Astrophysics Data System (ADS)

    Liu, Lixian; Wang, Yafei; Gao, Chunming; Huan, Huiting; Zhao, Binxing; Yan, Laijun

    2015-06-01

    Photoacoustic spectroscopy (PAS), the non-destructive method to detect residue of dimethyl-dichloro-vinyl-phosphate (DDVP) pesticide in a cuticle of apple, is described. After constructing the PA experimental setup and identifying three characteristic peaks of DDVP in the near ultraviolet region, the PA spectra of an apple cuticle contaminated with DDVP were collected. The artificial neural network method was then applied to analyze data quantitatively. The results show a correlation coefficient exceeding 0.99 and a detection limit of 0.2 ppm, which is within the national food safety standard for maximum residue limits for pesticides in food (GB 2763-2012). This fact and the non-destructive character of PAS make the approach promising for detection of pesticide residue in fruits.

  4. Non-destructive quality control of kiwi fruits by hyperspectral imaging

    NASA Astrophysics Data System (ADS)

    Serranti, S.; Bonifazi, G.; Luciani, V.

    2017-05-01

    This study aimed to evaluate the possibility to perform a fast, reliable and robust non-destructive monitoring of kiwifruits characteristics adopting an HyperSpectral Imaging (HSI) based approach. HSI was thus utilized for two different purposes: i) to test whether the postharvest ripeness of kiwifruits could be non-destructively determined and ii) for the diagnosis of pseudomonas infection in the Kiwi orchards. To reach the 1st goal (i.e. fruit ripening evaluation) a NIR Spectral Camera acting in the range between 900 and 1700 nm has been used. To reach the 2nd goal a hyperspectral camera working in the VIS-NIR range (400 nm - 1000 nm) was used. For both the approaches "only" significance and robustness of the collected data, in respect of the selected operative conditions, was investigated and the results have been evaluated in terms of different Principal Components (PC) images.

  5. Microwaving Blood as a Non-Destructive Technique for Haemoglobin Measurements on Microlitre Samples

    PubMed Central

    Basey-Fisher, Toby H.; Guerra, Nadia; Triulzi, Chiara; Gregory, Andrew; Hanham, Stephen M.; Stevens, Molly M.; Maier, Stefan A.; Klein, Norbert

    2016-01-01

    The non-destructive ex vivo determination of haemoglobin (Hgb) concentration offers the capability to conduct multiple red blood cell haematological measurements on a single sample, an advantage that current optical techniques are unable to offer. Here, a microwave method and device for the accurate and non-destructive determination of Hgb concentration in microlitre blood samples are described. Using broadband microwave spectroscopy, a relationship is established between the dielectric properties of murine blood and Hgb concentration that is utilized to create a technique for the determination of Hgb concentration. Subsequently, a microwave dielectric resonator-microfluidic system is implemented in the analysis of 52 murine samples with microlitre volumes and Hgb concentrations ranging from 0 to 17 g dL−1. Using the characterized relationship, independent and minimally invasive Hgb measurements are made on nine healthy mice as well as seven with mutations in the Adenomatous polyposis coli (APC) gene that leads to colorectal cancer and consequently anaemia. PMID:24002989

  6. Non-destructive measurement and monitoring of separation of charged particle micro-bunches

    NASA Astrophysics Data System (ADS)

    Zhang, H.; Konoplev, I. V.; Lancaster, A. J.; Harrison, H.; Doucas, G.; Aryshev, A.; Shevelev, M.; Terunuma, N.; Urakawa, J.

    2017-07-01

    Micro-bunched particle beams are used for a wide range of research including wakefield-based particle acceleration and tunable sources of radiation. In all applications, accurate and non-destructive monitoring of the bunch-to-bunch separation is required. With the development of femtosecond lasers, the generation of micro-bunched beams directly from a photocathode becomes routine; however, non-destructive monitoring of the separation is still a challenge. We present the results of proof-of-principle experiments conducted at the Laser Undulator Compact X-ray accelerator measuring the distance between micro-bunches via the amplitude modulation analysis of a monochromatic radiation signal. Good agreement with theoretical predictions is shown; limitations and further improvements are discussed.

  7. Can predatory bird feathers be used as a non-destructive biomonitoring tool of organic pollutants?

    PubMed Central

    Jaspers, Veerle L.B; Voorspoels, Stefan; Covaci, Adrian; Eens, Marcel

    2006-01-01

    The monitoring of different types of pollutants that are released into the environment and that present risks for both humans and wildlife has become increasingly important. In this study, we examined whether feathers of predatory birds can be used as a non-destructive biomonitor of organic pollutants. We demonstrate that polychlorinated biphenyls (PCBs), dichlorodiphenyltrichloroethane (DDT) and polybrominated diphenyl ethers (PBDEs) are measurable in one single tail feather of common buzzards (Buteo buteo) and that levels in this feather and internal tissues are significantly related to each other (0.35non-destructive biomonitoring of organic pollutants, although further validation may be necessary. PMID:17148383

  8. Probability of detection model for the non-destructive inspection of steam generator tubes of PWRs

    NASA Astrophysics Data System (ADS)

    Yusa, N.

    2017-06-01

    This study proposes a probability of detection (POD) model to discuss the capability of non-destructive testing methods for the detection of stress corrosion cracks appearing in the steam generator tubes of pressurized water reactors. Three-dimensional finite element simulations were conducted to evaluate eddy current signals due to stress corrosion cracks. The simulations consider an absolute type pancake probe and model a stress corrosion crack as a region with a certain electrical conductivity inside to account for eddy currents flowing across a flaw. The probabilistic nature of a non-destructive test is simulated by varying the electrical conductivity of the modelled stress corrosion cracking. A two-dimensional POD model, which provides the POD as a function of the depth and length of a flaw, is presented together with a conventional POD model characterizing a flaw using a single parameter. The effect of the number of the samples on the PODs is also discussed.

  9. Non-destructive optical methods for the study of soft tissues

    NASA Astrophysics Data System (ADS)

    Santiago-Lona, Cynthia V.; Hernández-Montes, María. del Socorro; Mendoza Santoyo, F.; Muñoz, Silvino; Mendoza, Fernando

    2015-08-01

    In optical metrology, non-destructive methods allow studying some mechanical properties of the samples to investigate by using light, which leads to non-contact testing. This paper shows recent results of the application of non-destructive optical methods based on Digital Holographic Interferometry to the study biological tissues; particularly vocal folds and the tympanic membrane. The displacements data and its corresponding patterns found generates information on its characteristics that can be correlated with their physiological state. These methods prove to be an alternative viable and appropriate to characterize these soft tissues so important for the proper function of the human body. The result shows a potential impact on its possible uses in the field of otorhinolaryngology.

  10. Non-destructive imaging of buried electronic interfaces using a decelerated scanning electron beam

    PubMed Central

    Hirohata, Atsufumi; Yamamoto, Yasuaki; Murphy, Benedict A.; Vick, Andrew J.

    2016-01-01

    Recent progress in nanotechnology enables the production of atomically abrupt interfaces in multilayered junctions, allowing for an increase in the number of transistors in a processor. However, uniform electron transport has not yet been achieved across the entire interfacial area in junctions due to the existence of local defects, causing local heating and reduction in transport efficiency. To date, junction uniformity has been predominantly assessed by cross-sectional transmission electron microscopy, which requires slicing and milling processes that can potentially introduce additional damage and deformation. It is therefore essential to develop an alternative non-destructive method. Here we show a non-destructive technique using scanning electron microscopy to map buried junction properties. By controlling the electron-beam energy, we demonstrate the contrast imaging of local junction resistances at a controlled depth. This technique can be applied to any buried junctions, from conventional semiconductor and metal devices to organic devices. PMID:27586090

  11. Non-destructive imaging of buried electronic interfaces using a decelerated scanning electron beam

    NASA Astrophysics Data System (ADS)

    Hirohata, Atsufumi; Yamamoto, Yasuaki; Murphy, Benedict A.; Vick, Andrew J.

    2016-09-01

    Recent progress in nanotechnology enables the production of atomically abrupt interfaces in multilayered junctions, allowing for an increase in the number of transistors in a processor. However, uniform electron transport has not yet been achieved across the entire interfacial area in junctions due to the existence of local defects, causing local heating and reduction in transport efficiency. To date, junction uniformity has been predominantly assessed by cross-sectional transmission electron microscopy, which requires slicing and milling processes that can potentially introduce additional damage and deformation. It is therefore essential to develop an alternative non-destructive method. Here we show a non-destructive technique using scanning electron microscopy to map buried junction properties. By controlling the electron-beam energy, we demonstrate the contrast imaging of local junction resistances at a controlled depth. This technique can be applied to any buried junctions, from conventional semiconductor and metal devices to organic devices.

  12. Non-destructive imaging of buried electronic interfaces using a decelerated scanning electron beam.

    PubMed

    Hirohata, Atsufumi; Yamamoto, Yasuaki; Murphy, Benedict A; Vick, Andrew J

    2016-09-02

    Recent progress in nanotechnology enables the production of atomically abrupt interfaces in multilayered junctions, allowing for an increase in the number of transistors in a processor. However, uniform electron transport has not yet been achieved across the entire interfacial area in junctions due to the existence of local defects, causing local heating and reduction in transport efficiency. To date, junction uniformity has been predominantly assessed by cross-sectional transmission electron microscopy, which requires slicing and milling processes that can potentially introduce additional damage and deformation. It is therefore essential to develop an alternative non-destructive method. Here we show a non-destructive technique using scanning electron microscopy to map buried junction properties. By controlling the electron-beam energy, we demonstrate the contrast imaging of local junction resistances at a controlled depth. This technique can be applied to any buried junctions, from conventional semiconductor and metal devices to organic devices.

  13. PANDA—A novel instrument for non-destructive sample analysis

    NASA Astrophysics Data System (ADS)

    Turunen, Jani; Peräjärvi, Kari; Pöllänen, Roy; Toivonen, Harri

    2010-01-01

    An instrument known as PANDA (Particles And Non-Destructive Analysis) for non-destructive sample analysis has been designed and built at the Finnish Radiation and Nuclear Safety Authority (STUK). In PANDA the measurement techniques and instruments designed for the basic research are applied to the analysis of environmental samples. PANDA has two vacuum chambers, one for loading samples and the other for measurements. In the measurement chamber there are two individual measurement positions. Currently the first one hosts an HPGe gamma detector and a position-sensitive alpha detector. The second measurement position is intended for precise characterization of found particles. PANDA's data are recorded in event mode and events are timestamped. In the present article the technical design of PANDA is presented in detail. In addition, its performance using depleted uranium particles and an air filter is demonstrated.

  14. The application of non-destructive techniques to the testing of a wind turbine blade

    SciTech Connect

    Sutherland, H.; Beattie, A.; Hansche, B.; Musial, W.; Allread, J.; Johnson, J.; Summers, M.

    1994-06-01

    NonDestructive Testing (NDT), also called NonDestructive Evaluation (NDE), is commonly used to monitor structures before, during, and after testing. This paper reports on the use of two NDT techniques to monitor the behavior of a typical wind turbine blade during a quasi-static test-to-failure. The two NDT techniques used were acoustic emission and coherent optical. The former monitors the acoustic energy produced by the blade as it is loaded. The latter uses electron shearography to measure the differences in surface displacements between two load states. Typical results are presented to demonstrate the ability of these two techniques to locate and monitor both high damage regions and flaws in the blade structure. Furthermore, this experiment highlights the limitations in the techniques that must be addressed before one or both can be transferred, with a high probability of success, to the inspection and monitoring of turbine blades during the manufacturing process and under normal operating conditions.

  15. Destructive and Non-Destructive Analysis Techniques for Failure Detection of QFN Packages

    NASA Astrophysics Data System (ADS)

    Adhila, M. N.; Wedianti, S.; Suhaimi, W. S. W. M.; Aishah, I.

    2010-03-01

    One of the latest developments in packaging technology is the QFN (Quad Flat Non-Lead) packages, which is both a chip scale package and plastic encapsulated package with lead pad at the bottom. In this paper, different type of commercial QFN single die packages were characterized by using destructive and non-destructive techniques. Non-destructive techniques such as Scanning Acoustic Microscope (SAM) and X-Ray analysis were used to observe package cracking, delamination and other failure mode. Application of SAM include detection of delaminations between lead frame, die face, paddle, heat sink, cracks and plastic encapsulant. In comparison to other techniques, SAM is sensitive to detect beneath the surface of devices which would be inaccessible otherwise by both conventional optical and electron microscopy inspection methods. Destructive technique such as Field Emission Electron Microscopy (FESEM) was implemented to address the failures of the QFN single die packages such as die cracking, lifted ball bonds and other failure mode.

  16. A novel quadruple excitation in high-Tc SQUID-based non-destructive evaluation

    NASA Astrophysics Data System (ADS)

    Kong, X. Y.; Ren, Y. F.; Li, J. W.; Yu, H. W.; Chen, G. H.; Yang, Q. S.

    2006-02-01

    A high-Tc SQUID-based non-destructive evaluation (NDE) system has been set up in our laboratory. The SQUID was made on a 24° bicystal SrTiO3 substrate. A novel quadruple excitation coil was proposed for the first time and applied in the artificial holes in the aluminium multilayer structure in a noisy unshielded environment. The experimental data shows that it has good balance and is very effective at detecting small hole defects.

  17. Non-Destructive Methods of Characterising the Strength of Adhesive-Bonded Joints.

    DTIC Science & Technology

    1985-10-01

    R D-RI68 191 NON-DESTRUCTIVE METHODS OF CHRACTERISING THE STRENGTH ±i𔃻 I OF ADHESIVE-BONDED..(U) ROYAL AIRCRAFT ESTABLISHMENT I FRNBOROUGH ( ENGLAND ... UK to monitor degrada- tion by means of ultrasound have used a conventional pulse-echo approach in which the .’#" direction of the ultrasonic wave is...UNCLASSIFIED 5. DRIC Code for Originator 6. Originator (Corporate Author) Name and Location 7673000W Royal Aircraft Establishment, Farnborough, Hants, UK 5a

  18. Conceptual design of non-destructive, time profile monitor for femtosecond-long electron bunches

    NASA Astrophysics Data System (ADS)

    Konoplev, I. V.; Harrison, H.; Lancaster, A. J.; Taheri, F. Bakkali; Doucas, G.; Aryshev, A.; Lekomtsev, K.; Shevelev, M.; Terunuma, N.; Urakawa, J.

    2017-03-01

    The main objective of the project is to build a high resolution time-profile monitor for femtosecond electron beams, based on the spectral analysis of coherent Smith-Purcell radiation (cSPr). The monitor will be capable of determining the electron bunch time profile non-destructively and on a shot-by-shot basis. The results of recent experimental and theoretical studies are presented, and the conceptual design of the monitor is discussed.

  19. Coded excitation for infrared non-destructive testing of carbon fiber reinforced plastics.

    PubMed

    Mulaveesala, Ravibabu; Venkata Ghali, Subbarao

    2011-05-01

    This paper proposes a Barker coded excitation for defect detection using infrared non-destructive testing. Capability of the proposed excitation scheme is highlighted with recently introduced correlation based post processing approach and compared with the existing phase based analysis by taking the signal to noise ratio into consideration. Applicability of the proposed scheme has been experimentally validated on a carbon fiber reinforced plastic specimen containing flat bottom holes located at different depths.

  20. Application of Non-destructive Methods of Stress-strain State at Hazardous Production Facilities

    NASA Astrophysics Data System (ADS)

    Shram, V.; Kravtsova, Ye; Selsky, A.; Bezborodov, Yu; Lysyannikova, N.; Lysyannikov, A.

    2016-06-01

    The paper deals with the sources of accidents in distillation columns, on the basis of which the most dangerous defects are detected. The analysis of the currently existing methods of non-destructive testing of the stress-strain state is performed. It is proposed to apply strain and acoustic emission techniques to continuously monitor dangerous objects, which helps prevent the possibility of accidents, as well as reduce the work.

  1. Development of the Portable Synchrotron MIRRORCLE-CV for High Precision Non-Destructive Testing

    SciTech Connect

    Hasegawa, Daisuke; Toyosugi, Norio; Noh, Young Deok; Yamada, Takanori; Morita, Masaki; Mantey, Edward; Masaoka, Sei; Yamada, Hironari

    2007-01-19

    We started the development of the portable synchrotron MIRRORCLE-CV series, which provides a high quality x-ray beam for high precision non-destructive testing (NDT). Computer simulations for the magnetic field design and electron dynamics reveal that the outer diameter of the synchrotron magnet can be as small as 30 cm. This synchrotron size approaches that of a conventional x-ray tube.

  2. MIRRORCLE-CV The Portable Synchrotron For Precise Non-Destructive Testing And Medical Diagnosis

    SciTech Connect

    Hasegawa, Daisuke; Yamada, Hironari

    2007-03-30

    We are developing the portable synchrotron MIRRORCLE-CV series, which provides a high quality x-ray beam for high precision non-destructive testing (NDT). Computer simulations for the magnetic field design and electron dynamics reveal that the outer diameter of the synchrotron magnet can be as small as 30 cm. This synchrotron size approaches that of a conventional x-ray tube.

  3. Non-destructive Phenotyping to Identify Brachiaria Hybrids Tolerant to Waterlogging Stress under Field Conditions

    PubMed Central

    Jiménez, Juan de la Cruz; Cardoso, Juan A.; Leiva, Luisa F.; Gil, Juanita; Forero, Manuel G.; Worthington, Margaret L.; Miles, John W.; Rao, Idupulapati M.

    2017-01-01

    Brachiaria grasses are sown in tropical regions around the world, especially in the Neotropics, to improve livestock production. Waterlogging is a major constraint to the productivity and persistence of Brachiaria grasses during the rainy season. While some Brachiaria cultivars are moderately tolerant to seasonal waterlogging, none of the commercial cultivars combines superior yield potential and nutritional quality with a high level of waterlogging tolerance. The Brachiaria breeding program at the International Center for Tropical Agriculture, has been using recurrent selection for the past two decades to combine forage yield with resistance to biotic and abiotic stress factors. The main objective of this study was to test the suitability of normalized difference vegetation index (NDVI) and image-based phenotyping as non-destructive approaches to identify Brachiaria hybrids tolerant to waterlogging stress under field conditions. Nineteen promising hybrid selections from the breeding program and three commercial checks were evaluated for their tolerance to waterlogging under field conditions. The waterlogging treatment was imposed by applying and maintaining water to 3 cm above soil surface. Plant performance was determined non-destructively using proximal sensing and image-based phenotyping and also destructively via harvesting for comparison. Image analysis of projected green and dead areas, NDVI and shoot biomass were positively correlated (r ≥ 0.8). Our results indicate that image analysis and NDVI can serve as non-destructive screening approaches for the identification of Brachiaria hybrids tolerant to waterlogging stress. PMID:28243249

  4. Giant Magnetoresistance Sensors: A Review on Structures and Non-Destructive Eddy Current Testing Applications

    PubMed Central

    Rifai, Damhuji; Abdalla, Ahmed N.; Ali, Kharudin; Razali, Ramdan

    2016-01-01

    Non-destructive eddy current testing (ECT) is widely used to examine structural defects in ferromagnetic pipe in the oil and gas industry. Implementation of giant magnetoresistance (GMR) sensors as magnetic field sensors to detect the changes of magnetic field continuity have increased the sensitivity of eddy current techniques in detecting the material defect profile. However, not many researchers have described in detail the structure and issues of GMR sensors and their application in eddy current techniques for nondestructive testing. This paper will describe the implementation of GMR sensors in non-destructive testing eddy current testing. The first part of this paper will describe the structure and principles of GMR sensors. The second part outlines the principles and types of eddy current testing probe that have been studied and developed by previous researchers. The influence of various parameters on the GMR measurement and a factor affecting in eddy current testing will be described in detail in the third part of this paper. Finally, this paper will discuss the limitations of coil probe and compensation techniques that researchers have applied in eddy current testing probes. A comprehensive review of previous studies on the application of GMR sensors in non-destructive eddy current testing also be given at the end of this paper. PMID:26927123

  5. Feasibility Study of Non-Destructive Techniques to Measure Corrosion in SAVY Containers

    SciTech Connect

    Davenport, Matthew Nicholas

    2016-07-15

    Stainless Steel SAVY containers are used to transport and store nuclear material. They are prone to interior corrosion in the presence of certain chemicals and a low-oxygen environment. SAVY containers also have relatively thin walls to reduce their weight, making their structural integrity more vulnerable to the effects of corrosion. A nondestructive evaluation system that finds and monitors corrosion within containers in use would improve safety conditions and preclude hazards. Non-destructive testing can determine whether oxidation or corrosion is occurring inside the SAVY containers, and there are a variety of non-destructive testing methods that may be viable. The feasibility study described will objectively decide which method best fits the requirements of the facility and the problem. To improve efficiency, the containers cannot be opened during the non-destructive examination. The chosen technique should also be user-friendly and relatively quick to apply. It must also meet facility requirements regarding wireless technology and maintenance. A feasibility study is an objective search for a new technology or product to solve a particular problem. First, the design, technical, and facility feasibility requirements are chosen and ranked in order of importance. Then each technology considered is given a score based upon a standard ranking system. The technology with the highest total score is deemed the best fit for a certain application.

  6. Non-destructive single-pass low-noise detection of ions in a beamline

    SciTech Connect

    Schmidt, Stefan; Murböck, Tobias; Birkl, Gerhard; Andelkovic, Zoran; Vogel, Manuel; Nörtershäuser, Wilfried; Stahl, Stefan

    2015-11-15

    We have conceived, built, and operated a device for the non-destructive single-pass detection of charged particles in a beamline. The detector is based on the non-resonant pick-up and subsequent low-noise amplification of the image charges induced in a cylindrical electrode surrounding the particles’ beam path. The first stage of the amplification electronics is designed to be operated from room temperature down to liquid helium temperature. The device represents a non-destructive charge counter as well as a sensitive timing circuit. We present the concept and design details of the device. We have characterized its performance and show measurements with low-energy highly charged ions (such as Ar{sup 13+}) passing through one of the electrodes of a cylindrical Penning trap. This work demonstrates a novel approach of non-destructive, low noise detection of charged particles which is, depending on the bunch structure, suitable, e.g., for ion traps, low-energy beamlines or accelerator transfer sections.

  7. Non-destructive techniques for determining the material characteristics of Cr-Mo-V rotor steel

    SciTech Connect

    Goto, Toru; Kadoya, Yoshikuni; Konishi, Takashi; Kamimura, Takeo; Suyama, Shouji; Haruki, Nirou; Ikuno, Takeshi; Yoshimura, Kouji

    1994-12-31

    Long-term service causes material deterioration, such as the accumulation of creep and fatigue damage, as well as softening and embrittlement, in the high-temperature components of fossil fuel power plants. Therefore, in order to extend plant life at minimum cost without any accidental outages, it is important to observe the material state, especially of rotors and conduct necessary repairs or replace them at the most appropriate time. Therefore, there is a need for non-destructive techniques to evaluate the material characteristics of Cr-Mo-V rotors under service. In this paper, a comparative report of non-destructive techniques using artificially aged and crept Cr-Mo-V steel specimens is given. The techniques tested include replication, hardness measurement, electro-magnetic and ultrasonic techniques, and conventional metallurgical techniques, which have been here to fore usable only in the laboratory, but due to expected advances in the non-destructive sampling of material from service rotors these techniques are now usable in the field. As a result of the studies, the features of each technique are well recognized and the suggestions for the further development of NDE methods for the evaluation of creep damage in Cr-Mo-V rotors are presented.

  8. A new non-destructive readout by using photo-recovered surface potential contrast

    NASA Astrophysics Data System (ADS)

    Wang, Le; Jin, Kui-Juan; Gu, Jun-Xing; Ma, Chao; He, Xu; Zhang, Jiandi; Wang, Can; Feng, Yu; Wan, Qian; Shi, Jin-An; Gu, Lin; He, Meng; Lu, Hui-Bin; Yang, Guo-Zhen

    2014-11-01

    Ferroelectric random access memory is still challenging in the feature of combination of room temperature stability, non-destructive readout and high intensity storage. As a non-contact and non-destructive information readout method, surface potential has never been paid enough attention because of the unavoidable decay of the surface potential contrast between oppositely polarized domains. That is mainly due to the recombination of the surface movable charges around the domain walls. Here, by introducing a laser beam into the combination of piezoresponse force microscopy and Kelvin probe force microscopy, we demonstrate that the surface potential contrast of BiFeO3 films can be recovered under light illumination. The recovering mechanism is understood based on the redistribution of the photo-induced charges driven by the internal electric field. Furthermore, we have created a 12-cell memory pattern based on BiFeO3 films to show the feasibility of such photo-assisted non-volatile and non-destructive readout of the ferroelectric memory.

  9. Giant Magnetoresistance Sensors: A Review on Structures and Non-Destructive Eddy Current Testing Applications.

    PubMed

    Rifai, Damhuji; Abdalla, Ahmed N; Ali, Kharudin; Razali, Ramdan

    2016-02-26

    Non-destructive eddy current testing (ECT) is widely used to examine structural defects in ferromagnetic pipe in the oil and gas industry. Implementation of giant magnetoresistance (GMR) sensors as magnetic field sensors to detect the changes of magnetic field continuity have increased the sensitivity of eddy current techniques in detecting the material defect profile. However, not many researchers have described in detail the structure and issues of GMR sensors and their application in eddy current techniques for nondestructive testing. This paper will describe the implementation of GMR sensors in non-destructive testing eddy current testing. The first part of this paper will describe the structure and principles of GMR sensors. The second part outlines the principles and types of eddy current testing probe that have been studied and developed by previous researchers. The influence of various parameters on the GMR measurement and a factor affecting in eddy current testing will be described in detail in the third part of this paper. Finally, this paper will discuss the limitations of coil probe and compensation techniques that researchers have applied in eddy current testing probes. A comprehensive review of previous studies on the application of GMR sensors in non-destructive eddy current testing also be given at the end of this paper.

  10. Non-destructively reading out information embedded inside real objects by using far-infrared light

    NASA Astrophysics Data System (ADS)

    Okada, Ayumi; Silapasuphakornwong, Piyarat; Suzuki, Masahiro; Torii, Hideyuki; Takashima, Youichi; Uehira, Kazutake

    2015-09-01

    This paper presents a technique that can non-destructively read out information embedded inside real objects by using far-infrared-light. We propose a technique that can protect the copyrights of digital content for homemade products using digital fabrication technologies such as those used in 3D printers. It embeds information on copyrights inside real objects produced by 3D printers by forming fine structures inside the objects as a watermark that cannot be observed from the outside. Fine structures are formed near the surface inside real objects when they are being fabricated. Information embedded inside real objects needs to be read out non-destructively. We used a technique that could non-destructively read out information from inside real objects by using far-infrared light. We conducted experiments where we structured fine cavities inside objects. The disposition of the fine domain contained valuable information. We used the flat and curved surfaces of the objects to identify them. The results obtained from the experiments demonstrated that the disposition patterns of the fine structures appeared on the surface of objects as a temperature profile when far-infrared light was irradiated on their surface. Embedded information could be read out successfully by analyzing the temperature profile images of the surface of the objects that were captured with thermography and these results demonstrated the feasibility of the technique we propose.

  11. Non-destructive analysis of extracellular matrix development in cardiovascular tissue-engineered constructs.

    PubMed

    Tuemen, M; Nguyen, D V A; Raffius, J; Flanagan, T C; Dietrich, M; Frese, J; Schmitz-Rode, T; Jockenhoevel, S

    2013-05-01

    In the field of tissue engineering, there is an increasing demand for non-destructive methods to quantify the synthesis of extracellular matrix (ECM) components such as collagens, elastin or sulphated glycosaminoglycans (sGAGs) in vitro as a quality control before clinical use. In this study, procollagen I carboxyterminal peptide (PICP), procollagen III aminoterminal peptide (PIIINP), tropoelastin and sGAGs are investigated for their potential use as non-destructive markers in culture medium of statically cultivated cell-seeded fibrin gels. Measurement of PICP as marker for type I collagen synthesis, and PIIINP as marker of type III collagen turnover, correlated well with the hydroxyproline content of the fibrin gels, with a Pearson correlation coefficient of 0.98 and 0.97, respectively. The measurement of tropoelastin as marker of elastin synthesis correlated with the amount of elastin retained in fibrin gels with a Pearson correlation coefficient of 0.99. sGAGs were retained in fibrin gels, but were not detectable in culture medium at any time of measurement. In conclusion, this study demonstrates the potential of PICP and tropoelastin as non-destructive culture medium markers for collagen and elastin synthesis. To our knowledge, this is the first study in cardiovascular tissue engineering investigating the whole of here proposed biomarkers of ECM synthesis to monitor the maturation process of developing tissue non-invasively, but for comprehensive assessment of ECM development, these biomarkers need to be investigated in further studies, employing dynamic cultivation conditions and more complex tissue constructs.

  12. Non-destructive single-pass low-noise detection of ions in a beamline.

    PubMed

    Schmidt, Stefan; Murböck, Tobias; Andelkovic, Zoran; Birkl, Gerhard; Nörtershäuser, Wilfried; Stahl, Stefan; Vogel, Manuel

    2015-11-01

    We have conceived, built, and operated a device for the non-destructive single-pass detection of charged particles in a beamline. The detector is based on the non-resonant pick-up and subsequent low-noise amplification of the image charges induced in a cylindrical electrode surrounding the particles' beam path. The first stage of the amplification electronics is designed to be operated from room temperature down to liquid helium temperature. The device represents a non-destructive charge counter as well as a sensitive timing circuit. We present the concept and design details of the device. We have characterized its performance and show measurements with low-energy highly charged ions (such as Ar(13+)) passing through one of the electrodes of a cylindrical Penning trap. This work demonstrates a novel approach of non-destructive, low noise detection of charged particles which is, depending on the bunch structure, suitable, e.g., for ion traps, low-energy beamlines or accelerator transfer sections.

  13. [Study on Non-Destructive Testing of Guqin Interior Structure Based on Computed Tomography].

    PubMed

    Zhao, De-da; Liu, Xing-e; Yang, Shu-min; Yu, Shenz; Tian, Gen-lin; Ma, Jian-feng; Wang, Qing-ping

    2015-12-01

    The wood property and production process affect quality of Guqin. At the same time, Guqin shape with cavity layout relations to the improvement of Guqin technology and inheritance, so it's very important to get the internal cavity characteristics and parameters on the condition of non-destructive the structure of Guqin. The image of interior structure in Guqin was investigated by overall scanning based on non-destructive testing technology of computed tomography, which texture of faceplate, connection method between faceplate and soleplate and interior defects were studied. The three-dimensional reconstruction of Guqin cavity was achieved through Mimics software of surface rendering method and put the two-dimensional CT tomography images convert into three-dimensional, which more complete show interior structural form in Guqin, and finally the parameter of cavity dimensions was obtained. Experimental research shows that there is significant difference in Guqin interior structure between Zhong-ni and Luo-xia type, in which the fluctuation of the interior surfacein Zhong-ni type's is larger than that in Luo-xia type; the interior volume of Zhong-ni typeis less than that of Luo-xia type, especially in Guqin neck. The accurate internal information of Guqin obtained through the computed tomography (CT) technology will provide technical support for the Guqin manufacture craft and the quality examination, as well as provide the reference in the aspect of non-destructive testing for other traditional precious internal structure research.

  14. A new non-destructive readout by using photo-recovered surface potential contrast.

    PubMed

    Wang, Le; Jin, Kui-juan; Gu, Jun-xing; Ma, Chao; He, Xu; Zhang, Jiandi; Wang, Can; Feng, Yu; Wan, Qian; Shi, Jin-an; Gu, Lin; He, Meng; Lu, Hui-bin; Yang, Guo-zhen

    2014-11-10

    Ferroelectric random access memory is still challenging in the feature of combination of room temperature stability, non-destructive readout and high intensity storage. As a non-contact and non-destructive information readout method, surface potential has never been paid enough attention because of the unavoidable decay of the surface potential contrast between oppositely polarized domains. That is mainly due to the recombination of the surface movable charges around the domain walls. Here, by introducing a laser beam into the combination of piezoresponse force microscopy and Kelvin probe force microscopy, we demonstrate that the surface potential contrast of BiFeO3 films can be recovered under light illumination. The recovering mechanism is understood based on the redistribution of the photo-induced charges driven by the internal electric field. Furthermore, we have created a 12-cell memory pattern based on BiFeO3 films to show the feasibility of such photo-assisted non-volatile and non-destructive readout of the ferroelectric memory.

  15. Non-destructive Phenotyping to Identify Brachiaria Hybrids Tolerant to Waterlogging Stress under Field Conditions.

    PubMed

    Jiménez, Juan de la Cruz; Cardoso, Juan A; Leiva, Luisa F; Gil, Juanita; Forero, Manuel G; Worthington, Margaret L; Miles, John W; Rao, Idupulapati M

    2017-01-01

    Brachiaria grasses are sown in tropical regions around the world, especially in the Neotropics, to improve livestock production. Waterlogging is a major constraint to the productivity and persistence of Brachiaria grasses during the rainy season. While some Brachiaria cultivars are moderately tolerant to seasonal waterlogging, none of the commercial cultivars combines superior yield potential and nutritional quality with a high level of waterlogging tolerance. The Brachiaria breeding program at the International Center for Tropical Agriculture, has been using recurrent selection for the past two decades to combine forage yield with resistance to biotic and abiotic stress factors. The main objective of this study was to test the suitability of normalized difference vegetation index (NDVI) and image-based phenotyping as non-destructive approaches to identify Brachiaria hybrids tolerant to waterlogging stress under field conditions. Nineteen promising hybrid selections from the breeding program and three commercial checks were evaluated for their tolerance to waterlogging under field conditions. The waterlogging treatment was imposed by applying and maintaining water to 3 cm above soil surface. Plant performance was determined non-destructively using proximal sensing and image-based phenotyping and also destructively via harvesting for comparison. Image analysis of projected green and dead areas, NDVI and shoot biomass were positively correlated (r ≥ 0.8). Our results indicate that image analysis and NDVI can serve as non-destructive screening approaches for the identification of Brachiaria hybrids tolerant to waterlogging stress.

  16. A new non-destructive readout by using photo-recovered surface potential contrast

    PubMed Central

    Wang, Le; Jin, Kui-juan; Gu, Jun-xing; Ma, Chao; He, Xu; Zhang, Jiandi; Wang, Can; Feng, Yu; Wan, Qian; Shi, Jin-an; Gu, Lin; He, Meng; Lu, Hui-bin; Yang, Guo-zhen

    2014-01-01

    Ferroelectric random access memory is still challenging in the feature of combination of room temperature stability, non-destructive readout and high intensity storage. As a non-contact and non-destructive information readout method, surface potential has never been paid enough attention because of the unavoidable decay of the surface potential contrast between oppositely polarized domains. That is mainly due to the recombination of the surface movable charges around the domain walls. Here, by introducing a laser beam into the combination of piezoresponse force microscopy and Kelvin probe force microscopy, we demonstrate that the surface potential contrast of BiFeO3 films can be recovered under light illumination. The recovering mechanism is understood based on the redistribution of the photo-induced charges driven by the internal electric field. Furthermore, we have created a 12-cell memory pattern based on BiFeO3 films to show the feasibility of such photo-assisted non-volatile and non-destructive readout of the ferroelectric memory. PMID:25381929

  17. Non-destructive mapping of grain orientations in 3D by laboratory X-ray microscopy

    PubMed Central

    McDonald, S. A.; Reischig, P.; Holzner, C.; Lauridsen, E. M.; Withers, P. J.; Merkle, A. P.; Feser, M.

    2015-01-01

    The ability to characterise crystallographic microstructure, non-destructively and in three-dimensions, is a powerful tool for understanding many aspects related to damage and deformation mechanisms in polycrystalline materials. To this end, the technique of X-ray diffraction contrast tomography (DCT) using monochromatic synchrotron and polychromatic laboratory X-ray sources has been shown to be capable of mapping crystal grains and their orientations non-destructively in 3D. Here we describe a novel laboratory-based X-ray DCT modality (LabDCT), enabling the wider accessibility of the DCT technique for routine use and in-depth studies of, for example, temporal changes in crystallographic grain structure non-destructively over time through ‘4D’ in situ time-lapse studies. The capability of the technique is demonstrated by studying a titanium alloy (Ti-β21S) sample. In the current implementation the smallest grains that can be reliably detected are around 40 μm. The individual grain locations and orientations are reconstructed using the LabDCT method and the results are validated against independent measurements from phase contrast tomography and electron backscatter diffraction respectively. Application of the technique promises to provide important insights related to the roles of recrystallization and grain growth on materials properties as well as supporting 3D polycrystalline modelling of materials performance. PMID:26494523

  18. Insight into hydrogen bonding of uranyl hydroxide layers and capsules by use of 1H magic-angle spinning NMR spectroscopy [Insight into the hydrogen bonding for uranyl hydroxides using 1H MAS NMR spectroscopy

    DOE PAGES

    Alam, Todd M.; Liao, Zuolei; Nyman, May; ...

    2016-04-27

    Solid-state 1H magic-angle spinning (MAS) NMR was used to investigate local proton environments in anhydrous [UO2(OH)2] (α-UOH) and hydrated uranyl hydroxide [(UO2)4O(OH)6·5H2O (metaschoepite). For the metaschoepite material, proton resonances of the μ2-OH hydroxyl and interlayer waters were resolved, with two-dimensional (2D) double-quantum (DQ) 1H–1H NMR correlation experiments revealing strong dipolar interactions between these different proton species. The experimental NMR results were combined with first-principles CASTEP GIPAW (gauge including projector-augmented wave) chemical shift calculations to develop correlations between hydrogen-bond strength and observed 1H NMR chemical shifts. Furthermore, these NMR correlations allowed characterization of local hydrogen-bond environments in uranyl U24 capsules andmore » of changes in hydrogen bonding that occurred during thermal dehydration of metaschoepite.« less

  19. Single-Crystal Time-of-Flight Neutron Diffraction and Magic-Angle-Spinning NMR Spectroscopy Resolve the Structure and (1)H and (7)Li Dynamics of the Uranyl Peroxide Nanocluster U60.

    PubMed

    Olds, Travis A; Dembowski, Mateusz; Wang, Xiaoping; Hoffman, Christina; Alam, Todd M; Hickam, Sarah; Pellegrini, Kristi L; He, Junhong; Burns, Peter C

    2017-08-21

    Single-crystal time-of-flight neutron diffraction has provided atomic resolution of H atoms of H2O molecules and hydroxyl groups, as well as Li cations in the uranyl peroxide nanocluster U60. Solid-state magic-angle-spinning nuclear magnetic resonance (MAS NMR) spectroscopy was used to confirm the dynamics of these constituents, revealing the transportation of Li atoms and H2O through cluster walls. H atoms of hydroxyl units that are located on the cluster surface are involved in the transfer of H2O and Li cations from inside to outside and vice versa. This exchange occurs as a concerted motion and happens rapidly even in the solid state. As a consequence of its large size and open hexagonal pores, U60 exchanges Li cations more rapidly compared to other uranyl nanoclusters.

  20. The use of non destructive biomarkers in the study of marine mammals.

    PubMed

    M Cristina Fossi And Letizia Marsili

    1997-01-01

    Marine mammals have been subject to heavy anthropogenic pressure by direct killing and chemical pollution all over the world. Most studies of contamination and biomarker responses in marine mammals have been conducted using animals killed by hunting out of a total of 12 cetacean species studied, 45 of the specimens were obtained by sacrificing the animal; out of a total of eight pinniped species studied, 40 of the specimens were obtained by killing. The development of a series of non destructive techniques to evaluate biomarker responses and residue levels is recommended for the hazard assessment and conservation of endangered species of marine mammals. Here we review the current status of the non destructive biomarker approach in marine mammals, describing the biological materials available for non destructive tests in stranded brain, liver, blood, skin, subcutaneous blubber, muscle and fur and free ranging animals blood, skin biopsy, fur and faeces and the respective biomarker techniques mixed function oxidase activity and DNA damage in skin biopsy samples; porphyrins in faeces and fur; esterases, porphyrins, clinical biochemical parameter, vitamin A and micronuclei in blood samples. Residue analysis can be carried out in the various biological materials. We also report the results of applying this methodological approach to cetaceans minke whale Balaenoptera acutorostrata, fin whale-- Balaenoptera physalus, beluga whale-- Delphinapterus leucas, short finned pilot whale-- Globicephala macrorhynchus, harbour porpoise -- Phocoena phocoena, Rissos dolphin-- Risso s Grampus griseus, Dall s porpoise-- Phocoenoides dalli dalli, melon headed whale-- Peponocephala electra, bottlenose dolphin -- Tursiops truncatus, striped dolphin-- Stenella coeruleoalba, spinner dolphin-- Stenella longirostris, killer whale-- Orcinus orca and pinnipeds northern fur seal- Callorhinus ursinus, hooded seal-- Cystophora cristata, grey seal-- Halichoerus grypus, harbour seal-- Phoca vitulina

  1. Non-destructive Assessment of Engineered Cartilage Composition by Near Infrared Spectroscopy

    PubMed Central

    McGoverin, Cushla M.; Hanifi, Arash; Palukuru, Uday P.; Yousefi, Farzad; Glenn, Padraig B. M.; Shockley, Michael; Spencer, Richard G.; Pleshko, Nancy

    2016-01-01

    Tissue engineering presents a strategy to overcome the limitations of current tissue healing methods. Scaffolds, cells, external growth factors and mechanical input are combined in an effort to obtain constructs with properties that mimic native tissues. However, engineered constructs developed using similar culture environments can have very different matrix composition and biomechanical properties. Accordingly, a non-destructive technique to assess constructs during development such that appropriate compositional endpoints can be defined is desirable. Near infrared spectroscopy (NIRS) analysis is a modality being investigated to address the challenges associated with current evaluation techniques, which includes non-destructive compositional assessment. In the present study, cartilage tissue constructs were grown using chondrocytes seeded onto polyglycolic acid (PGA) scaffolds in similar environments in three separate tissue culture experiments and monitored using NIRS. Multivariate partial least squares (PLS) analysis models of NIR spectra were calculated and used to predict tissue composition, with biochemical assay information used as the reference data. Results showed that for combined data from all tissue culture experiments, PLS models were able to assess composition with significant correlations to reference values, including engineered cartilage water (at 5200 cm−1, R = 0.68, p = 0.03), proteoglycan (at 4310 cm−1, R = 0.82, p = 0.007), and collagen (at 4610 cm−1, R = 0.84, p = 0.005). In addition, degradation of PGA was monitored using specific NIRS frequencies. These results demonstrate that NIR spectroscopy combined with multivariate analysis provides a non-destructive modality to assess engineered cartilage, which could provide information to determine the optimal time for tissue harvest for clinical applications. PMID:26817457

  2. A Monte Carlo approach applied to ultrasonic non-destructive testing

    NASA Astrophysics Data System (ADS)

    Mosca, I.; Bilgili, F.; Meier, T.; Sigloch, K.

    2012-04-01

    Non-destructive testing based on ultrasound allows us to detect, characterize and size discrete flaws in geotechnical and architectural structures and materials. This information is needed to determine whether such flaws can be tolerated in future service. In typical ultrasonic experiments, only the first-arriving P-wave is interpreted, and the remainder of the recorded waveform is neglected. Our work aims at understanding surface waves, which are strong signals in the later wave train, with the ultimate goal of full waveform tomography. At present, even the structural estimation of layered media is still challenging because material properties of the samples can vary widely, and good initial models for inversion do not often exist. The aim of the present study is to combine non-destructive testing with a theoretical data analysis and hence to contribute to conservation strategies of archaeological and architectural structures. We analyze ultrasonic waveforms measured at the surface of a variety of samples, and define the behaviour of surface waves in structures of increasing complexity. The tremendous potential of ultrasonic surface waves becomes an advantage only if numerical forward modelling tools are available to describe the waveforms accurately. We compute synthetic full seismograms as well as group and phase velocities for the data. We invert them for the elastic properties of the sample via a global search of the parameter space, using the Neighbourhood Algorithm. Such a Monte Carlo approach allows us to perform a complete uncertainty and resolution analysis, but the computational cost is high and increases quickly with the number of model parameters. Therefore it is practical only for defining the seismic properties of media with a limited number of degrees of freedom, such as layered structures. We have applied this approach to both synthetic layered structures and real samples. The former contributed to benchmark the propagation of ultrasonic surface

  3. Research Performed within the Non-Destructive Evaluation Team at NASA Glenn Research Center

    NASA Technical Reports Server (NTRS)

    Burns, Erin A.

    2004-01-01

    Non-destructive testing is essential in many fields of manufacturing and research in order to perform reliable examination of potentially damaged materials and parts without destroying the inherent structure of the materials. Thus, the Non-Destructive Evaluation (NDE) Team at NASA Glenn Research Center partakes in various projects to improve materials testing equipment as well as analyze materials, material defects, and material deficiencies. Due to the array of projects within the NDE Team at this time, five research aims were supplemental to some current projects. A literature survey of "DE and testing methodologies as related to rocks was performed. Also, Mars Expedition Rover technology was assessed to understand the requirements for instrumentation in harsh space environments (e.g. temperature). Potential instrumentation and technologies were also considered and documented. The literature survey provided background and potential sources for a proposal to acquire funding for ultrasonic instrumentation on board a future Mars expedition. The laboratory uses a Santec Systems AcousticScope AS200 acoustography system. Labview code was written within the current program in order to improve the current performance of the acoustography system. A sample of Reinforced Carbon/Carbon (RCC) material from the leading edge of the space shuttle underwent various non-destructive tests (guided wave scanning, thermography, computed tomography, real time x-ray, etc.) in order to characterize its structure and examine possible defects. Guided wave scan data of a ceramic matrix composite (CMC) panel was reanalyzed utilizing image correlations and signal processing variables. Additional guided wave scans and thermography were also performed on the CMC panel. These reevaluated data and images will be used in future presentations and publications. An additional axis for the guided wave scanner was designed, constructed, and implemented. This additional axis allowed incremental spacing

  4. Non-destructive estimation of foliar carotenoid content of tree species using merged vegetation indices.

    PubMed

    Fassnacht, Fabian E; Stenzel, Stefanie; Gitelson, Anatoly A

    2015-03-15

    Leaf pigment content is an important indicator of plant status and can serve to assess the vigor and photosynthetic activity of plants. The application of spectral information gathered from laboratory, field and remote sensing-based spectrometers to non-destructively assess total chlorophyll (Chl) content of higher plants has been demonstrated in earlier studies. However, the precise estimation of carotenoid (Car) content with non-destructive spectral measurements has so far not reached accuracies comparable to the results obtained for Chl content. Here, we examined the potential of a recently developed angular vegetation index (AVI) to estimate total foliar Car content of three tree species. Based on an iterative search of all possible band combinations, we identified a best candidate AVIcar. The identified index showed quite close but essentially not linear relation with Car contents of the examined species with increasing sensitivity to high Car content and a lack of sensitivity to low Car content for which earlier proposed vegetation indices (VI) performed better. To make use of the advantages of both VI types, we developed a simple merging procedure, which combined the AVIcar with two earlier proposed carotenoid indices. The merged indices had close linear relationship with total Car content and outperformed all other examined indices. The merged indices were able to accurately estimate total Car content with a percental root mean square error (%RMSE) of 8.12% and a coefficient of determination of 0.88. Our findings were confirmed by simulations using the radiative transfer model PROSPECT-5. For simulated data, the merged indices again showed a quasi linear relationship with Car content. This strengthens the assumption that the proposed merged indices have a general ability to accurately estimate foliar Car content. Further examination of the proposed merged indices to estimate foliar Car content of other plant species is desirable to prove the general

  5. Evaluation of Mechanical Properties of Nuclear Materials Using Non-Destructive Ball Indentation Technique

    SciTech Connect

    Mathew, M.D.; Linga Murty, K.

    2002-07-01

    Integrity of structural components depends on the deformation and fracture behavior of materials. For evaluating the material condition in-service, it is generally not feasible or practical or advisable to cut samples from operating structures. Non-destructive testing (NDT) techniques are required to evaluate the mechanical properties. Although several NDT techniques such as ultrasound, magnetic strength, Barkhausen noise, microhardness etc., are employed for estimating the mechanical property degradation, these methodologies are generally empirical and indirect. Automated Ball Indentation (ABI) is a non-destructive testing technique for direct measurement of mechanical and fracture properties of metallic engineering materials. Because of the small area over which the test is carried out, it is possible to determine point to point variations in the mechanical and fracture properties, such as those that exist in weldments. Although ABI technique is non-intrusive, it is a state-of-the-art mechanical test that measures directly the current/local deformation behavior of the material. In this paper, we present results from studies on the application of ABI technique to determine tensile and fracture properties of ferritic steels, an austenitic stainless steel, a nickel base superalloy and Zircaloy in different thermo-mechanical conditions. The effects of aging and cold work on these properties were determined from the ABI tests. Gradients in mechanical properties of ferritic steel welds, particularly in the narrow heat-affected zone, were clearly established. ABI technique was found to be useful in determining the anisotropy in the tensile properties of Zircaloy cladding tubes. The technique has potential as a non-destructive method for assessing structural integrity of aged components. (authors)

  6. Fast Non-Destructive Evaluation of Superconducting Magnet Wires using a Flow-Through SQUID Microscope

    NASA Astrophysics Data System (ADS)

    Matthews, John; Wellstood, Frederick; Weinstock, Harold

    2006-03-01

    We have developed a cryocooled high-Tc SQUID microscope for fast non-destructive evaluation (NDE) of long wires, designed for detecting defects in superconducting magnet wire. A feedthrough mechanism pulls the wire at speeds of up to 20 cm/s through a thin mylar tube that separates the room temperature wire from the SQUID. We present results on test wires where we detect defects down to about 0.3 mm diameter. We discuss how we extract information from the data, such as defect size and location, and also outline a method for fast automated detection of defects in long wires.

  7. Non-destructive method for determining neutron exposure and constituent concentrations of a body

    DOEpatents

    Gold, Raymond; McElroy, William N.

    1986-01-01

    A non-destructive method for determination of neutron exposure and constituent concentrations in an object, such as reactor pressure vessel, is based on the observation of characteristic gamma-rays emitted by activation products in the object by using a unique continuous gamma-ray spectrometer. The spectrometer views the object through appropriate collimators to determine the absolute emission rate of these characteristic gamma-rays, thereby ascertaining the absolute activity of given activation products in the object. These data can then be used to deduce the spatial and angular dependence of neutron exposure or the spatial constituent concentration at regions of interest within the object.

  8. Non-destructive method for determining neutron exposure and constituent concentrations of a body

    DOEpatents

    Gold, R.; McElroy, W.N.

    1984-02-22

    A non-destructive method for determination of neutron exposure and constituent concentrations in an object, such as a reactor pressure vessel, is based on the observation of characteristic gamma-rays emitted by activation products in the object by using a unique continuous gamma-ray spectrometer. The spectrometer views the object through appropriate collimators to determine the absolute emission rate of these characteristic gamma-rays, thereby ascertaining the absolute activity of given activation products in the object. These data can then be used to deduce the spatial and angular dependence of neutron exposure or the spatial constituent concentrations at regions of interest within the object.

  9. Non-destructive Testing by Infrared Thermography Under Random Excitation and ARMA Analysis

    NASA Astrophysics Data System (ADS)

    Bodnar, J. L.; Nicolas, J. L.; Candoré, J. C.; Detalle, V.

    2012-11-01

    Photothermal thermography is a non-destructive testing (NDT) method, which has many applications in the field of control and characterization of thin materials. This technique is usually implemented under CW or flash excitation. Such excitations are not adapted for control of fragile materials or for multi-frequency analysis. To allow these analyses, in this article, the use of a new control mode is proposed: infrared thermography under random excitation and auto regressive moving average analysis. First, the principle of this NDT method is presented. Then, the method is shown to permit detection, with low energy constraints, of detachments situated in mural paintings.

  10. Delayed Gamma-ray Spectroscopy for Non-Destructive Assay of Nuclear Materials

    SciTech Connect

    Mozin, Vladimir; Ludewigt, Bernhard; Campbell, Luke; Favalli, Andrea; Hunt, Alan

    2014-10-09

    This project addresses the need for improved non-destructive assay techniques for quantifying the actinide composition of spent nuclear fuel and for the independent verification of declared quantities of special nuclear materials at key stages of the fuel cycle. High-energy delayed gamma-ray spectroscopy following neutron irradiation is a potential technique for directly assaying spent fuel assemblies and achieving the safeguards goal of quantifying nuclear material inventories for spent fuel handling, interim storage, reprocessing facilities, repository sites, and final disposal. Other potential applications include determination of MOX fuel composition, characterization of nuclear waste packages, and challenges in homeland security and arms control verification.

  11. Application of magnetic resonance imaging to non-destructive void detection in watermelon

    NASA Astrophysics Data System (ADS)

    Saito, K.; Miki, T.; Hayashi, S.; Kajikawa, H.; Shimada, M.; Kawate, Y.; Nishizawa, T.; Ikegaya, D.; Kimura, N.; Takabatake, K.; Sugiura, N.; Suzuki, M.

    A novel application of magnetic resonance imaging (MRI) is described. The possibility of utilizing MRI for non-destructive quality evaluation of watermelons was studied. In this study, we applied MRI to the detection of internal voids in watermelons. In order to increase the measurement rate, we employed a one-dimensional projection profile method instead of observing a two-dimensional cross-sectional image. The void detection was carried out with this technique over 30 samples and 28 samples were correctly evaluated. The measurement rate was 900 ms per sample, which is an acceptable speed for a sorting machine in the agricultural field.

  12. Non-destructive testing of biaxial stress state in ferromagnetic materials

    NASA Astrophysics Data System (ADS)

    Vengrinovich, V. L.; Vintov, D. A.; Dmitrovich, D. V.

    2014-02-01

    The technique for biaxial stress state quantitative non destructive testing using magnetic, namely Barkhausen Noise, measurements is developed and checked experimentally. The main elaboration concerns the application of uni-axial calibration data for bi-axial stress measurement in the material which treatment pre-history is not definitely known. The article is aimed to get over difficulties, accompanying factual nondestructive stress evaluation, implied from its tensor nature. The developed technique of stress calibration and measurement assumes the bi-axial stress components recovery from uni-axial magnetic and Barkhausen noise measurement results. The complete technology, based on new calibration procedure with grid diagrams is considered in the article.

  13. Non-Destructive Testing with Atmospheric Pressure Radio-Frequency Plasma

    NASA Astrophysics Data System (ADS)

    May, A.; Andarawis, E.

    2007-03-01

    We summarize our recent work using radio-frequency (RF) atmospheric pressure plasma (APP) for non-destructive evaluation (NDE), specifically for: (1) Clearance sensing (0-5mm) on rotating components, and (2) Generation of broadband ultrasound in air at 900kHz. RF-APP showed potential in both of these common NDE requirements, but further work is required to better characterize and optimize the performance of the new techniques. Application of RF-APP to other NDE disciplines, such as plasma spectroscopy and gas flow measurement, is also likely to be advantageous, especially in harsh environments where existing approaches are prohibitively expensive or complex.

  14. [NIR spectrometer for non-destruction measurement of oil contents in a corn seed].

    PubMed

    Cui, Zhi-li; Xie, Jin-chun; Wang, Nan; Pan, Ling-ling; Song, Tong-ming; Zhang, Ye-hui; Xu, Xiao-jie

    2005-11-01

    NIR spectromneter for non-destruction measurement of oil contents in an integrated kernel of corn was manufactured. Using LED (light emitting diode) as the light source and six filters as the monochromator, the specifications of the instrument are compared with those of the commercial instruments. The regression coefficient, the standard error, and the relative error of measuring oil contents in an integrated kernel of corn are 0.9688, 0.72 and 0.062 respectively. The results meet the demand of high-oil corn breeding.

  15. Methods for Non-destructive Temperature Measurements in a Magneto-Optical Trap

    NASA Astrophysics Data System (ADS)

    Narducci, Frank A.; Duncan, Dwight; White, Grady R.; Lough, James; Davis, Jon P.

    2009-05-01

    Certain practical applications for precision measurements by atom interferometers require knowledge of the input atom cloud's temperature from realization to realization. Recent work [1,2] has shown how to measure the temperature of atoms in a magneto-optical trap in a non-destructive, in situ manner. We discuss an alternate, simpler method for the nondestructive measurement of the temperature of an atom cloud and compare our method with earlier techniques. [4pt] [1] T. Brzozowski, M. Brzozowska, J. Zachorowski, M. Zawada, W. Gawlik, PRA, 71, 013401 (2005).[0pt] [2] M. Brzozowska, T. Brzozowski J. Zachorowski, W. Gawlik, PRA, 72, 061401(R), (2005).

  16. Homeland Security, Medical, Pharmaceutical and Non-destructive Testing Applications of Terahertz Radiation

    NASA Astrophysics Data System (ADS)

    Kemp, Michael

    2005-03-01

    The terahertz region of the electromagnetic spectrum (300GHz-10THz) spans the region between radio and light. Recent advances in terahertz source, detector and systems technology are enabling new applications across a number of fields, based on both terahertz imaging and spectroscopy. This paper reviews our recent work on the development of practical systems and applications in security screening for the detection of explosives and non-metallic weapons; in medical imaging for cancer detection; as well as applications in non-destructive testing and the pharmaceutical industry.

  17. Non-destructive qualification tests for ITER cryogenic axial insulating breaks

    SciTech Connect

    Kosek, Jacek; Lopez, Roberto; Tommasini, Davide; Rodriguez-Mateos, Felix

    2014-01-29

    In the ITER superconducting magnets the dielectric separation between the CICC (Cable-In-Conduit Conductors) and the helium supply pipes is made through the so-called insulating breaks (IB). These devices shall provide the required dielectric insulation at a 30 kV level under different types of stresses and constraints: thermal, mechanical, dielectric and ionizing radiations. As part of the R and D program, the ITER Organization launched contracts with industrial companies aimed at the qualification of the manufacturing techniques. After reviewing the main functional aspects, this paper describes and discusses the protocol established for non-destructive qualification tests of the prototypes.

  18. Non-destructive terahertz imaging of illicit drugs using spectral fingerprints

    NASA Astrophysics Data System (ADS)

    Kawase, Kodo; Ogawa, Yuichi; Watanabe, Yuuki; Inoue, Hiroyuki

    2003-10-01

    The absence of non-destructive inspection techniques for illicit drugs hidden in mail envelopes has resulted in such drugs being smuggled across international borders freely. We have developed a novel basic technology for terahertz imaging, which allows detection and identification of drugs concealed in envelopes, by introducing the component spatial pattern analysis. The spatial distributions of the targets are obtained from terahertz multispectral transillumination images, using absorption spectra measured with a tunable terahertz-wave source. The samples we used were methamphetamine and MDMA, two of the most widely consumed illegal drugs in Japan, and aspirin as a reference.

  19. The development of non destructive remote measurement method of concrete contamination

    SciTech Connect

    Stepanov, V E; Potapov, V N; Ivanov, O P

    2013-07-01

    In the frame of the decommissioning of nuclear power plants or laboratories, the penetration depth of the contamination in concrete surfaces: walls, floor, is unknown. Its knowledge requires sample analysis, that is time consuming and expensive. The main goal of the work is to define and evaluate a non-destructive measurement technique for the evaluation of the contamination depth in concrete. Estimation of accuracy of measurements for different contamination levels, time of measurement, value of natural radionuclides (NRN) concentration in concrete and background radiation dose were carried out. The type of relevant detector depends of selected limiting sensitivity, the weight and sizes of the device. (authors)

  20. Non-Destructive Evaluation Method and Apparatus for Measuring Acoustic Material Nonlinearity

    NASA Technical Reports Server (NTRS)

    Yost, William T. (Inventor); Cantrell, John H. (Inventor)

    2002-01-01

    An acoustic non-linearity parameter (beta) measurement method and system for Non-Destructive Evaluation (NDE) of materials and structural members obviates the need for electronic calibration of the measuring equipment. Unlike known substitutional measuring techniques requiring elaborate calibration procedures, the electrical outputs of the capacitive detector of a sample with known beta and the test sample of unknown beta are compared to determine the unknown beta. In order to provide the necessary stability of the present-inventive reference-based approach, the bandpass filters of the measurement system are maintained in a temperature-controlled environment, and the line voltage supplied to said amplifiers is well-regulated.

  1. Computed tomography for non-destructive evaluation of composites: Applications and correlations

    NASA Technical Reports Server (NTRS)

    Goldberg, B.; Hediger, L.; Noel, E.

    1985-01-01

    The state-of-the-art fabrication techniques for composite materials are such that stringent species-specific acceptance criteria must be generated to insure product reliability. Non-destructive evaluation techniques including computed tomography (CT), X-ray radiography (RT), and ultrasonic scanning (UT) are investigated and compared to determine their applicability and limitations to graphite epoxy, carbon-carbon, and carbon-phenolic materials. While the techniques appear complementary, CT is shown to provide significant, heretofore unattainable data. Finally, a correlation of NDE techniques to destructive analysis is presented.

  2. Magnetic non-destructive evaluation of hardening of cold rolled reactor pressure vessel steel

    NASA Astrophysics Data System (ADS)

    Wang, Xuejiao; Qiang, Wenjiang; Shu, Guogang

    2017-08-01

    Non-destructive test (NDT) of reactor pressure vessel (RPV) steel is urgently required due to the life extension program of nuclear power plant. Here magnetic NDT of cold rolled RPV steel is studied. The strength, hardness and coercivity increase with the increasing deformation, and a good linear correlation between the increment of coercivity, hardness and yield strength is found, which may be helpful to develop magnetic NDT of degradation of RPV steel. It is also found that besides dislocation density, the distribution of dislocations may affect coercivity as well.

  3. Application of golay complementary coded excitation schemes for non-destructive testing of sandwich structures

    NASA Astrophysics Data System (ADS)

    Arora, Vanita; Mulaveesala, Ravibabu

    2017-06-01

    In recent years, InfraRed Thermography (IRT) has become a widely accepted non-destructive testing technique to evaluate the structural integrity of composite sandwich structures due to its full-field, remote, fast and in-service inspection capabilities. This paper presents a novel infrared thermographic approach named as Golay complementary coded thermal wave imaging is presented to detect disbonds in a sandwich structure having face sheets from Glass/Carbon Fibre Reinforced (GFR/CFR) laminates and core of the wooden block.

  4. Additive Manufacturing (AM) Activities and Non-Destructive Evaluation (NDE) at GSFC

    NASA Technical Reports Server (NTRS)

    Jones, Justin S.

    2017-01-01

    NASA personnel will be meeting with a delegation from the Japan Aerospace Exploration Agency (JAXA) Office of Safety and Mission Assurance (OSMA) at Langley Research Center on 2217 through 3217. The purpose of the meeting is a technical interchange between NASA and JAXA to discuss Non-Destructive Evaluation (NDE) of Additive Manufacturing (AM) parts and the HALT process (relates to accelerated life testing). The visitors will be a small group of Japanese citizens. Goddard Space Flight Center (GSFC) has been asked to participate in the meeting, either in person or via teleconference. This presentation covers NDE efforts at GSFC and provides a cursory overview of AM and lab capabilities.

  5. PREFACE: III All-Russian Scientific and Practical Conference on Innovations in Non-Destructive Testing (SibTest 2015)

    NASA Astrophysics Data System (ADS)

    2016-01-01

    This issue of the journal is devoted to the research and studies presented at the III All-Russian Scientific and Practical Conference on Innovations in Non-Destructive Testing SibTest. The conference was held in Altai, Russia, on 27-31 July 2015. The conference brought together experts from different countries and organizations who had a great opportunity to share knowledge during oral and poster presentations and to initiate discussions on topics that are of interest to the conference attendees. The conference aimed to discuss innovative methods and the application of advanced technologies in non-destructive testing. The conference also attempted to bring together university, academic and industrial science, to expand the co-operation of scientists from different countries in research and development and the commercialization of innovative technologies in non-destructive testing. The key themes of the conference were: ultrasonic and acoustic testing; electromagnetic and thermal testing; various types of radiation non-destructive testing; passive and active testing techniques. The conference organizers are the Institute of Non-Destructive Testing, Tomsk Polytechnic University, with the assistance of the Russian Society for Non-Destructive Testing and Technical Diagnostics, Institute of Strength Physics and Materials Science, Siberian Branch of the Russian Academy of Sciences, National Research Tomsk State University, Moscow State Institute of Radio Engineering, Electronics and Automation.

  6. NON-DESTRUCTIVE THERMAL BARRIER COATING SPALLATION PREDICTION BY A LOADBASED MICRO-INDENTATION TECHNIQUE

    SciTech Connect

    J. M. Tannenbaum; K. Lee; B. S.-J. Kang; M.A. Alvin

    2010-11-18

    Currently, the durability and life cycle of thermal barrier coatings (TBC) applied to gas turbine blades and combustor components are limiting the maximum temperature and subsequent efficiency at which gas turbine engines operate. The development of new materials, coating technologies and evaluation techniques is required if enhanced efficiency is to be achieved. Of the current ceramic coating materials used in gas turbine engines, yttria stabilized zirconia (YSZ) is most prevalent, its low thermal conductivity, high thermal expansion coefficient and outstanding mechanical strength make it ideal for use in TBC systems. However, residual stresses caused by coefficients of thermal expansion mismatches within the TBC system and unstable thermally grown oxides are considered the primary causes for its premature and erratic spallation failure. Through finite element simulations, it is shown that the residual stresses generated within the thermally grown oxide (TGO), bond coat (BC), YSZ and their interfaces create slight variations in indentation unloading surface stiffness response prior to spallation failure. In this research, seven air plasma sprayed and one electron beam physical vapor deposition yttria partially stabilized zirconia TBCs were subjected to isothermal and cyclic loadings at 1100°C. The associated coating degradation was evaluated using a non-destructive multiple partial unloading micro-indentation procedure. The results show that the proposed non-destructive micro-indentation evaluation technique can be an effective and specimenindependent TBC failure prediction tool capable of determining the location of initial spallation failure prior to its actual occurrence.

  7. Non-destructive forensic latent fingerprint acquisition with chromatic white light sensors

    NASA Astrophysics Data System (ADS)

    Leich, Marcus; Kiltz, Stefan; Dittmann, Jana; Vielhauer, Claus

    2011-02-01

    Non-destructive latent fingerprint acquisition is an emerging field of research, which, unlike traditional methods, makes latent fingerprints available for additional verification or further analysis like tests for substance abuse or age estimation. In this paper a series of tests is performed to investigate the overall suitability of a high resolution off-the-shelf chromatic white light sensor for the contact-less and non-destructive latent fingerprint acquisition. Our paper focuses on scanning previously determined regions with exemplary acquisition parameter settings. 3D height field and reflection data of five different latent fingerprints on six different types of surfaces (HDD platter, brushed metal, painted car body (metallic and non-metallic finish), blued metal, veneered plywood) are experimentally studied. Pre-processing is performed by removing low-frequency gradients. The quality of the results is assessed subjectively; no automated feature extraction is performed. Additionally, the degradation of the fingerprint during the acquisition period is observed. While the quality of the acquired data is highly dependent on surface structure, the sensor is capable of detecting the fingerprint on all sample surfaces. On blued metal the residual material is detected; however, the ridge line structure dissolves within minutes after fingerprint placement.

  8. Early non-destructive biofouling detection and spatial distribution: Application of oxygen sensing optodes.

    PubMed

    Farhat, N M; Staal, M; Siddiqui, A; Borisov, S M; Bucs, Sz S; Vrouwenvelder, J S

    2015-10-15

    Biofouling is a serious problem in reverse osmosis/nanofiltration (RO/NF) applications, reducing membrane performance. Early detection of biofouling plays an essential role in an adequate anti-biofouling strategy. Presently, fouling of membrane filtration systems is mainly determined by measuring changes in pressure drop, which is not exclusively linked to biofouling. Non-destructive imaging of oxygen concentrations (i) is specific for biological activity of biofilms and (ii) may enable earlier detection of biofilm accumulation than pressure drop. The objective of this study was to test whether transparent luminescent planar O2 optodes, in combination with a simple imaging system, can be used for early non-destructive biofouling detection. This biofouling detection is done by mapping the two-dimensional distribution of O2 concentrations and O2 decrease rates inside a membrane fouling simulator (MFS). Results show that at an early stage, biofouling development was detected by the oxygen sensing optodes while no significant increase in pressure drop was yet observed. Additionally, optodes could detect spatial heterogeneities in biofouling distribution at a micro scale. Biofilm development started mainly at the feed spacer crossings. The spatial and quantitative information on biological activity will lead to better understanding of the biofouling processes, contributing to the development of more effective biofouling control strategies. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Non-destructive dielectric assessment of water permeation in composite structures

    SciTech Connect

    Boinard, P.; Boinard, E.; Pethrick, R.A.; Banks, W.M.; Crane, R.L.

    2000-07-01

    Over the last ten years, the application of high frequency dielectric spectroscopy techniques for the assessment of composite structures has been investigated. Novel approaches to assess non-destructively the evolution during ageing of adhesively bonded carbon fiber reinforced plastic (CFRP) structures and bulk glass fiber reinforced plastic (GRP) structures are presented in this paper and the results are critically assessed. The applicability and limitations of dielectric measurements, in both frequency and time domain, to the monitoring of water ingress at 30 C and 60 C are examined. The correlation between gravimetric and high frequency dielectric spectroscopy data demonstrates the suitability of the techniques regarding the assessment of water uptake in composites structures and illustrates its potential as a non-destructive evaluation (NDE) technique. The dielectric time domain response (TDR) study of adhesively bonded structures indicates a new way to assess such structures. The approach for frequency domain analysis of bulk GRP using a coaxial probe technique indicates the potential portability of the technique for in-situ measurements.

  10. A Spatially Offset Raman Spectroscopy Method for Non-Destructive Detection of Gelatin-Encapsulated Powders

    PubMed Central

    Chao, Kuanglin; Dhakal, Sagar; Qin, Jianwei; Peng, Yankun; Schmidt, Walter F.; Kim, Moon S.; Chan, Diane E.

    2017-01-01

    Non-destructive subsurface detection of encapsulated, coated, or seal-packaged foods and pharmaceuticals can help prevent distribution and consumption of counterfeit or hazardous products. This study used a Spatially Offset Raman Spectroscopy (SORS) method to detect and identify urea, ibuprofen, and acetaminophen powders contained within one or more (up to eight) layers of gelatin capsules to demonstrate subsurface chemical detection and identification. A 785-nm point-scan Raman spectroscopy system was used to acquire spatially offset Raman spectra for an offset range of 0 to 10 mm from the surfaces of 24 encapsulated samples, using a step size of 0.1 mm to obtain 101 spectral measurements per sample. As the offset distance was increased, the spectral contribution from the subsurface powder gradually outweighed that of the surface capsule layers, allowing for detection of the encapsulated powders. Containing mixed contributions from the powder and capsule, the SORS spectra for each sample were resolved into pure component spectra using self-modeling mixture analysis (SMA) and the corresponding components were identified using spectral information divergence values. As demonstrated here for detecting chemicals contained inside thick capsule layers, this SORS measurement technique coupled with SMA has the potential to be a reliable non-destructive method for subsurface inspection and authentication of foods, health supplements, and pharmaceutical products that are prepared or packaged with semi-transparent materials. PMID:28335453

  11. Rapid non-destructive assessment of pork edible quality by using VIS/NIR spectroscopic technique

    NASA Astrophysics Data System (ADS)

    Zhang, Leilei; Peng, Yankun; Dhakal, Sagar; Song, Yulin; Zhao, Juan; Zhao, Songwei

    2013-05-01

    The objectives of this research were to develop a rapid non-destructive method to evaluate the edible quality of chilled pork. A total of 42 samples were packed in seal plastic bags and stored at 4°C for 1 to 21 days. Reflectance spectra were collected from visible/near-infrared spectroscopy system in the range of 400nm to 1100nm. Microbiological, physicochemical and organoleptic characteristics such as the total viable counts (TVC), total volatile basic-nitrogen (TVB-N), pH value and color parameters L* were determined to appraise pork edible quality. Savitzky-Golay (SG) based on five and eleven smoothing points, Multiple Scattering Correlation (MSC) and first derivative pre-processing methods were employed to eliminate the spectra noise. The support vector machines (SVM) and partial least square regression (PLSR) were applied to establish prediction models using the de-noised spectra. A linear correlation was developed between the VIS/NIR spectroscopy and parameters such as TVC, TVB-N, pH and color parameter L* indexes, which could gain prediction results with Rv of 0.931, 0.844, 0.805 and 0.852, respectively. The results demonstrated that VIS/NIR spectroscopy technique combined with SVM possesses a powerful assessment capability. It can provide a potential tool for detecting pork edible quality rapidly and non-destructively.

  12. Non destructive examination of UN / U-Si fuel pellets using neutrons (preliminary assessment)

    SciTech Connect

    Bourke, Mark Andrew; Vogel, Sven C.; Voit, Stewart Lancaster; Mcclellan, Kenneth James; Losko, Adrian S.; Tremsin, Anton

    2016-03-31

    Tomographic imaging and diffraction measurements were performed on nine pellets; four UN/ U Si composite formulations (two enrichment levels), three pure U3Si5 reference formulations (two enrichment levels) and two reject pellets with visible flaws (to qualify the technique). The U-235 enrichments ranged from 0.2 to 8.8 wt.%. The nitride/silicide composites are candidate compositions for use as Accident Tolerant Fuel (ATF). The monophase U3Si5 material was included as a reference. Pellets from the same fabrication batches will be inserted in the Advanced Test Reactor at Idaho during 2016. The goal of the Advanced Non-destructive Fuel Examination work package is the development and application of non-destructive neutron imaging and scattering techniques to ceramic and metallic nuclear fuels. Data reported in this report were collected in the LANSCE run cycle that started in September 2015 and ended in March 2016. Data analysis is ongoing; thus, this report provides a preliminary review of the measurements and provides an overview of the characterized samples.

  13. Study of concrete drilling for automated non-destructive evaluation and rehabilitation system for bridge decks

    NASA Astrophysics Data System (ADS)

    Trkov, Mitja; Liu, Fei; Yi, Jingang; Baruh, Haim

    2011-04-01

    Robotic drilling is the basic process for the non-destructive rehabilitation (NDR) system in the Automated Non-destructive Evaluation and Rehabilitation System (ANDERS) for bridge decks. In this paper, we present a study and testing of a concrete drilling process that is used for robotic drilling process for bridge decks repair. We first review the ANDERS and NDR design. Then we present the experimental setup for the drilling process study. A set of testing experiments are performed considering drilling process parameters such as drill bit size, drill rotating speed, drill thrust force and types of concrete composites. Based on the experiments and analysis, we identify and find that the optimal set of drilling process parameters for the ANDERS application is 1/4-inch bit size, drill rotational speed of 1500 rpm and thrust force around 35 lbs. We also demonstrate that the monitoring of drill feeding displacement and thrust force cannot be used to detect and identify the cracks in bridge decks.

  14. Non-destructive techniques for the detection of fungal infection in cereal grains.

    PubMed

    Orina, Irene; Manley, Marena; Williams, Paul J

    2017-10-01

    Infection of cereal grains by fungi is a serious problem worldwide. Depending on the environmental conditions, cereal grains may be colonised by different species of fungi. These fungi cause reduction in yield, quality and nutritional value of the grain; and of major concern is their production of mycotoxins which are harmful to both humans and animals. Early detection of fungal contamination is an essential control measure for ensuring storage longevity and food safety. Conventional methods for detection of fungal infection, such as culture and colony techniques or immunological methods are either slow, labour intensive or difficult to automate. In recent years, there has been an increasing need to develop simple, rapid, non-destructive methods for early detection of fungal infection and mycotoxins contamination in cereal grains. Methods such as near infrared (NIR) spectroscopy, NIR hyperspectral imaging, and electronic nose were evaluated for these purposes. This paper reviews the different non-destructive techniques that have been considered thus far for detection of fungal infection and mycotoxins in cereal grains, including their principles, application and limitations. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. Non-destructive observation of electrically detected magnetic resonance in bulk material using AC bias.

    PubMed

    Sato, Toshiyuki; Yokoyama, Hidekatsu; Ohya, Hiroaki

    2005-07-01

    DC bias is normally found in conventional measurements of electrically detected magnetic resonance (EDMR). Usually, electrodes are formed on the sample surface to make ohmic contacts for detecting changes in the electrical characteristics of the sample material. Thus, destructive procedures are required to detect the EDMR signal of bulk material with such methods. An AC bias detection technique was developed to allow the non-destructive EDMR measurement of bulk materials. An AC bridge circuit was constructed to detect the change in impedance of the sample, which when changed by ESR, an unbalanced AC voltage can be detected. By detecting this AC bias, it is possible to cancel the effects, such as Shottky barriers, that disturb the ohmic contact between the electrodes and a sample material. Further, the AC bias current penetrates the thin surface layer of a sample such as silicon oxide, which normally obstructs a DC current. This method was utilized using conductive rubber contacts for non-destructive EDMR measurements of part of a silicon wafer. EDMR spectra observed were the same as those obtained by the conventional method of using DC bias detection.

  16. Non-destructive observation of electrically detected magnetic resonance in bulk material using AC bias

    NASA Astrophysics Data System (ADS)

    Sato, Toshiyuki; Yokoyama, Hidekatsu; Ohya, Hiroaki

    2005-07-01

    DC bias is normally found in conventional measurements of electrically detected magnetic resonance (EDMR). Usually, electrodes are formed on the sample surface to make ohmic contacts for detecting changes in the electrical characteristics of the sample material. Thus, destructive procedures are required to detect the EDMR signal of bulk material with such methods. An AC bias detection technique was developed to allow the non-destructive EDMR measurement of bulk materials. An AC bridge circuit was constructed to detect the change in impedance of the sample, which when changed by ESR, an unbalanced AC voltage can be detected. By detecting this AC bias, it is possible to cancel the effects, such as Shottky barriers, that disturb the ohmic contact between the electrodes and a sample material. Further, the AC bias current penetrates the thin surface layer of a sample such as silicon oxide, which normally obstructs a DC current. This method was utilized using conductive rubber contacts for non-destructive EDMR measurements of part of a silicon wafer. EDMR spectra observed were the same as those obtained by the conventional method of using DC bias detection.

  17. Non-destructive Magnetic Evaluation of Laser Weld Quality in Hot Rolled Coils

    NASA Astrophysics Data System (ADS)

    Mohapatra, J. N.; Chakradhar, I.; Rao, K. R. C.; Rao, V. V. L.; Kaza, Marutiram

    2015-06-01

    Weld quality evaluation was conducted on laser welded thin sectsions (2 mm) of hot-rolled (HR) low-carbon steel coils during cold rolling process. The analysis revealed that the poor welds consisting of the weld defects like incomplete fusion, cluster of porosity, and large difference in hardness between the weld zone and base metal were responsible for the weld failures. Experiments were conducted by varying the welding parameters; laser power and welding speed to optimize the parameters for minimizing the weld defects. The optimized weld process parameters have helped elimination of weld defects and the results are verified with microscopy and microhardness measurements. As destructive evaluation techniques are time consuming and not always permitted in industrial applications, attempts have been made in the present investigation for the utilization of suitable non-destructive techniques for the evaluation of weld quality. Non-destructive magnetic techniques of magnetic hysteresis loop and magnetic Barkhausen emissions were used in the present investigation to establish possible correlations of magnetic properties across the weld seam with the mechanical property (microhardness) for evaluation of weld quality. It is inferred that the magnetic properties of coercivity and inverse of root mean square voltage can be effectively utilized to determine weld quality in HR steel coils.

  18. Non-destructive Testing of Forged Metallic Materials by Active Infrared Thermography

    NASA Astrophysics Data System (ADS)

    Maillard, S.; Cadith, J.; Bouteille, P.; Legros, G.; Bodnar, J. L.; Detalle, V.

    2012-11-01

    Nowadays, infrared thermography is considered as the reference method in many applications such as safety, the inspection of electric installations, or the inspection of buildings' heat insulation. In recent years, the evolution of both material and data-processing tools also allows the development of thermography as a real non-destructive testing method. Thus, by subjecting the element to be inspected to an external excitation and by analyzing the propagation of heat in the examined zone, it is possible to highlight surface or subsurface defects such as cracks, delaminations, or corrosion. One speaks then about active infrared thermography. In this study, some results obtained during the collective studies carried out by CETIM and the University of Reims for the forging industry are presented. Various experimental possibilities offered by active thermography are presented and the interest in this method in comparison with the traditional non-destructive testing methods (penetrant testing and magnetic particle inspection) is discussed. For example, comparative results on a forged cracked hub, a steering joint, and a threaded rod are presented. They highlight the interest of infrared thermography stimulated by induction for forged parts.

  19. Non-destructive analysis for the investigation of decomposition phenomena of historical manuscripts and prints

    NASA Astrophysics Data System (ADS)

    Faubel, Werner; Staub, Susanne; Simon, Rolf; Heissler, Stefan; Pataki, Andrea; Banik, Gerhard

    2007-07-01

    As a contribution to the increasing efforts to preserve cultural heritage, historical books as well as illuminated manuscripts endangered by corrosive writing and printing materials or destructive coloring matters, non-destructive analytical methods are highly desirable enabling an in-situ examination of the surface status of an object. The development and application of a novel combination of non-destructive analytic methods based on (a) synchrotron radiation induced micro-X-ray fluorescence (SR-μXRF) and (b) Fourier transform infrared (FTIR) microscope allows to investigate the state as well as the effectiveness of conservation procedures for historical manuscripts. Examples of measurements include (1) an iron gall ink manuscript of a historical memo on legal land description of the year 1769, (2) an original hand colored herbal of the years 1536/38 from the Senckenbergische Bibliothek, Frankfurt, and (3) the incunabula Johannes von Saaz: "Der Ackermann aus Boehmen" fated from 1463 and printed by Albrecht Pfister, Bamberg, owned by the Herzog August Bibliothek, Wolfenbuettel.

  20. Non-destructive 3D shape measurement of transparent and black objects with thermal fringes

    NASA Astrophysics Data System (ADS)

    Brahm, Anika; Rößler, Conrad; Dietrich, Patrick; Heist, Stefan; Kühmstedt, Peter; Notni, Gunther

    2016-05-01

    Fringe projection is a well-established optical method for the non-destructive contactless three-dimensional (3D) measurement of object surfaces. Typically, fringe sequences in the visible wavelength range (VIS) are projected onto the surfaces of objects to be measured and are observed by two cameras in a stereo vision setup. The reconstruction is done by finding corresponding pixels in both cameras followed by triangulation. Problems can occur if the properties of some materials disturb the measurements. If the objects are transparent, translucent, reflective, or strongly absorbing in the VIS range, the projected patterns cannot be recorded properly. To overcome these challenges, we present a new alternative approach in the infrared (IR) region of the electromagnetic spectrum. For this purpose, two long-wavelength infrared (LWIR) cameras (7.5 - 13 μm) are used to detect the emitted heat radiation from surfaces which is induced by a pattern projection unit driven by a CO2 laser (10.6 μm). Thus, materials like glass or black objects, e.g. carbon fiber materials, can be measured non-destructively without the need of any additional paintings. We will demonstrate the basic principles of this heat pattern approach and show two types of 3D systems based on a freeform mirror and a GOBO wheel (GOes Before Optics) projector unit.

  1. Design of an electron-accelerator-driven compact neutron source for non-destructive assay

    NASA Astrophysics Data System (ADS)

    Murata, A.; Ikeda, S.; Hayashizaki, N.

    2017-09-01

    The threat of nuclear and radiological terrorism remains one of the greatest challenges to international security, and the threat is constantly evolving. In order to prevent nuclear terrorism, it is important to avoid unlawful import of nuclear materials, such as uranium and plutonium. Development of technologies for non-destructive measurement, detection and recognition of nuclear materials is essential for control at national borders. At Tokyo Institute of Technology, a compact neutron source system driven by an electron-accelerator has been designed for non-destructive assay (NDA). This system is composed of a combination of an S-band (2.856 GHz) RF-gun, a tungsten target to produce photons by bremsstrahlung, a beryllium target, which is suitable for use in generating neutrons because of the low threshold energy of photonuclear reactions, and a moderator to thermalize the fast neutrons. The advantage of this system can accelerate a short pulse beam with a pulse width less than 1 μs which is difficult to produce by neutron generators. The amounts of photons and neutron produced by electron beams were simulated using the Monte Carlo simulation code PHITS 2.82. When the RF-gun is operated with an average electron beam current of 0.1 mA, it is expected that the neutron intensities are 1.19 × 109 n/s and 9.94 × 109 n/s for incident electron beam energies of 5 MeV and 10 MeV, respectively.

  2. A Distributive, Non-Destructive, Real-Time Approach to Snowpack Monitoring

    NASA Technical Reports Server (NTRS)

    Frolik, Jeff; Skalka, Christian

    2012-01-01

    This invention is designed to ascertain the snow water equivalence (SWE) of snowpacks with better spatial and temporal resolutions than present techniques. The approach is ground-based, as opposed to some techniques that are air-based. In addition, the approach is compact, non-destructive, and can be communicated with remotely, and thus can be deployed in areas not possible with current methods. Presently there are two principal ground-based techniques for obtaining SWE measurements. The first is manual snow core measurements of the snowpack. This approach is labor-intensive, destructive, and has poor temporal resolution. The second approach is to deploy a large (e.g., 3x3 m) snowpillow, which requires significant infrastructure, is potentially hazardous [uses a approximately equal to 200-gallon (approximately equal to 760-L) antifreeze-filled bladder], and requires deployment in a large, flat area. High deployment costs necessitate few installations, thus yielding poor spatial resolution of data. Both approaches have limited usefulness in complex and/or avalanche-prone terrains. This approach is compact, non-destructive to the snowpack, provides high temporal resolution data, and due to potential low cost, can be deployed with high spatial resolution. The invention consists of three primary components: a robust wireless network and computing platform designed for harsh climates, new SWE sensing strategies, and algorithms for smart sampling, data logging, and SWE computation.

  3. Non-Destructive Observations of Internal Micro-Defects Using Scanning Electron-Induced Acoustic Microscope

    NASA Astrophysics Data System (ADS)

    Koyama, Atsuhiro; Shibutani, Yoji

    Scanning electron-induced acoustic microscope (SEAM) has been developed as a new tool for non-destructive observations of the internal microstructures of materials. It consists of the electric chopper to pulse the high current electron beam and the detector of the longitudinal acoustic waves, both being attached to the commercial scanning electron microscope (SEM). The cyclic chopping of electron beam with extremely high frequency of a few hundred kilohertz makes the thermal wave due to the cyclic temperature rise with the short period. The wavelength of thermal wave may determine the essential SEAM resolution, because it's much smaller than the thermal stress wave (that is, the acoustic wave), which has just the role of conveying the information of thermal wave disturbance due to unexpected change as defects. Our own-built SEAM gives the best performance for observing the internal defects like the micro-voids, because it susceptibly senses the local difference of thermal properties in the sample. The paper indicates that some non-destructive observations for the micro-voids with a few microns order existing in the sintered materials are exhibited in conjunction with their destructive observations using focused-ion beam (FIB) technique to make certain of those as the proof.

  4. Are those bugs reflective? Non-destructive biofilm imaging with white light interferometry

    SciTech Connect

    Larimer, Curtis J.; Brann, Michelle R.; Suter, Jonathan D.; Bonheyo, George T.; Addleman, Raymond S.

    2016-08-28

    White light interferometry (WLI) is not typically used to image bacterial biofilms that are immersed in water because there is insufficient refractive index contrast to induce reflection from the biofilm’s interface. The soft structure and water-like bulk properties of hydrated biofilms make them difficult to characterize in situ by any means, especially in a non-destructive manner. Here we describe a new method for measuring and monitoring the thickness and topology of live biofilms using a WLI microscope. A microfluidic system was used to create a reflective interface on the surface of biofilms. Live biofilm samples were monitored non-destructively over time. The method enables surface metrology measurements (roughness, surface area) and a novel approach to measuring thickness of the thin hydrated biofilms. Increase in surface roughness preceded observable increase in biofilm thickness, indicating that this measure may be used to predict future development of biofilms. We have also developed a flow cell that enables WLI biofilm imaging in a dynamic environment. We have used this flow cell to observe changes in biofilm structure in response to changes in environmental conditions - flow velocity, availability of nutrients, and presence of biocides.

  5. Non-invasive and non-destructive measurements of confluence in cultured adherent cell lines

    PubMed Central

    Busschots, Steven; O’Toole, Sharon; O’Leary, John J.; Stordal, Britta

    2014-01-01

    Many protocols used for measuring the growth of adherent monolayer cells in vitro are invasive, destructive and do not allow for the continued, undisturbed growth of cells within flasks. Protocols often use indirect methods for measuring proliferation. Microscopy techniques can analyse cell proliferation in a non-invasive or non-destructive manner but often use expensive equipment and software algorithms. In this method images of cells within flasks are captured by photographing under a standard inverted phase contract light microscope using a digital camera with a camera lens adaptor. Images are analysed for confluence using ImageJ freeware resulting in a measure of confluence known as an Area Fraction (AF) output. An example of the AF method in use on OVCAR8 and UPN251 cell lines is included. • Measurements of confluence from growing adherent cell lines in cell culture flasks is obtained in a non-invasive, non-destructive, label-free manner. • The technique is quick, affordable and eliminates sample manipulation. • The technique provides an objective, consistent measure of when cells reach confluence and is highly correlated to manual counting with a haemocytometer. The average correlation co-efficient from a Spearman correlation (n = 3) was 0.99 ± 0.008 for OVCAR8 (p = 0.01) and 0.99 ± 0.01 for UPN251 (p = 0.01) cell lines. PMID:26150966

  6. Non-destructive staging of barley reproductive development for molecular analysis based upon external morphology.

    PubMed

    Gómez, José Fernández; Wilson, Zoe A

    2012-06-01

    A prerequisite to study the molecular genetic pathways of pollen and anther development is an accurate staging system for reproductive development. However in barley, floret formation occurs mainly within the pseudostem, which makes the observation of floret development and access to the floret particularly difficult without dissecting the plant. Thus selecting stages for molecular analysis cannot be done non-destructively. A staging method has therefore been developed for barley in order to define the relationship between readily detectable growth points and reproductive development, to provide a clear key to enable accurate selection of reproductive material. Initial staging followed the traditional Zadoks decimal system, with minor adaptations to stages 31-34 and stage 37. The later stages, from 37 onward, were replaced by growth staging based upon the last flag elongation (LFE) and the position occupied by the spike within the pseudostem. Spike size could be readily predicted by using the staging system incorporating Zadoks stages 31-37, supplemented with substages and by LFE staging to improve accuracy. The different spike sizes, as well as the LFE stages, showed a clear relationship to events occurring within the anther, as confirmed by light microscopy of the anthers. The defined relationship between spike size and development to anther development now makes possible the accurate prediction of anther and pollen progression by external staging. This, therefore, provides a mechanism for non-destructive selection of material for analysis that is critical for the molecular characterization of genes in anther and pollen development.

  7. Non-destructive measurement of soil liquefaction density change by crosshole radar tomography, Treasure Island, California

    USGS Publications Warehouse

    Kayen, Robert E.; Barnhardt, Walter A.; Ashford, Scott; Rollins, Kyle

    2000-01-01

    A ground penetrating radar (GPR) experiment at the Treasure Island Test Site [TILT] was performed to non-destructively image the soil column for changes in density prior to, and following, a liquefaction event. The intervening liquefaction was achieved by controlled blasting. A geotechnical borehole radar technique was used to acquire high-resolution 2-D radar velocity data. This method of non-destructive site characterization uses radar trans-illumination surveys through the soil column and tomographic data manipulation techniques to construct radar velocity tomograms, from which averaged void ratios can be derived at 0.25 - 0.5m pixel footprints. Tomograms of void ratio were constructed through the relation between soil porosity and dielectric constant. Both pre- and post-blast tomograms were collected and indicate that liquefaction related densification occurred at the site. Volumetric strains estimated from the tomograms correlate well with the observed settlement at the site. The 2-D imagery of void ratio can serve as high-resolution data layers for numerical site response analysis.

  8. Neural network and principal component regression in non-destructive soluble solids content assessment: a comparison.

    PubMed

    Chia, Kim-seng; Abdul Rahim, Herlina; Abdul Rahim, Ruzairi

    2012-02-01

    Visible and near infrared spectroscopy is a non-destructive, green, and rapid technology that can be utilized to estimate the components of interest without conditioning it, as compared with classical analytical methods. The objective of this paper is to compare the performance of artificial neural network (ANN) (a nonlinear model) and principal component regression (PCR) (a linear model) based on visible and shortwave near infrared (VIS-SWNIR) (400-1000 nm) spectra in the non-destructive soluble solids content measurement of an apple. First, we used multiplicative scattering correction to pre-process the spectral data. Second, PCR was applied to estimate the optimal number of input variables. Third, the input variables with an optimal amount were used as the inputs of both multiple linear regression and ANN models. The initial weights and the number of hidden neurons were adjusted to optimize the performance of ANN. Findings suggest that the predictive performance of ANN with two hidden neurons outperforms that of PCR.

  9. Processes for non-destructive transfer of graphene: widening the bottleneck for industrial scale production

    NASA Astrophysics Data System (ADS)

    Zaretski, Aliaksandr V.; Lipomi, Darren J.

    2015-05-01

    The exceptional charge-transport, mechanical, and barrier properties of graphene are well known. High-quality films of single-layer graphene produced over large areas, however, are extremely expensive. The high cost of graphene precludes its use in industries--such as transparent electrodes and flexible packaging--that might take full advantage of its properties. This minireview presents several strategies for the transfer of graphene from the substrates used for growth to substrates used for the final application. Each strategy shares the characteristic of being non-destructive: that is, the growth substrate remains reusable for further synthesis of new graphene. These processes have the potential to lower significantly the costs of manufacturing graphene, to increase production yields, and to minimize environmental impact. This article is divided into sections on (i) the synthesis of high-quality single-layer graphene and (ii) its non-destructive transfer to a host substrate. Section (ii) is further divided according to the substrate from which graphene is transferred: single-crystalline wafers or flexible copper foils. We also comment, wherever possible, on defects produced as a result of the transfer, and potential strategies to mitigate these defects. We conclude that several methods for the green synthesis and transfer of graphene have several of the right characteristics to be useful in industrial scale production.

  10. Non-destructive on-chip cell sorting system with real-time microscopic image processing.

    PubMed

    Takahashi, Kazunori; Hattori, Akihiro; Suzuki, Ikurou; Ichiki, Takanori; Yasuda, Kenji

    2004-06-03

    Studying cell functions for cellomics studies often requires the use of purified individual cells from mixtures of various kinds of cells. We have developed a new non-destructive on-chip cell sorting system for single cell based cultivation, by exploiting the advantage of microfluidics and electrostatic force. The system consists of the following two parts: a cell sorting chip made of poly-dimethylsiloxane (PDMS) on a 0.2-mm-thick glass slide, and an image analysis system with a phase-contrast/fluorescence microscope. The unique features of our system include (i) identification of a target from sample cells is achieved by comparison of the 0.2-microm-resolution phase-contrast and fluorescence images of cells in the microchannel every 1/30 s; (ii) non-destructive sorting of target cells in a laminar flow by application of electrostatic repulsion force for removing unrequited cells from the one laminar flow to the other; (iii) the use of agar gel for electrodes in order to minimize the effect on cells by electrochemical reactions of electrodes, and (iv) pre-filter, which was fabricated within the channel for removal of dust contained in a sample solution from tissue extracts. The sorting chip is capable of continuous operation and we have purified more than ten thousand cells for cultivation without damaging them. Our design has proved to be very efficient and suitable for the routine use in cell purification experiments.

  11. Compressive strength evaluation of structural lightweight concrete by non-destructive ultrasonic pulse velocity method.

    PubMed

    Bogas, J Alexandre; Gomes, M Glória; Gomes, Augusto

    2013-07-01

    In this paper the compressive strength of a wide range of structural lightweight aggregate concrete mixes is evaluated by the non-destructive ultrasonic pulse velocity method. This study involves about 84 different compositions tested between 3 and 180 days for compressive strengths ranging from about 30 to 80 MPa. The influence of several factors on the relation between the ultrasonic pulse velocity and compressive strength is examined. These factors include the cement type and content, amount of water, type of admixture, initial wetting conditions, type and volume of aggregate and the partial replacement of normal weight coarse and fine aggregates by lightweight aggregates. It is found that lightweight and normal weight concretes are affected differently by mix design parameters. In addition, the prediction of the concrete's compressive strength by means of the non-destructive ultrasonic pulse velocity test is studied. Based on the dependence of the ultrasonic pulse velocity on the density and elasticity of concrete, a simplified expression is proposed to estimate the compressive strength, regardless the type of concrete and its composition. More than 200 results for different types of aggregates and concrete compositions were analyzed and high correlation coefficients were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Variation in gymnemic acid content and non-destructive harvesting of Gymnema sylvestre (Gudmar).

    PubMed

    Pandey, Ashok Kumar; Yadav, Swati

    2010-09-01

    Madhunashini (Gymnema sylvestre R. Br.) commonly known as 'Gudmar' in Hindi is an important medicinal climber and extensively used in almost all Indian System of Medicine as a remedy for diabetes, rheumatism, cough, ulcer, jaundice, dyspepsia, constipation, eyes pain and also in snakebite. In India, it is found growing in Andhra Pradesh, Bihar, Chhattisgarh, Karnataka, Kerala, Madhya Pradesh, Maharastra, Orissa, Tamil Nadu, Uttar Pradesh and West Bengal. The major phytoconstituents are gymnemic acids, gudmarin and saponins. In the present study, Gymnema germplasm collected from various regions of Madhya Pradesh was evaluated on the basis of their morphological characteristics and gymnemic acid content. Gymnemic acid content in the leaves was estimated by HPLC. We have also standardized the non-destructive harvesting practices of Gudmar. Selective harvesting was done without harming the main plant. Only mature leaves (60%) were hand plucked in the month of October. Second harvest was done in the month of June. Data revealed that gymnemic acid content varied between 0.96% ± 0.03 (Seoni) to 1.58% ±0.03 (Amarkantak). It was also observed that the leaves left at the time of 1(st) harvest during October matured in June at the time of 2(nd) harvest. Non destructive harvesting practice did not have any negative impact on overall development of the plant. It is evident that there is wide variation in the morphological characteristics and gymnemic acid content in G. sylvestre collected from various locations, which can be exploited for further crop improvement programmes.

  13. Non-destructive inspection in industrial equipment using robotic mobile manipulation

    NASA Astrophysics Data System (ADS)

    Maurtua, Iñaki; Susperregi, Loreto; Ansuategui, Ander; Fernández, Ane; Ibarguren, Aitor; Molina, Jorge; Tubio, Carlos; Villasante, Cristobal; Felsch, Torsten; Pérez, Carmen; Rodriguez, Jorge R.; Ghrissi, Meftah

    2016-05-01

    MAINBOT project has developed service robots based applications to autonomously execute inspection tasks in extensive industrial plants in equipment that is arranged horizontally (using ground robots) or vertically (climbing robots). The industrial objective has been to provide a means to help measuring several physical parameters in multiple points by autonomous robots, able to navigate and climb structures, handling non-destructive testing sensors. MAINBOT has validated the solutions in two solar thermal plants (cylindrical-parabolic collectors and central tower), that are very demanding from mobile manipulation point of view mainly due to the extension (e.g. a thermal solar plant of 50Mw, with 400 hectares, 400.000 mirrors, 180 km of absorber tubes, 140m height tower), the variability of conditions (outdoor, day-night), safety requirements, etc. Once the technology was validated in simulation, the system was deployed in real setups and different validation tests carried out. In this paper two of the achievements related with the ground mobile inspection system are presented: (1) Autonomous navigation localization and planning algorithms to manage navigation in huge extensions and (2) Non-Destructive Inspection operations: thermography based detection algorithms to provide automatic inspection abilities to the robots.

  14. Non-destructive sampling of rock-dwelling microbial communities using sterile adhesive tape.

    PubMed

    Cutler, Nick A; Oliver, Anna E; Viles, Heather A; Whiteley, Andrew S

    2012-12-01

    Building stone provides a habitat for an array of microorganisms, many of which have been demonstrated to have a deleterious effect on the appearance and/or structural integrity of stone masonry. It is essential to understand the composition and structure of stone-dwelling (lithobiontic) microbial communities if successful stone conservation strategies are to be applied, particularly in the face of global environmental change. Ideally, the techniques used to sample such assemblages should be non-destructive due to the sensitive conservation status of many stone buildings. This paper quantitatively assesses the performance of sterile adhesive tape as a non-destructive sampling technique and compares the results of tape sampling with an alternative, destructive, sampling method. We used DNA fingerprinting (TRFLP) to characterise the algal, fungal and bacterial communities living on a stone slab. Our results demonstrate that tape sampling may be used to collect viable quantities of microbial DNA from environmental samples. This technique is ideally suited to the sampling of microbial biofilms, particularly when these communities are dominated by green algae. It provides a good approximation of total community diversity (i.e. the aggregate diversity of epilithic and endolithic communities). Tape sampling is straightforward, rapid and cost effective. When combined with molecular analytical techniques, this sampling method has the potential to make a major contribution to efforts to understand the structure of lithobiontic microbial communities and our ability to predict the response of such communities to future environmental change.

  15. Non-destructive high-throughput DNA extraction and genotyping methods for cotton seeds and seedlings.

    PubMed

    Zheng, Xiuting; Hoegenauer, Kevin A; Maeda, Andrea B V; Wang, Fei; Stelly, David M; Nichols, Robert L; Jones, Don C

    2015-05-01

    Extensive use of targeted PCR-based genotyping is precluded for many plant research laboratories by the cost and time required for DNA extraction. Using cotton (Gossypium hirsutum) as a model for plants with medium-sized seeds, we report here manual procedures for inexpensive non-destructive high-throughput extraction of DNA suitable for PCR-based genotyping of large numbers of individual seeds and seedlings. By sampling only small amounts of cotyledon tissue of ungerminated seed or young seedlings, damage is minimized, and viability is not discernibly affected. The yield of DNA from each seed or seedling is typically sufficient for 1000 or 500 PCR reactions, respectively. For seeds, the tissue sampling procedure relies on a modified 96-well plate that is used subsequently for seed storage. For seeds and seedlings, the DNA is extracted in a strongly basic DNA buffer that is later neutralized and diluted. Extracts can be used directly for high-throughput PCR-based genotyping. Any laboratory can thus extract DNA from thousands of individual seeds/seedlings per person-day at a very modest cost for consumables (~$0.05 per sample). Being non-destructive, our approach enables a wide variety of time- and resource-saving applications, such as marker-assisted selection (MAS), before planting, transplanting, and flowering.

  16. Non-destructive detection of pesticide residues in cucumber using visible/near-infrared spectroscopy.

    PubMed

    Jamshidi, Bahareh; Mohajerani, Ezeddin; Jamshidi, Jamshid; Minaei, Saeid; Sharifi, Ahmad

    2015-01-01

    The feasibility of using visible/near-infrared (Vis/NIR) spectroscopy was assessed for non-destructive detection of diazinon residues in intact cucumbers. Vis/NIR spectra of diazinon solution and cucumber samples without and with different concentrations of diazinon residue were analysed at the range of 450-1000 nm. Partial least squares-discriminant analysis (PLS-DA) models were developed based on different spectral pre-processing techniques to classify cucumbers with contents of diazinon below and above the MRL as safe and unsafe samples, respectively. The best model was obtained using a first-derivative method with the lowest standard error of cross-validation (SECV = 0.366). Moreover, total percentages of correctly classified samples in calibration and prediction sets were 97.5% and 92.31%, respectively. It was concluded that Vis/NIR spectroscopy could be an appropriate, fast and non-destructive technology for safety control of intact cucumbers by the absence/presence of diazinon residues.

  17. Non-invasive and non-destructive measurements of confluence in cultured adherent cell lines.

    PubMed

    Busschots, Steven; O'Toole, Sharon; O'Leary, John J; Stordal, Britta

    2015-01-01

    Many protocols used for measuring the growth of adherent monolayer cells in vitro are invasive, destructive and do not allow for the continued, undisturbed growth of cells within flasks. Protocols often use indirect methods for measuring proliferation. Microscopy techniques can analyse cell proliferation in a non-invasive or non-destructive manner but often use expensive equipment and software algorithms. In this method images of cells within flasks are captured by photographing under a standard inverted phase contract light microscope using a digital camera with a camera lens adaptor. Images are analysed for confluence using ImageJ freeware resulting in a measure of confluence known as an Area Fraction (AF) output. An example of the AF method in use on OVCAR8 and UPN251 cell lines is included. •Measurements of confluence from growing adherent cell lines in cell culture flasks is obtained in a non-invasive, non-destructive, label-free manner.•The technique is quick, affordable and eliminates sample manipulation.•The technique provides an objective, consistent measure of when cells reach confluence and is highly correlated to manual counting with a haemocytometer. The average correlation co-efficient from a Spearman correlation (n = 3) was 0.99 ± 0.008 for OVCAR8 (p = 0.01) and 0.99 ± 0.01 for UPN251 (p = 0.01) cell lines.

  18. Processes for non-destructive transfer of graphene: widening the bottleneck for industrial scale production.

    PubMed

    Zaretski, Aliaksandr V; Lipomi, Darren J

    2015-06-14

    The exceptional charge-transport, mechanical, and barrier properties of graphene are well known. High-quality films of single-layer graphene produced over large areas, however, are extremely expensive. The high cost of graphene precludes its use in industries-such as transparent electrodes and flexible packaging-that might take full advantage of its properties. This minireview presents several strategies for the transfer of graphene from the substrates used for growth to substrates used for the final application. Each strategy shares the characteristic of being non-destructive: that is, the growth substrate remains reusable for further synthesis of new graphene. These processes have the potential to lower significantly the costs of manufacturing graphene, to increase production yields, and to minimize environmental impact. This article is divided into sections on (i) the synthesis of high-quality single-layer graphene and (ii) its non-destructive transfer to a host substrate. Section (ii) is further divided according to the substrate from which graphene is transferred: single-crystalline wafers or flexible copper foils. We also comment, wherever possible, on defects produced as a result of the transfer, and potential strategies to mitigate these defects. We conclude that several methods for the green synthesis and transfer of graphene have several of the right characteristics to be useful in industrial scale production.

  19. A Spatially Offset Raman Spectroscopy Method for Non-Destructive Detection of Gelatin-Encapsulated Powders.

    PubMed

    Chao, Kuanglin; Dhakal, Sagar; Qin, Jianwei; Peng, Yankun; Schmidt, Walter F; Kim, Moon S; Chan, Diane E

    2017-03-18

    Non-destructive subsurface detection of encapsulated, coated, or seal-packaged foods and pharmaceuticals can help prevent distribution and consumption of counterfeit or hazardous products. This study used a Spatially Offset Raman Spectroscopy (SORS) method to detect and identify urea, ibuprofen, and acetaminophen powders contained within one or more (up to eight) layers of gelatin capsules to demonstrate subsurface chemical detection and identification. A 785-nm point-scan Raman spectroscopy system was used to acquire spatially offset Raman spectra for an offset range of 0 to 10 mm from the surfaces of 24 encapsulated samples, using a step size of 0.1 mm to obtain 101 spectral measurements per sample. As the offset distance was increased, the spectral contribution from the subsurface powder gradually outweighed that of the surface capsule layers, allowing for detection of the encapsulated powders. Containing mixed contributions from the powder and capsule, the SORS spectra for each sample were resolved into pure component spectra using self-modeling mixture analysis (SMA) and the corresponding components were identified using spectral information divergence values. As demonstrated here for detecting chemicals contained inside thick capsule layers, this SORS measurement technique coupled with SMA has the potential to be a reliable non-destructive method for subsurface inspection and authentication of foods, health supplements, and pharmaceutical products that are prepared or packaged with semi-transparent materials.

  20. Application of non-destructive techniques to assess the state of Hagia Sophia's mosaics

    NASA Astrophysics Data System (ADS)

    Moropoulou, Antonia; Karoglou, Maria; Labropoulos, Kyriakos C.; Delegou, Ekaterini T.; Katsiotis, Nikolaos K.; Karagiannis-Bakolas, Asterios

    2012-04-01

    The church of Hagia Sophia in Istanbul is a world heritage monument that epitomizes the byzantine ecclesiastic architecture. The church is decorated with mosaics from various historic periods. The preservation state of the mosaics is of high importance. In this study, non-destructive techniques (ground penetrating radar, infra-red thermography, fibreoptics microscopy) were employed on south upper gallery mosaic areas. The main aim of this on-site investigation was the evaluation of the preservation state of the mosaics and the previous interventions (materials characterization and decay diagnosis) in order to assess the performance of previous conservation/restoration interventions, as well as to verify the presence of mosaics in layers below the external plaster surfaces. Results indicated that is indeed possible to locate the grid of rendered mosaics. Regarding the preservation state of the mosaics, it was indicated that the main environmental decay factors were the high relative humidity levels with co-action of salt damp as well as the air pollutants. Moreover, it was revealed that previous incompatible restoration/conservation interventions have often accelerated the mosaics' degradation processes. Using non-destructive techniques it was possible to identify areas where the mosaic materials (tesserae and mortars) presented decay problems and in addition identify sub-layers that pose risk of detachment or decay intensification. In this way, NDT can contribute to the development of a strategic planning for mosaics conservation, protection and revealing.