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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. New magic angle bumps and magic translation bumps

    SciTech Connect

    Seeman, J.

    1983-10-28

    SLC beams of opposite charge can be transversely deflected in the same direction by RF fields in the accelerating cavities caused by girder tilts, coupler-asymmetries, or manufacturing errors. A symmetric deflection can be corrected by a magic angle bump if the deflection is located adjacent to one of the linac quadrupoles. However, if the deflection is located between quadrupoles, two magic angle bumps or a magic angle bump and a magic translation bump are needed for the correction. Several examples of translation bumps are included. A new magic angle bump is also presented which is longitudinally compressed and has significantly reduced particle excursions. Finally, if new correctors are added midway along the girders so that the number of correctors are doubled, then the longitudinal extent and the maximum particle excursion of these new magic bumps can be further reduced.

  3. 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

  4. MAGIC SHIMMING: gradient shimming with magic angle sample spinning.

    PubMed

    Nishiyama, Yusuke; Tsutsumi, Yu; Utsumi, Hiroaki

    2012-03-01

    A simple method to automatically shim NMR samples spinning at the magic angle is introduced based on the gradient shimming approach. The field inhomogeneity along the spinning axis is measured and automatically corrected. The combination of a normal magic angle spinning (MAS) probe, a conventional homospoil gradient, and a set of properly chosen standard room-temperature shims are used to perform the gradient shimming of samples spinning at the magic angle. The resulting (13)C NMR adamantane linewidth is less than 1 Hz (0.0078 ppm at 11.7 T). PMID:22370722

  5. MAGIC SHIMMING: Gradient shimming with magic angle sample spinning

    NASA Astrophysics Data System (ADS)

    Nishiyama, Yusuke; Tsutsumi, Yu; Utsumi, Hiroaki

    2012-03-01

    A simple method to automatically shim NMR samples spinning at the magic angle is introduced based on the gradient shimming approach. The field inhomogeneity along the spinning axis is measured and automatically corrected. The combination of a normal magic angle spinning (MAS) probe, a conventional homospoil gradient, and a set of properly chosen standard room-temperature shims are used to perform the gradient shimming of samples spinning at the magic angle. The resulting 13C NMR adamantane linewidth is less than 1 Hz (0.0078 ppm at 11.7 T).

  6. The magic angle: a solved mystery.

    PubMed

    Jouffrey, B; Schattschneider, P; Hébert, C

    2004-12-01

    We resolve the long-standing mysterious discrepancy between the experimental magic angle in EELS--approximately 2theta(E)--and the quantum mechanical prediction of approximately 4theta(E). A relativistic approach surpassing the usually applied kinematic correction yields a magic angle close to the experimental value. The reason is that the relativistic correction of the inelastic scattering cross section in anisotropic systems is significantly higher than in isotropic ones. PMID:15556701

  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. 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.

  9. Magic-angle-spinning NMR studies of zeolite SAPO-5

    NASA Astrophysics Data System (ADS)

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

    1988-01-01

    SAPO-5 was synthesized using triethylamine as template. Magic-angle-spinning (MAS) NMR of 1H, 27Al, 29Si and 31P was used to study the silicon incorporation into the framework and the nature of the Brønsted sites. 1H MAS NMR shows two types of bridging hydroxyl groups. 29Si MAS NMR indicates that silicon substitutes mostly for phosphorus and that there is a small amount of crystalline SiO 2 in the zeolite powder.

  10. 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.

  11. 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 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, {beta}{sub m} = Arccos(3{sup -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 {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

  12. Methods for magnetic resonance analysis using magic angle technique

    DOEpatents

    Hu, Jian Zhi; Wind, Robert A.; Minard, Kevin R.; Majors, Paul D.

    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.

  13. 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.

  14. Ultrashort TE T1ρ magic angle imaging.

    PubMed

    Du, Jiang; Statum, Sheronda; Znamirowski, Richard; Bydder, Graeme M; Chung, Christine B

    2013-03-01

    An ultrashort TE T(1)ρ sequence was used to measure T(1) ρ of the goat posterior cruciate ligament (n = 1) and human Achilles tendon specimens (n = 6) at a series of angles relative to the B(0) field and spin-lock field strengths to investigate the contribution of dipole-dipole interaction to T(1)ρ relaxation. Preliminary results showed a significant magic angle effect. T(1)ρ of the posterior cruciate ligament increased from 6.9 ± 1.3 ms at 0° to 36 ± 5 ms at 55° and then gradually reduced to 12 ± 3 ms at 90°. Mean T(1)ρ of the Achilles tendon increased from 5.5 ± 2.2 ms at 0° to 40 ± 5 ms at 55°. T(1)ρ dispersion study showed a significant T(1)ρ increase from 2.3 ± 0.9 ms to 11 ± 3 ms at 0° as the spin-lock field strength increased from 150 Hz to 1 kHz, and from 30 ± 3 ms to 42 ± 4 ms at 55° as the spin-lock field strength increased from 100 to 500 Hz. These results suggest that dipolar interaction is the dominant T(1)ρ relaxation mechanism in tendons and ligaments. PMID:22539354

  15. 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.

  16. 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. PMID:21862372

  17. 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.

  18. Solid effect in magic angle spinning dynamic nuclear polarization

    NASA Astrophysics Data System (ADS)

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

    2012-08-01

    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 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 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 to address the unfavorable field dependence of the solid effect.

  19. 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

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

    PubMed

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

    2012-08-01

    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 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. PMID:22894339

  1. 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.

  2. Direct determination of phosphate sugars in biological material by (1)H high-resolution magic-angle-spinning NMR spectroscopy.

    PubMed

    Diserens, Gaëlle; Vermathen, Martina; Gjuroski, Ilche; Eggimann, Sandra; Precht, Christina; Boesch, Chris; Vermathen, Peter

    2016-08-01

    The study aim was to unambiguously assign nucleotide sugars, mainly UDP-X that are known to be important in glycosylation processes as sugar donors, and glucose-phosphates that are important intermediate metabolites for storage and transfer of energy directly in spectra of intact cells, as well as in skeletal muscle biopsies by (1)H high-resolution magic-angle-spinning (HR-MAS) NMR. The results demonstrate that sugar phosphates can be determined quickly and non-destructively in cells and biopsies by HR-MAS, which may prove valuable considering the importance of phosphate sugars in cell metabolism for nucleic acid synthesis. As proof of principle, an example of phosphate-sugar reaction and degradation kinetics after unfreezing the sample is shown for a cardiac muscle, suggesting the possibility to follow by HR-MAS NMR some metabolic pathways. Graphical abstract Glucose-phosphate sugars (Glc-1P and Glc-6P) detected in muscle by 1H HR-MAS NMR. PMID:27271261

  3. 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

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

    NASA Astrophysics Data System (ADS)

    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 160 K. 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

  5. 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

  6. NON-DESTRUCTIVE BEAM MEASUREMENTS.

    SciTech Connect

    BAI,M.

    2004-07-05

    In high energy accelerators, especially storage rings, non-destructive beam measurements are highly desirable to minimize the impact on the beam quality. In principle, the non-destructive tools can be either passive detectors like Schottky, or active devices which excite either longitudinal or transverse beam motions for the corresponding measurements. An example of such a device is an ac dipole, a magnet with oscillating field, which can be used to achieve large coherent betatron oscillations. It has been demonstrated in the Brookhaven AGS that by adiabatically exciting the beam, the beam emittance growth due to the filamentation in the phase space can be avoided. This paper overviews both techniques in general. In particular, this paper also presents the beam tune measurement with a Schottky detector, phase advance measurements as well as nonlinear resonance measurements with the ac dipoles in the Brookhaven RHIC.

  7. 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.

  8. An efficient amplification pulse sequence for measuring chemical shift anisotropy under fast magic-angle spinning.

    PubMed

    Hung, Ivan; Gan, Zhehong

    2011-12-01

    A two-dimensional experiment for measuring chemical shift anisotropy (CSA) under fast magic-angle spinning (MAS) is presented. The chemical shift anisotropy evolution is amplified by a sequence of π-pulses that repetitively interrupt MAS averaging. The amplification generates spinning sideband manifolds in the indirect dimension separated by the isotropic shift along the direct dimension. The basic unit of the pulse sequence is designed based on the magic-angle turning experiment and can be concatenated for larger amplification factors. PMID:21962909

  9. Simple cylindrical magic-angle spinner for NMR studies in electromagnets

    NASA Astrophysics Data System (ADS)

    Mai, Michael T.; Ribeiro, Anthony; Jardetzky, Oleg

    A novel cylindrical magic-angle spinner for use in electromagnet systems is described. It features radial and thrust air bearings and easily constructed rotors of relatively large sample volume (˜0.7 cm 3) assembled into a removable spinner/coil Teflon housing. The design allows stable spinning speeds in the range 0.3 to 2.4 kHz with excellent rotor-to-rotor magic-angle resettabilities. High resolution, solid-state NMR studies are illustrated with 13C NMR spectra for crystalline adamantane and a macromolecule, lysozyme.

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

    NASA Astrophysics Data System (ADS)

    Krzywiecki, Maciej; Sarfraz, Adnan; Erbe, Andreas

    2015-12-01

    The application of a non-destructive method for characterization of electronic structure of an ultra-thin SnO1angle dependent XPS, we quantified stoichiometry changes inside the SnO1

  11. True Pathologic Abnormality versus Artifact Foot Position and Magic Angle Artifact in the Peroneal Tendons with 3T Imaging.

    PubMed

    Horn, Deena B; Meyers, Steven; Astor, William

    2015-09-01

    Magnetic resonance imaging is a commonly ordered examination by many foot and ankle surgeons for ankle pain and suspected peroneal tendon pathologic abnormalities. Magic angle artifact is one of the complexities associated with this imaging modality. Magic angle refers to the increased signal on magnetic resonance images associated with the highly organized collagen fibers in tendons and ligaments when they are orientated at a 55° angle to the main magnetic field. We present several examples from a clinical practice setting using 3T imaging illustrating a substantial reduction in magic angle artifact of the peroneal tendon in the prone plantarflexed position compared with the standard neutral (right angle) position. PMID:26429616

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

    DOEpatents

    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.

  13. 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.

  14. 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.

  15. 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

    2014-11-01

    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. PMID:25286333

  16. 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.

  17. 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.

  18. 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.

  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. 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.

  1. Excitation of multiple quantum transitions under magic angle spinning conditions: Adamantane

    NASA Astrophysics Data System (ADS)

    Meier, B. H.; Earl, William L.

    1986-11-01

    A pulse sequence designed for the excitation of multiple quantum transitions in magic angle spinning solid state NMR spectroscopy is presented. It is shown that under the action of the standard time-reversal pulse sequence, the change in the sign of the dipole coupling (which is used to generate the multiple quantum coherences) upon rotation causes the multiple quantum intensity to vanish after each rotor period. This effect is demonstrated both in calculations and in experimental 1H spectra of adamantane. A modification of the time-reversal pulse sequence, which involves switching the phase of the rf pulses every half-rotor period causes the spin part of the Hamiltonian to switch sign in synchrony with the modulation of the spacial part. This allows the creation of multiple quantum coherences in solids with magic angle spinning. The effectiveness of this pulse sequence is demonstrated through calculations and experiments.

  2. 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.

  3. Excitation of multiple quantum transitions under magic angle spinning conditions: Adamantane

    SciTech Connect

    Meier, B.H.; Earl, W.L.

    1986-11-01

    A pulse sequence designed for the excitation of multiple quantum transitions in magic angle spinning solid state NMR spectroscopy is presented. It is shown that under the action of the standard time-reversal pulse sequence, the change in the sign of the dipole coupling (which is used to generate the multiple quantum coherences) upon rotation causes the multiple quantum intensity to vanish after each rotor period. This effect is demonstrated both in calculations and in experimental /sup 1/H spectra of adamantane. A modification of the time-reversal pulse sequence, which involves switching the phase of the rf pulses every half-rotor period causes the spin part of the Hamiltonian to switch sign in synchrony with the modulation of the spacial part. This allows the creation of multiple quantum coherences in solids with magic angle spinning. The effectiveness of this pulse sequence is demonstrated through calculations and experiments.

  4. 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. PMID:25965280

  5. 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.

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

    NASA Astrophysics Data System (ADS)

    Hung, Ivan; Gan, Zhehong

    2015-07-01

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

  7. Solid-state proton multiple-quantum NMR spectroscopy with fast magic angle spinning

    NASA Astrophysics Data System (ADS)

    Geen, Helen; Titman, Jeremy J.; Gottwald, Johannes; Spiess, Hans W.

    1994-09-01

    The feasibility of multiple-quantum NMR spectroscopy with high resolution for protons in solids is explored. A new multiple-quantum excitation sequence suitable for use with fast magic angle spinning is described, and its performance is compared to that of both static and slow-spinning multiple-quantum methods. Modified sequences with scale the rate of development of the multiple-quantum coherences are also demonstrated, and two-dimensional double-quantum spectra of adamantane and polycarbonate are presented.

  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. PMID:22936994

  9. 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. PMID:19246221

  10. 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

  11. 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.

  12. 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

  13. 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. PMID:27192290

  14. Tethered or adsorbed supported lipid bilayers in nanotubes characterized by deuterium magic angle spinning NMR spectroscopy.

    PubMed

    Wattraint, Olivier; Warschawski, Dror E; Sarazin, Catherine

    2005-04-12

    2H solid-state NMR experiments were performed under magic angle spinning on lipid bilayers oriented into nanotubes arrays, as a new method to assess the geometrical arrangement of the lipids. Orientational information is obtained from the intensities of the spinning sidebands. The lipid bilayers are formed by fusion of small unilamellar vesicles of DMPC-d54 inside a nanoporous anodic aluminum oxide, either by direct adsorption on the support or by tethering through a streptavidin/biotin linker. The results support that the quality of the lipid bilayers alignment is clearly in favor of the tethering rather than an adsorbed strategy. PMID:15807556

  15. On the magic-angle turning and phase-adjusted spinning sidebands experiments.

    PubMed

    Hung, Ivan; Gan, Zhehong

    2010-05-01

    The underlying relation between the magic-angle turning (MAT) and phase-adjusted spinning sidebands (PASS) experiments is examined. The MAT experiment satisfies the PASS conditions for separating spinning sidebands with a non-constant total evolution time and only requires linear t(1) increments of up to one rotor period. The time-domain data of the two experiments are related by a shearing transformation. A combination of the linear evolution-time increments of MAT and simple data processing of PASS are particularly attractive for the implementation of MAT for measuring chemical shift anisotropy. PMID:20202873

  16. High-resolution magic-angle-spinning NMR spectroscopy of intact tissue.

    PubMed

    Giskeødegård, Guro F; Cao, Maria D; Bathen, Tone F

    2015-01-01

    High-resolution magic-angle-spinning (HR-MAS) NMR spectroscopy is a nondestructive technique that is used to obtain the metabolite profile of a tissue sample. This method requires minimal sample preparation. However, it is important to handle the sample with care and keep it frozen during preparation to minimize degradation. Here, we describe a typical protocol for HR-MAS analysis of intact tissue. We also include examples of typical pulse sequence programs and quantification methods that are used today. PMID:25677145

  17. 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.

  18. 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.

  19. 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.

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

    DOEpatents

    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.

  1. 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. PMID:26920834

  2. Measurement of nuclear magnetic dipole—dipole couplings in magic angle spinning NMR

    NASA Astrophysics Data System (ADS)

    Tycko, Robert; Dabbagh, Gary

    1990-10-01

    We describe a method for measuring nuclear magnetic dipole—dipole couplings in NMR spectra of solids undergoing rapid magic angle spinning (MAS). We show in theory, simulations, and experiments that the couplings, which are averaged out by MAS alone, can be recovered by applying simple resonant radiofrequency pulse sequences in synchrony with the sample rotation. Experimental 13C dipolar powder pattern spectra of polycrystalline ( 13CH 3) 2C(OH)SO 3Na obtained in a two-dimensional experiment based on this method are presented. The method provides a means of determining internuclear distances in polycrystalline and noncrystalline solids while retaining the high resolution and sensitivity afforded by MAS.

  3. 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

  4. 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. PMID:22750637

  5. 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. PMID:26920838

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

    DOE PAGESBeta

    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

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

    NASA Astrophysics Data System (ADS)

    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.

  8. 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.

  9. 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.

  10. High Resolution 1H NMR Spectroscopy in Rat Liver Using Magic Angle Turning at a 1 Hz Spinning Rate

    SciTech Connect

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

    2001-12-01

    It is demonstrated that a high resolution 1H NMR spectrum of excised rat liver can be obtained using the technique of magic angle turning at a sample spinning rate of 1 Hz. A variant of the phase-corrected magic angle turning (PHORMAT) pulse sequence that includes a water suppression segment was developed for the investigation. The spectral resolution achieved with PHORMAT is approaching that obtained from a standard magic angle spinning experiment at a spinning rate of several kHz. With such ultra-slow spinning, tissue and cell damage associated with the standard MAS experiment is minimized or eliminated. The technique is potentially useful for obtaining high-resolution 1H spectra in live animals.

  11. 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.

  12. Primary processes in isolated Photosystem II reaction centres probed by magic angle transient absorption spectroscopy

    NASA Astrophysics Data System (ADS)

    Klug, David R.; Rech, Thomas; Melissa Joseph, D.; Barber, James; Durrant, James R.; Porter, George

    1995-05-01

    There is currently some disagreement regarding the dominant time constant for formation of the radical pair state P680 +Ph - in isolated photosystem two reaction centres. It has recently been suggested that this disagreement may originate, at least in part, from different polarisations of the pump and probe beams used in optical experiments. In this paper, we present data collected using a magic angle configuration of the pump and probe polarisations. We find that these data support our previous interpretation of data collected using a parallel polarisation configuration. Moreover, we present further evidence to support our conclusion that formation of the P680 +Ph - state primarily occurs with a 21 ps time constant when P680 is directly excited. A 3 ps component is also observed; this component is not associated with a large proportion of the radical pair formation. We discuss our data and interpretation in comparison with those of other groups.

  13. 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

    2014-09-01

    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. PMID:25102442

  14. 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. PMID:25797007

  15. 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.

  16. 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 .

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

    NASA Astrophysics Data System (ADS)

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

    2015-06-01

    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.

  18. 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.

  19. Magic angle spinning solid-state NMR experiments for structural characterization of proteins.

    PubMed

    Shi, Lichi; Ladizhansky, Vladimir

    2012-01-01

    Solid-state nuclear magnetic resonance (SSNMR) has become a prominent method in biology and is suitable for the characterization of insoluble proteins and protein aggregates such as amyloid fibrils, membrane-lipid complexes, and precipitated proteins. Often, the initial and the most critical step is to obtain spectroscopic assignments, that is, to determine chemical shifts of individual atoms. The procedures for SSNMR spectroscopic assignments are now well established for small microcrystalline proteins, where high signal-to-noise can be obtained. The sensitivity of the experiments and spectral resolution decrease with the increasing molecular weight, which makes setting SSNMR experiments in large proteins a much more challenging and demanding procedure. Here, we describe the protocol for the most common set of 3D magic angle spinning (MAS) SSNMR experiments. While the procedures described in the text are well known to SSNMR practitioners, we hope they will be of interest to scientists interested in extending their repertoire of biophysical techniques. PMID:22760319

  20. Forensic examination of electrical tapes using high resolution magic angle spinning ¹H NMR spectroscopy.

    PubMed

    Schoenberger, Torsten; Simmross, Ulrich; Poppe, Christian

    2016-01-01

    The application of high resolution magic angle spinning (HR-MAS) (1)H NMR spectroscopy is ideally suited for the differentiation of plastics. In addition to the actual material composition, the different types of polymer architectures and tacticity provide characteristic signals in the fingerprint of the (1)H NMR spectra. The method facilitates forensic comparison, as even small amounts of insoluble but swellable plastic particles are utilized. The performance of HR-MAS NMR can be verified against other methods that were recently addressed in various articles about forensic tape comparison. In this study samples of the 90 electrical tapes already referenced by the FBI laboratory were used. The discrimination power of HR-MAS is demonstrated by the fact that more tape groups can be distinguished by NMR spectroscopy than by using the combined evaluation of several commonly used analytical techniques. An additional advantage of this robust and quick method is the very simple sample preparation. PMID:26558760

  1. 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.

  2. 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. PMID:27314744

  3. Pulsed field gradient magic angle spinning NMR self-diffusion measurements in liquids.

    PubMed

    Viel, Stéphane; Ziarelli, Fabio; Pagès, Guilhem; Carrara, Caroline; Caldarelli, Stefano

    2008-01-01

    Several investigations have recently reported the combined use of pulsed field gradient (PFG) with magic angle spinning (MAS) for the analysis of molecular mobility in heterogeneous materials. In contrast, little attention has been devoted so far to delimiting the role of the extra force field induced by sample rotation on the significance and reliability of self-diffusivity measurements. The main purpose of this work is to examine this phenomenon by focusing on pure liquids for which its impact is expected to be largest. Specifically, we show that self-diffusion coefficients can be accurately determined by PFG MAS NMR diffusion measurements in liquids, provided that specific experimental conditions are met. First, the methodology to estimate the gradient uniformity and to properly calibrate its absolute strength is briefly reviewed and applied on a MAS probe equipped with a gradient coil aligned along the rotor spinning axis, the so-called 'magic angle gradient' coil. Second, the influence of MAS on the outcome of PFG MAS diffusion measurements in liquids is investigated for two distinct typical rotors of different active volumes, 12 and 50 microL. While the latter rotor led to totally unreliable results, especially for low viscosity compounds, the former allowed for the determination of accurate self-diffusion coefficients both for fast and slowly diffusing species. Potential implications of this work are the possibility to measure accurate self-diffusion coefficients of sample-limited mixtures or to avoid radiation damping interferences in NMR diffusion measurements. Overall, the outlined methodology should be of interest to anyone who strives to improve the reliability of MAS diffusion studies, both in homogeneous and heterogeneous media. PMID:18006344

  4. Method for non-destructive testing

    DOEpatents

    Akers, Douglas W.

    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.

  5. 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

  6. 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. PMID:11097812

  7. 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.

  8. 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

  9. 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

  10. 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. PMID:27306000

  11. High-resolution magic angle spinning 1H MRS in prostate cancer.

    PubMed

    Decelle, Emily A; Cheng, Leo L

    2014-01-01

    Prostate cancer (PCa) is the most frequently diagnosed malignancy in men worldwide, largely as a result of the increased use of the annual serum prostate-specific antigen (PSA) screening test for detection. PSA screening has saved lives, but it has also resulted in the overtreatment of many patients with PCa because of a limited ability to accurately localize and characterize PCa lesions through imaging. High-resolution magic angle spinning (HRMAS) (1)H MRS has proven to be a strong potential clinical tool for PCa diagnosis and prognosis. The HRMAS technique allows valuable metabolic information to be obtained from ex vivo intact tissue samples and also enables the performance of histopathology on the same tissue specimens. Studies have found that the quantification of individual metabolite levels and metabolite ratios, as well as metabolomic profiles, shows strong potential to improve accuracy in PCa detection, diagnosis and monitoring. Ex vivo HRMAS is also a valuable tool for the interpretation of in vivo results, including the localization of tumors, and thus has the potential to improve in vivo diagnostic tests used in the clinic. Here, we primarily review publications of HRMAS (1)H MRS and its use for the study of intact human prostate tissue. PMID:23529951

  12. 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.

  13. 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.

  14. Magnetization transfer magic-angle-spinning z-spectroscopy of excised tissues

    NASA Astrophysics Data System (ADS)

    Avni, Reut; Mangoubi, Oren; Bhattacharyya, Rangeet; Degani, Hadassa; Frydman, Lucio

    2009-07-01

    NMR experiments devised to aid in analyses of tissues include magnetization transfer (MT), which can highlight the signals of biological macromolecules through cross-relaxation and/or chemical exchange processes with the bulk 1H water resonance, and high-resolution magic-angle-spinning (HRMAS) methods, akin to those used in solid-state NMR to introduce additional spectral resolution via the averaging of spin anisotropies. This paper explores the result of combining these methodologies, and reports on MT "z-spectroscopy" between water and cell components in excised tissues under a variety of HRMAS conditions. Main features arising from the resulting 1H "MTMAS" experiments include strong spinning sideband manifolds centered at the liquid water shift, high-resolution isotropic features coinciding with aliphatic and amide proton resonances, and a second sideband manifold arising as spinning speeds are increased. Interpretations are given for the origin of these various features, including simulations shedding further light onto the nature of MT NMR signals observed for tissue samples. Concurrently, histological examinations are reported validating the limits of HRMAS NMR procedures to the analysis of tissue samples preserved in a number of different ways.

  15. 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.

  16. 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. PMID:27489348

  17. A LOW-E MAGIC ANGLE SPINNING PROBE FOR BIOLOGICAL SOLID STATE NMR AT 750 MHz

    PubMed Central

    McNeill, Seth A.; Gor’kov, Peter L.; Shetty, Kiran; Brey, William W.; Long, Joanna R.

    2009-01-01

    Crossed-coil NMR probes are a useful tool for reducing sample heating for biological solid state NMR. In a crossed-coil probe, the higher frequency 1H field, which is the primary source of sample heating in conventional probes, is produced by a separate low-inductance resonator. Because a smaller driving voltage is required, the electric field across the sample and the resultant heating is reduced. In this work we describe the development of a magic angle spinning (MAS) solid state NMR probe utilizing a dual resonator. This dual resonator approach, referred to as “Low-E,” was originally developed to reduce heating in samples of mechanically aligned membranes. The study of inherently dilute systems, such as proteins in lipid bilayers, via MAS techniques requires large sample volumes at high field to obtain spectra with adequate signal-to-noise ratio under physiologically relevant conditions. With the Low-E approach, we are able to obtain homogeneous and sufficiently strong radiofrequency fields for both 1H and 13C frequencies in a 4 mm probe with a 1H frequency of 750 MHz. The performance of the probe using windowless dipolar recoupling sequences is demonstrated on model compounds as well as membrane embedded peptides. PMID:19138870

  18. Alignment of high resolution magic angle spinning magnetic resonance spectra using warping methods.

    PubMed

    Giskeødegård, Guro F; Bloemberg, Tom G; Postma, Geert; Sitter, Beathe; Tessem, May-Britt; Gribbestad, Ingrid S; Bathen, Tone F; Buydens, Lutgarde M C

    2010-12-17

    The peaks of magnetic resonance (MR) spectra can be shifted due to variations in physiological and experimental conditions, and correcting for misaligned peaks is an important part of data processing prior to multivariate analysis. In this paper, five warping algorithms (icoshift, COW, fastpa, VPdtw and PTW) are compared for their feasibility in aligning spectral peaks in three sets of high resolution magic angle spinning (HR-MAS) MR spectra with different degrees of misalignments, and their merits are discussed. In addition, extraction of information that might be present in the shifts is examined, both for simulated data and the real MR spectra. The generic evaluation methodology employs a number of frequently used quality criteria for evaluation of the alignments, together with PLS-DA to assess the influence of alignment on the classification outcome. Peak alignment greatly improved the internal similarity of the data sets. Especially icoshift and COW seem suitable for aligning HR-MAS MR spectra, possibly because they perform alignment segment-wise. The choice of reference spectrum can influence the alignment result, and it is advisable to test several references. Information from the peak shifts was extracted, and in one case cancer samples were successfully discriminated from normal tissue based on shift information only. Based on these findings, general recommendations for alignment of HR-MAS MRS data are presented. Where possible, observations are generalized to other data types (e.g. chromatographic data). PMID:21094376

  19. Frequency-stepped acquisition in nuclear magnetic resonance spectroscopy under magic angle spinning

    NASA Astrophysics Data System (ADS)

    Pell, Andrew J.; Clément, Raphaële J.; Grey, Clare P.; Emsley, Lyndon; Pintacuda, Guido

    2013-03-01

    The nuclear magnetic resonance of paramagnetic solids is usually characterized by the presence of large chemical shifts and shift anisotropies due to hyperfine interactions. Frequently the resulting spectra cover a frequency range of several megahertz, which is greater than the bandwidth of commercially available radio-frequency (RF) probes, making it impossible to acquire the whole spectrum in a single experiment. In these cases it common to record a series of spectra, in which the probe is tuned to a different frequency for each, and then sum the results to give the "true" spectrum. While this method is very widely used on static samples, the application of frequency stepping under magic-angle spinning (MAS) is less common, owing to the increased complexity of the spin dynamics when describing the interplay of the RF irradiation with the mechanical rotation of the shift tensor. In this paper, we present a theoretical description, based on the jolting frame formalism of Caravatti et al. [J. Magn. Reson. 55, 88 (1983), 10.1016/0022-2364(83)90279-2], for describing the spin dynamics of a powder sample under MAS when subjected to a selective pulse of low RF-field amplitude. The formalism is used to describe the frequency stepping method under MAS, and under what circumstances the true spectrum is reproduced. We also present an experimental validation of the methodology under ultra-fast MAS with the paramagnetic materials LiMnPO4 and TbCsDPA.

  20. Deuterium magic angle spinning studies of substrates bound to cytochrome P450.

    PubMed

    Lee, H; Ortiz de Montellano, P R; McDermott, A E

    1999-08-17

    We report solid-state deuterium magic angle spinning NMR spectra of perdeuterated adamantane bound to the active site of microcrystalline cytochrome P450cam (CP450cam) in its resting state. CP450cam contains a high-spin ferric (Fe3+) heme in the resting state; the isotropic shift was displaced from the diamagnetic value and varied with temperature consistent with Curie-law dependence. A nondeuterated competitive tighter binding ligand, camphor, was used to displace the adamantane-bound species. This addition resulted in the disappearance of the hyperfine-shifted signal associated with a perdeuterated adamantane bound to CP450cam, while signals presumably associated with adamantane bound to other cavities persisted. We simulated the deuterium spinning side-band intensities for the enzyme-bound species using dipolar hyperfine coupling as the only anisotropic interaction; the deuterium quadrupolar interaction was apparently averaged due to a fast high-symmetry motion. These data provide direct support for previous proposals that substrates are conformationally mobile on the time scale of enzymatic turnover. The simulations suggested that the adamantane binds with an average metal-deuterium distance of 6.2 (+/-0.2) A, corresponding to a dipolar coupling constant of 6.5 (+/-0.5) kHz. PMID:10451377

  1. Molecular dynamics in paramagnetic materials as studied by magic-angle spinning 2H NMR spectra.

    PubMed

    Mizuno, Motohiro; Suzuki, You; Endo, Kazunaka; Murakami, Miwa; Tansho, Masataka; Shimizu, Tadashi

    2007-12-20

    A magic-angle spinning (MAS) 2H NMR experiment was applied to study the molecular motion in paramagnetic compounds. The temperature dependences of 2H MAS NMR spectra were measured for paramagnetic [M(H2O)6][SiF6] (M=Ni2+, Mn2+, Co2+) and diamagnetic [Zn(H2O)6][SiF6]. The paramagnetic compounds exhibited an asymmetric line shape in 2H MAS NMR spectra because of the electron-nuclear dipolar coupling. The drastic changes in the shape of spinning sideband patterns and in the line width of spinning sidebands due to the 180 degrees flip of water molecules and the reorientation of [M(H2O)6]2+ about its C3 axis were observed. In the paramagnetic compounds, paramagnetic spin-spin relaxation and anisotropic g-factor result in additional linebroadening of each of the spinning sidebands. The spectral simulation of MAS 2H NMR, including the effects of paramagnetic shift and anisotropic spin-spin relaxation due to electron-nuclear dipolar coupling and anisotropic g-factor, was performed for several molecular motions. Information about molecular motions in the dynamic range of 10(2) s(-1)

  2. High-resolution magic-angle spinning (13)C spectroscopy of brain tissue at natural abundance.

    PubMed

    Yang, Yongxia; Chen, Lei; Gao, Hongchang; Zeng, Danlin; Yue, Yong; Liu, Maili; Lei, Hao; Deng, Feng; Ye, Chaohui

    2006-03-01

    High-resolution magic-angle spinning (MAS) (1)H and (13)C magnetic resonance spectroscopy (MRS) has recently been applied to study the metabolism in intact biological tissue samples. Because of the low natural abundance and the low gyromagnetic ratio of the (13)C nuclei, signal enhancement techniques such as cross-polarization (CP) and distortionless enhancement by polarization transfer (DEPT) are often employed in MAS (13)C MRS to improve the detection sensitivity. In this study, several sensitivity enhancement techniques commonly used in liquid- and solid-state NMR, including CP, DEPT and nuclear Overhauser enhancement (NOE), were combined with MAS to acquire high-resolution (13)C spectra on intact rat brain tissue at natural abundance, and were compared for their performances. The results showed that different signal enhancement techniques are sensitive to different classes of molecules/metabolites, depending on their molecular weights and mobility. DEPT was found to enhance the signals of low-molecular weight metabolites exclusively, while the signals of lipids, which often are associated with membranes and have relatively lower mobility, were highly sensitive to CP enhancement. PMID:16477685

  3. 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. PMID:27035630

  4. Structure of a protein determined by solid-state magic-angle-spinning NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Castellani, Federica; van Rossum, Barth; Diehl, Annette; Schubert, Mario; Rehbein, Kristina; Oschkinat, Hartmut

    2002-11-01

    The determination of a representative set of protein structures is a chief aim in structural genomics. Solid-state NMR may have a crucial role in structural investigations of those proteins that do not easily form crystals or are not accessible to solution NMR, such as amyloid systems or membrane proteins. Here we present a protein structure determined by solid-state magic-angle-spinning (MAS) NMR. Almost complete 13C and 15N resonance assignments for a micro-crystalline preparation of the α-spectrin Src-homology 3 (SH3) domain formed the basis for the extraction of a set of distance restraints. These restraints were derived from proton-driven spin diffusion (PDSD) spectra of biosynthetically site-directed, labelled samples obtained from bacteria grown using [1,3-13C]glycerol or [2-13C]glycerol as carbon sources. This allowed the observation of long-range distance correlations up to ~7Å. The calculated global fold of the α-spectrin SH3 domain is based on 286 inter-residue 13C-13C and six 15N-15N restraints, all self-consistently obtained by solid-state MAS NMR. This MAS NMR procedure should be widely applicable to small membrane proteins that can be expressed in bacteria.

  5. 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

  6. 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.

  7. Rotary resonance recoupling of 13C- 1H dipolar interactions in magic angle spinning 13C NMR of dynamic solids

    NASA Astrophysics Data System (ADS)

    Kitchin, Simon J.; Harris, Kenneth D. M.; Aliev, Abil E.; Apperley, David C.

    2000-06-01

    Rotary resonance recoupling of heteronuclear 13C- 1H dipolar interactions in magic angle spinning solid state 13C NMR spectra (recorded under conditions of 1H decoupling at frequency ν1 and magic angle spinning at frequency νr) has been studied for three examples of molecular solids (adamantane, ferrocene and hexamethylbenzene) in which substantial molecular motion is known to occur. It is shown that when rotary resonance conditions are satisfied (i.e. ν1/νr= n, for n=1 or 2), the recoupling can lead to motionally averaged Pake-like powder patterns from which information on 13C- 1H internuclear distances and/or molecular motion can be derived.

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

    NASA Astrophysics Data System (ADS)

    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 (˜12K) 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). H1 MAS NMR with the coil temperature of ˜20K was successfully observed for solid adamantane rotating at room temperature, and signal-to-noise increment due to this cryocoil approach was confirmed.

  9. High resolution structural characterization of Aβ42 amyloid fibrils by magic angle spinning NMR.

    PubMed

    Colvin, Michael T; Silvers, Robert; Frohm, Birgitta; Su, Yongchao; Linse, Sara; Griffin, Robert G

    2015-06-17

    The presence of amyloid plaques composed of amyloid beta (Aβ) fibrils is a hallmark of Alzheimer's disease (AD). The Aβ peptide is present as several length variants with two common alloforms consisting of 40 and 42 amino acids, denoted Aβ1-40 and Aβ1-42, respectively. While there have been numerous reports that structurally characterize fibrils of Aβ1-40, very little is known about the structure of amyloid fibrils of Aβ1-42, which are considered the more toxic alloform involved in AD. We have prepared isotopically (13)C/(15)N labeled AβM01-42 fibrils in vitro from recombinant protein and examined their (13)C-(13)C and (13)C-(15)N magic angle spinning (MAS) NMR spectra. In contrast to several other studies of Aβ fibrils, we observe spectra with excellent resolution and a single set of chemical shifts, suggesting the presence of a single fibril morphology. We report the initial structural characterization of AβM01-42 fibrils utilizing (13)C and (15)N shift assignments of 38 of the 43 residues, including the backbone and side chains, obtained through a series of cross-polarization based 2D and 3D (13)C-(13)C, (13)C-(15)N MAS NMR experiments for rigid residues along with J-based 2D TOBSY experiments for dynamic residues. We find that the first ∼5 residues are dynamic and most efficiently detected in a J-based TOBSY spectrum. In contrast, residues 16-42 are easily observed in cross-polarization experiments and most likely form the amyloid core. Calculation of ψ and φ dihedral angles from the chemical shift assignments indicate that 4 β-strands are present in the fibril's secondary structure. PMID:26001057

  10. High Resolution Structural Characterization of Aβ42 Amyloid Fibrils by Magic Angle Spinning NMR

    PubMed Central

    2015-01-01

    The presence of amyloid plaques composed of amyloid beta (Aβ) fibrils is a hallmark of Alzheimer’s disease (AD). The Aβ peptide is present as several length variants with two common alloforms consisting of 40 and 42 amino acids, denoted Aβ1–40 and Aβ1–42, respectively. While there have been numerous reports that structurally characterize fibrils of Aβ1–40, very little is known about the structure of amyloid fibrils of Aβ1–42, which are considered the more toxic alloform involved in AD. We have prepared isotopically 13C/15N labeled AβM01–42 fibrils in vitro from recombinant protein and examined their 13C–13C and 13C–15N magic angle spinning (MAS) NMR spectra. In contrast to several other studies of Aβ fibrils, we observe spectra with excellent resolution and a single set of chemical shifts, suggesting the presence of a single fibril morphology. We report the initial structural characterization of AβM01–42 fibrils utilizing 13C and 15N shift assignments of 38 of the 43 residues, including the backbone and side chains, obtained through a series of cross-polarization based 2D and 3D 13C–13C, 13C–15N MAS NMR experiments for rigid residues along with J-based 2D TOBSY experiments for dynamic residues. We find that the first ∼5 residues are dynamic and most efficiently detected in a J-based TOBSY spectrum. In contrast, residues 16–42 are easily observed in cross-polarization experiments and most likely form the amyloid core. Calculation of ψ and φ dihedral angles from the chemical shift assignments indicate that 4 β-strands are present in the fibril’s secondary structure. PMID:26001057

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. Tailored low-power cross-polarization under fast magic-angle spinning

    NASA Astrophysics Data System (ADS)

    Demers, Jean-Philippe; Vijayan, Vinesh; Becker, Stefan; Lange, Adam

    2010-08-01

    High static magnetic fields and very fast magic-angle spinning (MAS) promise to improve resolution and sensitivity of solid-state NMR experiments. The fast MAS regime has permitted the development of low-power cross-polarization schemes, such as second-order cross-polarization (SOCP), which prevent heat deposition in the sample. Those schemes are however limited in bandwidth, as weak radio-frequency (RF) fields only cover a small chemical shift range for rare nuclei (e.g. 13C). Another consideration is that the efficiency of cross-polarization is very sensitive to magnetization decay that occurs during the spin-lock pulse on the abundant nuclei (e.g. 1H). Having characterized this decay in glutamine at 60 kHz MAS, we propose two complementary strategies to tailor cross-polarization to desired spectral regions at low RF power. In the case of multiple sites with small chemical shift dispersion, a larger bandwidth for SOCP is obtained by slightly increasing the RF power while avoiding recoupling conditions that lead to fast spin-lock decay. In the case of two spectral regions with large chemical shift offset, an extension of the existing low-power schemes, called MOD-CP, is introduced. It consists of a spin-lock on 1H and an amplitude-modulated spin-lock on the rare nucleus. The range of excited chemical shifts is assessed by experimental excitation profiles and numerical simulation of an I 2S spin system. All SOCP-based schemes exhibit higher sensitivity than high-power CP schemes, as demonstrated on solid (glutamine) and semi-solid (hydrated, micro-crystalline ubiquitin) samples.

  16. Correlating high-resolution magic angle spinning NMR spectroscopy and gene analysis in osteoarthritic cartilage.

    PubMed

    Tufts, Lauren; Shet Vishnudas, Keerthi; Fu, Eunice; Kurhanewicz, John; Ries, Michael; Alliston, Tamara; Li, Xiaojuan

    2015-05-01

    Osteoarthritis (OA) is a common multifactorial and heterogeneous degenerative joint disease, and biochemical changes in cartilage matrix occur during the early stages of OA before morphological changes occur. Thus, it is desired to measure regional biochemical changes in the joint. High-resolution magic angle spinning (HRMAS) NMR spectroscopy is a powerful method of observing cartilaginous biochemical changes ex vivo, including the concentrations of alanine and N-acetyl, which are markers of collagen and total proteoglycan content, respectively. Previous studies have observed significant changes in chondrocyte metabolism of OA cartilage via the altered gene expression profiles of ACAN, COL2A1 and MMP13, which encode aggrecan, type II collagen and matrix metalloproteinase 13 (a protein crucial in the degradation of type II collagen), respectively. Employing HRMAS, this study aimed to elucidate potential relationships between N-acetyl and/or alanine and ACAN, COL2A1 and/or MMP13 expression profiles in OA cartilage. Thirty samples from the condyles of five subjects undergoing total knee arthroplasty to treat OA were collected. HRMAS spectra were obtained at 11.7 T for each sample. RNA was subsequently extracted to determine gene expression profiles. A significant negative correlation between N-acetyl metabolite and ACAN gene expression levels was observed; this provides further evidence of N-acetyl as a biomarker of cartilage degeneration. The alanine doublet was distinguished in the spectra of 15 of the 30 specimens of this study. Alanine can only be detected with HRMAS NMR spectroscopy when the collagen framework has been degraded such that alanine is sufficiently mobile to form a distinguished peak in the spectrum. Thus, HRMAS NMR spectroscopy may provide unique localized measurements of collagenous degeneration in OA cartilage. The identification of imaging markers that could provide a link between OA pathology and chondrocyte metabolism will facilitate the

  17. Spinning-sideband patterns in multiple-quantum magic-angle spinning NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Friedrich, Ulli

    1998-12-01

    Recent interest has focused on solid-state NMR experiments which excite multiple-quantum (MQ) coherences in the presence of magic-angle spinning (MAS). Such experiments have been applied to both dipolar-coupled spin Ι = 1/2 and half-integer quadrupolar systems. A feature common to both cases is the observation of interesting spinning sideband patterns in the indirect (MQ) dimension. In this paper, the origin of these patterns is reviewed in terms of two distinct mechanisms: first, rotor encoding of the dipolar or quadrupolar interaction caused by the change in the Hamiltonian active during the MQ reconversion period relative to the excitation period (reconversion rotor encoding, RRE); and, second, rotor modulation of the interaction during the evolution of the MQ coherences in the t1 dimension (evolution rotor modulation, ERM). Only the first mechanism is present for total spin coherences, while for lower-order MQ coherences both mechanisms contribute to the pattern. For dipolar and quadrupolar model systems, i.e., the three protons of a methyl group and quadrupolar nuclei with spin Ι = 3/2 and Ι = 5/2 and axially symmetric first-order quadrupolar interactions, analytical expressions are derived for all orders of MQ MAS signals. Simulations based on these analytical expressions and numerical density matrix simulations are compared with experimental spectra. Additional perturbing influences, such as the heteronuclear dipolar coupling between a quadrupolar and a spin Ι = 1/2 nucleus, are taken into account. The effect of dipolar couplings on a quadrupolar MQ spectrum is found to be enhanced by the order of the observed MQ coherence.

  18. 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.

  19. 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. PMID:23220181

  20. 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.

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

    PubMed

    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(1S)) 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 4mm diameter sapphire rotor containing the sample. The predicted average B(1S) field is 13μT/W(1/2), where S denotes the electron spin. For a routinely achievable input power of 5W the corresponding value is γ(S)B(1S)=0.84MHz. 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 (ϵ) vs. ω(1S)/(2π) for a sample of (13)C-urea dissolved in a 60:40 glycerol/water mixture containing the polarizing agent TOTAPOL; very good agreement was obtained between theory and experiment. PMID:21382733

  2. Intermolecular structure determination of amyloid fibrils with magic-angle spinning and dynamic nuclear polarization NMR

    PubMed Central

    Bayro, Marvin J.; Debelouchina, Galia T.; Eddy, Matthew T.; Birkett, Neil R.; MacPhee, Catherine E.; Rosay, Melanie; Maas, Werner E.; Dobson, Christopher M.

    2011-01-01

    We describe magic-angle spinning NMR experiments designed to elucidate the interstrand architecture of amyloid fibrils. Three methods are introduced for this purpose, two being based on the analysis of long-range 13C-13C correlation spectra and a third based on the identification of intermolecular interactions in 13C-15N spectra. We show, in studies of fibrils formed by the 86-residue SH3 domain of PI3 kinase (PI3-SH3), that efficient 13C-13C correlation spectra display a resonance degeneracy that establishes a parallel, in-register alignment of the proteins in the amyloid fibrils. In addition, this degeneracy can be circumvented to yield direct intermolecular constraints. The 13C-13C experiments are corroborated by 15N-13C correlation spectrum obtained from a mixed [15N,12C]/[14N,13C] sample which directly quantifies interstrand distances. Furthermore, when the spectra are recorded with signal enhancement provided by dynamic nuclear polarization (DNP) at 100 K, we demonstrate a dramatic increase (from 23 to 52) in the number of intermolecular 15N-13C constraints present in the spectra. The increase in the information content is due to the enhanced signal intensities and to the fact that dynamic processes, leading to spectral intensity losses, are quenched at low temperatures. Thus, acquisition of low temperature spectra addresses a problem that is frequently encountered in MAS spectra of proteins. In total the experiments provide 111 intermolecular 13C-13C and 15N-13C constraints that establish that the PI3-SH3 protein strands are aligned in a parallel, in-register arrangement within the amyloid fibril. PMID:21774549

  3. Microwave Field Distribution in a Magic Angle Spinning Dynamic Nuclear Polarization NMR Probe

    PubMed Central

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

    2011-01-01

    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 (B1S) 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 B1S field is 13µT/W1/2, where S denotes the electron spin. For a routinely achievable input power of 5 W the corresponding value is γ SB1S = 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 (ε) vs. ω1S/(2π) 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. PMID:21382733

  4. Nuclear depolarization and absolute sensitivity in magic-angle spinning cross effect dynamic nuclear polarization.

    PubMed

    Mentink-Vigier, Frédéric; Paul, Subhradip; Lee, Daniel; Feintuch, Akiva; Hediger, Sabine; Vega, Shimon; De Paëpe, Gaël

    2015-09-14

    Over the last two decades solid state Nuclear Magnetic Resonance has witnessed a breakthrough in increasing the nuclear polarization, and thus experimental sensitivity, with the advent of Magic Angle Spinning Dynamic Nuclear Polarization (MAS-DNP). To enhance the nuclear polarization of protons, exogenous nitroxide biradicals such as TOTAPOL or AMUPOL are routinely used. Their efficiency is usually assessed as the ratio between the NMR signal intensity in the presence and the absence of microwave irradiation εon/off. While TOTAPOL delivers an enhancement εon/off of about 60 on a model sample, the more recent AMUPOL is more efficient: >200 at 100 K. Such a comparison is valid as long as the signal measured in the absence of microwaves is merely the Boltzmann polarization and is not affected by the spinning of the sample. However, recent MAS-DNP studies at 25 K by Thurber and Tycko (2014) have demonstrated that the presence of nitroxide biradicals combined with sample spinning can lead to a depolarized nuclear state, below the Boltzmann polarization. In this work we demonstrate that TOTAPOL and AMUPOL both lead to observable depolarization at ≈110 K, and that the magnitude of this depolarization is radical dependent. Compared to the static sample, TOTAPOL and AMUPOL lead, respectively, to nuclear polarization losses of up to 20% and 60% at a 10 kHz MAS frequency, while Trityl OX63 does not depolarize at all. This experimental work is analyzed using a theoretical model that explains how the depolarization process works under MAS and gives new insights into the DNP mechanism and into the spin parameters, which are relevant for the efficiency of a biradical. In light of these results, the outstanding performance of AMUPOL must be revised and we propose a new method to assess the polarization gain for future radicals. PMID:26235749

  5. 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.

  6. Non-destructive testing method and apparatus

    DOEpatents

    Akers, Douglas W.

    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.

  7. 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.

  8. Solid-state {sup 17}O magic-angle and dynamic-angle spinning NMR study of the SiO{sub 2} polymorph coesite

    SciTech Connect

    Grandinetti, P.J.; Baltisberger, J.H.; Farnan, I.; Stebbins, J.F.; Werner, U.; Pines, A. |

    1995-08-10

    Five distinctly resolved {sup 17}O solid-state NMR resonances in room temperature coesite, an SiO{sub 2} polymorph, have been observed and assigned using dynamic angle spinning (DAS) at 11.7 T along with magic angle spinning (MAS) spectra at 9.4 and 11.7 T. The {sup 17}O quadrupolar parameters for each of the five oxygen environments in coesite are correlated with the Si-O-Si bridging bond angles determined by diffraction experiments. The sign of e{sup 2}-qQ/h along with the orientation of the electric field gradient for oxygen in the Si-O-Si linkage were determined from a Townes-Dailey analysis of the data. 41 refs., 7 figs., 5 tabs.

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. Magic-angle-spinning NMR of the drug resistant S31N M2 proton transporter from influenza A.

    PubMed

    Andreas, Loren B; Eddy, Matthew T; Chou, James J; Griffin, Robert G

    2012-05-01

    We report chemical shift assignments of the drug-resistant S31N mutant of M2(18-60) determined using 3D magic-angle-spinning (MAS) NMR spectra acquired with a (15)N-(13)C ZF-TEDOR transfer followed by (13)C-(13)C mixing by RFDR. The MAS spectra reveal two sets of resonances, indicating that the tetramer assembles as a dimer of dimers, similar to the wild-type channel. Helicies from the two sets of chemical shifts are shown to be in close proximity at residue H37, and the assignments reveal a difference in the helix torsion angles, as predicted by TALOS+, for the key resistance residue N31. In contrast to wild-type M2(18-60), chemical shift changes are minimal upon addition of the inhibitor rimantadine, suggesting that the drug does not bind to S31N M2. PMID:22480220

  18. 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

  19. SCAM-STMAS: satellite-transition MAS NMR of quadrupolar nuclei with self-compensation for magic-angle misset

    NASA Astrophysics Data System (ADS)

    Ashbrook, Sharon E.; Wimperis, Stephen

    2003-06-01

    Several methods are available for the acquisition of high-resolution solid-state NMR spectra of quadrupolar nuclei with half-integer spin quantum number. Satellite-transition MAS (STMAS) offers an approach that employs only conventional MAS hardware and can yield substantial signal enhancements over the widely used multiple-quantum MAS (MQMAS) experiment. However, the presence of the first-order quadrupolar interaction in the satellite transitions imposes the requirement of a high degree of accuracy in the setting of the magic angle on the NMR probehead. The first-order quadrupolar interaction is only fully removed if the sample spinning angle, χ, equals cos-1(1/ 3) exactly and rotor synchronization is performed. The required level of accuracy is difficult to achieve experimentally, particularly when the quadrupolar interaction is large. If the magic angle is not set correctly, the first-order splitting is reintroduced and the spectral resolution is severely compromised. Recently, we have demonstrated a novel STMAS method (SCAM-STMAS) that is self-compensated for angle missets of up to ±1° via coherence transfer between the two different satellite transitions ST +( mI=+3/2↔+1/2) and ST -( mI=-1/2↔-3/2) midway through the t1 period. In this work we describe in more detail the implementation of SCAM-STMAS and demonstrate its wider utility through 23Na ( I=3/2), 87Rb ( I=3/2), 27Al ( I=5/2), and 59Co ( I=7/2) NMR. We discuss linewidths in SCAM-STMAS and the limits over which angle-misset compensation is achieved and we demonstrate that SCAM-STMAS is more tolerant of temporary spinning rate fluctuations than STMAS, resulting in less " t1 noise" in the two-dimensional spectrum. In addition, alternative correlation experiments, for example involving the use of double-quantum coherences, that similarly display self-compensation for angle misset are investigated. The use of SCAM-STMAS is also considered in systems where other high-order interactions, such as third

  20. 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

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

    PubMed

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

    2010-12-01

    We introduce a cylindrical permanent magnet design that generates a homogeneous and strong magnetic field having an arbitrary inclination with respect to the axis of the cylinder. The analytical theory of 3 D magnetostatics has been applied to this problem, and a hybrid magnet structure has been designed. This structure contains two magnets producing a longitudinal and transverse component for the magnetic field, whose amplitudes and homogeneities can be fully controlled by design. A simple prototype has been constructed using inexpensive small cube magnets, and its magnetic field has been mapped using Hall and NMR probe sensors. This magnet can, in principle, be used for magic angle field spinning NMR and MRI experiments allowing for metabolic chemical shift profiling in small living animals. PMID:20891027

  2. 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. PMID:21958755

  3. Magic angle spinning NMR investigation of influenza A M2(18-60): support for an allosteric mechanism of inhibition.

    PubMed

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

    2010-08-18

    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 (Rmt). We report magic angle spinning NMR spectra of POPC and DPhPC membrane-embedded M2(18-60), both apo and in the presence of Rmt. Similar line widths in the spectra of apo and bound M2 indicate that Rmt 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. An Rmt titration supports a binding stoichiometry of >1 Rmt molecule per channel and shows that nonspecific binding 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

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

    NASA Astrophysics Data System (ADS)

    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 LiCoO 2 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.

  5. 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.

  6. Two-dimensional (13)C-(13)C correlation spectroscopy with magic angle spinning and dynamic nuclear polarization.

    PubMed

    Rosay, Melanie; Weis, Volker; Kreischer, Kenneth E; Temkin, Richard J; Griffin, Robert G

    2002-04-01

    The sensitivity of solid-state NMR experiments can be enhanced with dynamic nuclear polarization (DNP), a technique that transfers the high Boltzmann polarization of unpaired electrons to nuclei. Signal enhancements of up to 23 have been obtained for magic angle spinning (MAS) experiments at 5 T and 85-90 K using a custom-designed high-power gyrotron. The extended stability of MAS/DNP experiments at low temperature is demonstrated with (1)H-driven (13)C spin-diffusion experiments on the amino acid proline. These (13)C-(13)C chemical shift correlation spectra are the first two-dimensional MAS/DNP experiments performed at high field (>1.4 T). PMID:11916398

  7. Molecular orientational dynamics in solid C70: Investigation by one- and two-dimensional magic angle spinning nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Tycko, R.; Dabbagh, G.; Vaughan, G. B. M.; Heiney, P. A.; Strongin, R. M.; Cichy, M. A.; Smith, A. B., III

    1993-11-01

    We present the results of 13C nuclear magnetic resonance (NMR) measurements that probe molecular orientational dynamics in solid C70 in the temperature range 223-343 K. Orientational dynamics affect the NMR line shapes and spin-lattice relaxation rates by modulating the 13C chemical shift anisotropy (CSA). Motionally averaged CSA line shapes, determined from both one-dimensional and two-dimensional magic angle spinning NMR spectra, and relaxation rates are determined for each of the five inequivalent carbon sites in the C70 molecule. Comparisons of the results for the five sites provide evidence for rapid uniaxial molecular reorientation in the monoclinic (T≤280 K) and rhombohedral (280≤T≤330 K) phases and rapid isotropic reorientation in the face-centered cubic (T≥330 K) phase. The orientational correlation time is roughly 2 ns at 250 K and of the order of 5 ps at 340 K.

  8. Biochemical classification of kidney carcinoma biopsy samples using magic-angle-spinning 1H nuclear magnetic resonance spectroscopy.

    PubMed

    Moka, D; Vorreuther, R; Schicha, H; Spraul, M; Humpfer, E; Lipinski, M; Foxall, P J; Nicholson, J K; Lindon, J C

    1998-05-01

    High resolution 1H nuclear magnetic resonance (NMR) spectra using spinning at the magic angle (1H MAS NMR) have been obtained on intact normal and pathological kidney tissue samples from patients undergoing surgery for renal cell carcinoma (RCC). The spectra were measured on ca. 80 mg samples and provided high resolution 1H NMR spectra in which effects of dipolar couplings, chemical shift anisotropy and magnetic susceptibility differences are minimised thus yielding high spectral resolution. Conventional one-dimensional and spin-echo spectra and two-dimensional J-resolved, TOCSY and 1H-13C HMQC spectra were also measured on selected samples and these allowed the assignment of resonances of endogenous substances comprising both cytosolic and membrane components. The tumour tissues were characterised principally by an increased lipid content. These are the first reported results on human tumour tissues using this technique and the approach offers potential for the rapid classification of different types of tumour tissue. PMID:9608434

  9. 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.

  10. 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.

  11. Non-destructive testing and fracture mechanics: A short discussion

    NASA Astrophysics Data System (ADS)

    Zerbst, Uwe; Heckel, Thomas; Carboni, Michele

    2016-02-01

    A short discussion is provided on the relationship between non-destructive testing and fracture mechanics. The basic tasks behind this are to guarantee the safety of a component at a potential hazard loading event, to specify inspection intervals or, alternatively, of demands on non-destructive testing for a fixed inspection regime, to plan accompanying actions for cases of temporary continued operation of structures in which cracks have been detected, and, finally, fatigue strength considerations which take into account initial defects.

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

    SciTech Connect

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

    2011-08-04

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

  13. (1)H and (13)C magic-angle spinning nuclear magnetic resonance studies of the chicken eggshell.

    PubMed

    Pisklak, Dariusz Maciej; Szeleszczuk, Lukasz; Wawer, Iwona

    2012-12-19

    The chicken eggshell, a product of biomineralization, contains inorganic and organic substances whose content changes during the incubation process. Bloch-decay (BD) (1)H, (13)C, and cross-polarization (CP) (13)C nuclear magnetic resonance (NMR) spectra of chicken eggshells were acquired under magic-angle spinning (MAS). Variable contact time (13)C CP MAS NMR experiments revealed the signals of carbonyl groups from organic and inorganic compounds. In the (13)C BD NMR spectra, a single peak at 168.1 ppm was detected, whereas in the (1)H BD spectra, the signals from water and the bicarbonate ion were assigned. A simultaneous decrease of the water signal in the (1)H MAS NMR spectra and an increase of the carbonate ion signal in the (13)C CP MAS NMR spectra of eggshells collected during the incubation period indicate the substitution of calcium ions by hydrogen ions in the calcium carbonate crystalline phase during the incubation of an egg. PMID:23157303

  14. 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

  15. 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

  16. 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. PMID:15140428

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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 13C NMR signals in the 100-200 range are demonstrated with DNP at 25 K. The dependences of signal amplitudes on sample temperature, as well as microwave power, polarization, and frequency, are presented. We show that sample temperatures below 30 K 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.

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

    NASA Astrophysics Data System (ADS)

    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 [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.

  20. 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

  1. 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. PMID:26920835

  2. 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. PMID:26302269

  3. Concentration Profiling in Rat Tissue by High-Resolution Magic-Angle Spinning NMR Spectroscopy: Investigation of a Model Drug

    PubMed Central

    Lucas, Laura H.; Wilson, Sarah F.; Lunte, Craig E.; Larive, Cynthia K.

    2008-01-01

    The utility of high-resolution magic-angle spinning (HR-MAS) NMR for studying drug delivery in whole tissues was explored by dosing female Sprague–Dawley rats with topical or injectable benzoic acid (BA). In principle, HR-MAS NMR permits the detection of both intra- and extracellular compounds. This is an advantage over the previous detection of topically applied BA using microdialysis coupled to HPLC/UV as microdialysis samples only the extracellular space. Skin and muscle samples were analyzed by 1H HR-MAS NMR, and BA levels were determined using an external standard solution added to the sample rotor. One to two percent of the BA topical dose was detected in the muscle, showing that BA penetrated through the dermal and subcutaneous layers. Since BA was not detected in the muscle in the microdialysis studies, the NMR spectra revealed the intracellular localization of BA. The amount of BA detected in muscle after subcutaneous injection correlated with the distance from the dosing site. Overall, the results suggest that HR-MAS NMR can distinguish differences in the local concentration of BA varying with tissue type, dosage method, and tissue proximity to the dosing site. The results illustrate the potential of this technique for quantitative analysis of drug delivery and distribution and the challenges to be addressed as the method is refined. PMID:15859619

  4. 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.

  5. Order-selective multiple-quantum excitation in magic-angle spinning NMR: creating triple-quantum coherences with a trilinear Hamiltonian

    NASA Astrophysics Data System (ADS)

    Edén, Mattias

    2002-12-01

    Order-selective multiple-quantum excitation in magic-angle spinning nuclear magnetic resonance is explored using a class of symmetry-based pulse sequences, denoted S Mχ. Simple rules are presented that aid the design of S Mχ schemes with certain desirable effective Hamiltonians. They are applied to construct sequences generating trilinear effective dipolar Hamiltonians, suitable for efficient excitation of triple-quantum coherences in rotating solids. The new sequences are investigated numerically and demonstrated by 1H experiments on adamantane.

  6. Non-destructive methods for food texture assessment

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  7. Automated Non-Destructive Testing Array Evaluation System

    SciTech Connect

    Wei, T; Zavaljevski, N; Bakhtiari, S; Miron, A; Kupperman, D

    2004-12-24

    Automated Non-Destructive Testing Array Evaluation System (ANTARES) sofeware alogrithms were developed for use on X-probe(tm) data. Data used for algorithm development and preliminary perfomance determination was obtained for USNRC mock-up at Argone and data from EPRI.

  8. 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.

  9. Metabolic profiling of a Schistosoma mansoni infection in mouse tissues using magic angle spinning-nuclear magnetic resonance spectroscopy.

    PubMed

    Li, Jia V; Holmes, Elaine; Saric, Jasmina; Keiser, Jennifer; Dirnhofer, Stephan; Utzinger, Jürg; Wang, Yulan

    2009-04-01

    In order to enhance our understanding of physiological and pathological consequences of a patent Schistosoma mansoni infection in the mouse, we examined the metabolic responses of different tissue samples recovered from the host animal using a metabolic profiling strategy. Ten female NMRI mice were infected with approximately 80 S. mansoni cercariae each, and 10 uninfected age- and sex-matched animals served as controls. At day 74 post infection (p.i.), mice were killed and jejunum, ileum, colon, liver, spleen and kidney samples were removed. We employed (1)H magic angle spinning-nuclear magnetic resonance spectroscopy to generate tissue-specific metabolic profiles. The spectral data were analyzed using multivariate modelling methods including an orthogonal signal corrected-projection to latent structure analysis and hierarchical principal component analysis to assess the differences and/or similarities in metabolic responses between infected and non-infected control mice. Most tissues obtained from S. mansoni-infected mice were characterized by high levels of amino acids, such as leucine, isoleucine, lysine, glutamine and asparagine. High levels of membrane phospholipid metabolites, including glycerophosphoryl choline and phosphoryl choline were found in the ileum, colon, liver and spleen of infected mice. Additionally, low levels of energy-related metabolites, including lipids, glucose and glycogen were observed in ileum, spleen and liver samples of infected mice. Energy-related metabolites in the jejunum, liver and renal medulla were found to be positively correlated with S. mansoni worm burden upon dissection. These findings show that a patent S. mansoni infection causes clear disruption of metabolism in a range of tissues at a molecular level, which can be interpreted in relation to the previously reported signature in a biofluid (i.e. urine), giving further evidence of the global effect of the infection. PMID:19068218

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

    PubMed

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

    2013-10-01

    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

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

    PubMed

    Righi, Valeria; Constantinou, Caterina; Kesarwani, Meenu; Rahme, Laurence G; Tzika, Aria A

    2013-09-01

    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 (1)H 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

  12. Characterization of metabolites in infiltrating gliomas using ex vivo ¹H high-resolution magic angle spinning spectroscopy.

    PubMed

    Elkhaled, Adam; Jalbert, Llewellyn; Constantin, Alexandra; Yoshihara, Hikari A I; Phillips, Joanna J; Molinaro, Annette M; Chang, Susan M; Nelson, Sarah J

    2014-05-01

    Gliomas are routinely graded according to histopathological criteria established by the World Health Organization. Although this classification can be used to understand some of the variance in the clinical outcome of patients, there is still substantial heterogeneity within and between lesions of the same grade. This study evaluated image-guided tissue samples acquired from a large cohort of patients presenting with either new or recurrent gliomas of grades II-IV using ex vivo proton high-resolution magic angle spinning spectroscopy. The quantification of metabolite levels revealed several discrete profiles associated with primary glioma subtypes, as well as secondary subtypes that had undergone transformation to a higher grade at the time of recurrence. Statistical modeling further demonstrated that these metabolomic profiles could be differentially classified with respect to pathological grading and inter-grade conversions. Importantly, the myo-inositol to total choline index allowed for a separation of recurrent low-grade gliomas on different pathological trajectories, the heightened ratio of phosphocholine to glycerophosphocholine uniformly characterized several forms of glioblastoma multiforme, and the onco-metabolite D-2-hydroxyglutarate was shown to help distinguish secondary from primary grade IV glioma, as well as grade II and III from grade IV glioma. These data provide evidence that metabolite levels are of interest in the assessment of both intra-grade and intra-lesional malignancy. Such information could be used to enhance the diagnostic specificity of in vivo spectroscopy and to aid in the selection of the most appropriate therapy for individual patients. PMID:24596146

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

    NASA Astrophysics Data System (ADS)

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

    2002-06-01

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

  14. Magic-Angle Spinning Solid-State NMR Spectroscopy of Nanodisc– Embedded Human CYP3A4†

    PubMed Central

    Kijac, Aleksandra; Li, Ying; Sligar, Stephen G.; Rienstra, Chad M.

    2008-01-01

    Cytochrome P450 (CYP) 3A4 contributes to the metabolism of approximately 50% of commercial drugs by oxidizing a large number of structurally diverse substrates. Like other endoplasmic reticulum-localized P450s, CYP3A4 contains a membrane-anchoring N-terminal helix and a significant number of hydrophobic domains, important for the interaction between CYP3A4 and the membrane. Although the membrane affects specificity of CYP3A4 ligand binding, the structural details of the interaction have not been revealed so far because x-ray crystallography studies are available only for the soluble domain of CYP3A4. Here we report sample preparation and initial magic-angle spinning (MAS) solid-state NMR (SSNMR) of CYP3A4 (Δ3−12) embedded in a nanoscale membrane bilayer, or Nanodisc. The growth protocol yields ∼2.5 mg of the enzymatically active, uniformly 13C, 15N-enriched CYP3A4 from a liter of growth medium. Polyethylene glycol 3350-precipitated CYP3A4 in Nanodiscs yields spectra of high resolution and sensitivity, consistent with a folded, homogeneous protein. CYP3A4 in Nanodiscs remains enzymatically active throughout the precipitation protocol as monitored by bromocriptine binding. The 13C line widths measured from 13C-13C 2D chemical shift correlation spectra are ∼0.5 ppm. The secondary structure distribution within several amino acid types determined from 13C chemical shifts is consistent with the ligand-free x-ray structures. These results demonstrate that MAS SSNMR can be performed on Nanodisc-embedded membrane proteins in a folded, active state. The combination of SSNMR and Nanodisc methodologies opens up new possibilities for obtaining structural information on CYP3A4 and other integral membrane proteins with full retention of functionality. PMID:17985934

  15. High-resolution paramagnetically enhanced solid-state NMR spectroscopy of membrane proteins at fast magic angle spinning.

    PubMed

    Ward, Meaghan E; Wang, Shenlin; Krishnamurthy, Sridevi; Hutchins, Howard; Fey, Michael; Brown, Leonid S; Ladizhansky, Vladimir

    2014-01-01

    Magic angle spinning nuclear magnetic resonance (MAS NMR) is well suited for the study of membrane proteins in membrane mimetic and native membrane environments. These experiments often suffer from low sensitivity, due in part to the long recycle delays required for magnetization and probe recovery, as well as detection of low gamma nuclei. In ultrafast MAS experiments sensitivity can be enhanced through the use of low power sequences combined with paramagnetically enhanced relaxation times to reduce recycle delays, as well as proton detected experiments. In this work we investigate the sensitivity of (13)C and (1)H detected experiments applied to 27 kDa membrane proteins reconstituted in lipids and packed in small 1.3 mm MAS NMR rotors. We demonstrate that spin diffusion is sufficient to uniformly distribute paramagnetic relaxation enhancement provided by either covalently bound or dissolved CuEDTA over 7TM alpha helical membrane proteins. Using paramagnetic enhancement and low power decoupling in carbon detected experiments we can recycle experiments ~13 times faster than under traditional conditions. However, due to the small sample volume the overall sensitivity per unit time is still lower than that seen in the 3.2 mm probe. Proton detected experiments, however, showed increased efficiency and it was found that the 1.3 mm probe could achieve sensitivity comparable to that of the 3.2 mm in a given amount of time. This is an attractive prospect for samples of limited quantity, as this allows for a reduction in the amount of protein that needs to be produced without the necessity for increased experimental time. PMID:24338448

  16. 19F Magic angle spinning NMR reporter molecules: empirical measures of surface shielding, polarisability and H-bonding.

    PubMed

    Budarin, Vitaliy L; Clark, James H; Deswarte, Fabien E I; Mueller, Karl T; Tavener, Stewart J

    2007-06-14

    Magic Angle Spinning (MAS) (19)F NMR spectra have been obtained and chemical shifts measured for 37 molecules in the gas phase and adsorbed on the surfaces of six common materials: octadecyl- and octyl-functionalised chromatography silicas, Kieselgel 100 silica, Brockmann neutral alumina, Norit activated charcoal and 3-(1-piperidino)propyl functionalised silica. From these six surfaces, octadecyl-silica is selected as a non-polar reference to which the others are compared. The change in chemical shift of a fluorine nucleus within a molecule on adsorption to a surface from the gas phase, Deltadelta(gas)(surface), is described by the empirical relationship: Deltadelta(gas)(surface) = delta(s) + (alpha(s)+pi(s))/alpha(r) (Deltadelta(gas)(reference) - delta(r)) + delta(HBA) + delta(HBD), where delta(s) and delta(r) are constants that describe the chemical shift induced by the electromagnetic field of the surface under investigation and reference surface, alpha(s) and alpha(r) are the relative surface polarisability for the surface and reference, pi(s) is an additional contribution to the surface polarisabilities due to its ability to interact with aromatic molecules, and delta(HBA) and delta(HBD) are measurements of the hydrogen acceptor and donor properties of the surface. These empirical parameters are measured for the surfaces under study. Silica and alumina are found to undergo specific interactions with aromatic reporter molecules and both accept and donate H-bonds. Activated charcoal was found to have an extreme effect on shielding but no specific interactions with the adsorbed molecules. 3-(1-Piperidino)propyl functionalised silica exhibits H-bond acceptor ability, but does not donate H-bonds. PMID:17487325

  17. 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

  18. The mobility of chondroitin sulfate in articular and artificial cartilage characterized by 13C magic-angle spinning NMR spectroscopy.

    PubMed

    Scheidt, Holger A; Schibur, Stephanie; Magalhães, Alvicler; de Azevedo, Eduardo R; Bonagamba, Tito J; Pascui, Ovidiu; Schulz, Ronny; Reichert, Detlef; Huster, Daniel

    2010-06-01

    We have studied the molecular dynamics of one of the major macromolecules in articular cartilage, chondroitin sulfate. Applying (13)C high-resolution magic-angle spinning NMR techniques, the NMR signals of all rigid macromolecules in cartilage can be suppressed, allowing the exclusive detection of the highly mobile chondroitin sulfate. The technique is also used to detect the chondroitin sulfate in artificial tissue-engineered cartilage. The tissue-engineered material that is based on matrix producing chondrocytes cultured in a collagen gel should provide properties as close as possible to those of the natural cartilage. Nuclear relaxation times of the chondroitin sulfate were determined for both tissues. Although T(1) relaxation times are rather similar, the T(2) relaxation in tissue-engineered cartilage is significantly shorter. This suggests that the motions of chondroitin sulfate in natural and artificial cartilage are different. The nuclear relaxation times of chondroitin sulfate in natural and tissue-engineered cartilage were modeled using a broad distribution function for the motional correlation times. Although the description of the microscopic molecular dynamics of the chondroitin sulfate in natural and artificial cartilage required the identical broad distribution functions for the correlation times of motion, significant differences in the correlation times of motion that are extracted from the model indicate that the artificial tissue does not fully meet the standards of the natural ideal. This could also be confirmed by macroscopic biomechanical elasticity measurements. Nevertheless, these results suggest that NMR is a useful tool for the investigation of the quality of artificially engineered tissue. PMID:20091673

  19. 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.

  20. 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. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26687421

  1. 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

  2. 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

  3. 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!

  4. 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.

  5. Mathematical models applied in inductive non-destructive testing

    NASA Astrophysics Data System (ADS)

    Wac-Wlodarczyk, A.; Goleman, R.; Czerwinski, D.; Gizewski, T.

    Non-destructive testing are the wide group of investigative methods of non-homogenous material. Methods of computer tomography, ultrasonic, magnetic and inductive methods still developed are widely applied in industry. In apparatus used for non-destructive tests, the analysis of signals is made on the basis of complex system answers. The answer is linearized due to the model of research system. In this paper, the authors will discuss the applications of the mathematical models applied in investigations of inductive magnetic materials. The statistical models and other gathered in similarity classes will be taken into consideration. Investigation of mathematical models allows to choose the correct method, which in consequence leads to precise representation of the inner structure of examined object. Inductive research of conductive media, especially those with ferromagnetic properties, are run with high frequency magnetic field (eddy-currents method), which considerably decrease penetration depth.

  6. 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. PMID:22163754

  7. Non-destructive metallurgical analysis of astrolabes utilizing synchrotron radiation.

    SciTech Connect

    Newbury, B.; Stephenson, B.; Almer, J. D.; Notis, M.; Haeffner, D. R.; Slade Cargill, G., III

    2002-05-22

    From the experiments performed it is possible to determine a wide range of information about the metallurgy of the astrolabes studied. It was found that different brass alloys were used for components that were cast and those that were mechanically deformed. Chemical composition, forming history, and thickness measurements are all determined non-destructively, illustrating that this technique could be useful for many applications with metal artifact analysis where non-intrusive methods are required.

  8. 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.

  9. Sensitivity and resolution enhanced solid-state NMR for paramagnetic systems and biomolecules under very fast magic angle spinning.

    PubMed

    Parthasarathy, Sudhakar; Nishiyama, Yusuke; Ishii, Yoshitaka

    2013-09-17

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

  10. 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

  11. Non-destructive electrical characterization of controlled Waspaloy microstructures

    NASA Astrophysics Data System (ADS)

    G. Kelekanjeri, V. Siva Kumar

    In this research, controlled Waspaloy microstructures are produced with the objective of studying microstructural evolution in this alloy via non-destructive electrical measurements. Waspaloy is a precipitation-hardenable gamma-gamma' nickel-base superalloy that is used in turbine blade applications demanding superior strength retention capabilities at elevated temperatures. Overall, three different sets of microstructures were produced that varied systematically as a function of the matrix (gamma) grain size and gamma' precipitate size distribution or just the latter. Initial solutionizing treatments conducted at 1045°C, 1090°C and 1145°C resulted in average y grain size of 13, 52 and 89 mum respectively. A vacancy stabilization treatment at 1045°C followed the solutionizing treatments in Set I experiments, after which the specimens were aged at 800°C for durations ranging from 0.1 hrs to 100 hrs. In Sets 11 and III, the matrix grain size was kept unchanged by an initial solution-treatment at 1145°C. The stabilization treatment at 1045°C was only conducted in Set II after the solution-treatment. Aging experiments were then conducted at 700°C (or 725°C in Set III), 800°C and 875°C to study the growth kinetics of gamma' precipitate distribution. The specimens with controlled microstructures were investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), x-ray diffraction (XRD), ultra small-angle x-ray scattering (USAXS) and dc four-point probe resistivity. The applicability of two and four-probe ac impedance techniques was also investigated. Characterization of heat-treated specimens. Solution-treated SEM microstructures showed the presence of polygonal etch-pit shapes, which was proposed to be due to the condensation of excess quenched-in vacancies along crystallographically soft-directions in the gamma phase. The etch-pits evolved upon subsequent aging into progressively irregular shapes, concurrent with gamma' growth inside

  12. Investigations and Non-destructive Testing in New Building Design

    NASA Astrophysics Data System (ADS)

    Klimenov, V.; Ovchinnikov, A.; Osipov, S.; Shtein, A.; Ustinov, A.; Danilson, A.

    2016-01-01

    Mechanical rebar couplers are preferable in the advanced building construction and structural design of antiseismic elements. The paper presents destructive inspection techniques used to investigate stress fields (tensile and compressive) and deformation curves for mechanical rebar splicing. The properties of mechanical rebar splicing are investigated by the non-destructive testing digital radiography. The behavior of real connections (column-to- column, beam-to-column) is studied under static and dynamic loads. Investigation results allow the elaboration of recommendations on their application in the universal prefabricated antiseismic structural system developed at Tomsk State University of Architecture and Building, Tomsk, Russia.

  13. Potential techniques for non-destructive evaluation of cable materials

    NASA Astrophysics Data System (ADS)

    Gillen, Kenneth T.; Clough, Roger L.; Mattson, Bengt; Stenberg, Bengt; Oestman, Erik

    This paper describes the connection between mechanical degradation of common cable materials, in radiation and elevated temperature environments, and density increases caused by the oxidation which leads to this degradation. Two techniques based on density changes are suggested as potential non-destructive evaluation (NDE) procedures which may be applicable to monitoring the mechanical condition of cable materials in power plant environments. The first technique is direct measurement of density changes, via a density gradient column, using small shavings removed from the surface of cable jackets at selected locations. The second technique is computed X-ray tomography, utilizing a portable scanning device.

  14. 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)

  15. Non-destructive characterization using pulsed fast-thermal neutrons

    NASA Astrophysics Data System (ADS)

    Womble, P. C.; Schultz, F. J.; Vourvopoulos, G.

    1995-05-01

    Explosives, illicit drugs, and other contraband materials contain various chemical elements in quantities and ratios that differentiate them from each other and from innocuous substances. Furthermore, the major chemical elements in coal can provide information about various parameters of importance to the coal industry. In both examples, the non-destructive identification of chemical elements can be performed using pulsed fast-thermal neutrons that, through nuclear reactions, excite the nuclei of the various elements. This technique is being currently developed for the dismantling of nuclear weapons classified as trainers, and for the on-line coal bulk analysis.

  16. 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. PMID:27364976

  17. Unexpected effects of third-order cross-terms in heteronuclear spin systems under simultaneous radio-frequency irradiation and magic-angle spinning NMR

    NASA Astrophysics Data System (ADS)

    Tatton, Andrew S.; Frantsuzov, Ilya; Brown, Steven P.; Hodgkinson, Paul

    2012-02-01

    We recently noted [R. K. Harris, P. Hodgkinson, V. Zorin, J.-N. Dumez, B. Elena, L. Emsley, E. Salager, and R. Stein, Magn. Reson. Chem. 48, S103 (2010), 10.1002/mrc.2636] anomalous shifts in apparent 1H chemical shifts in experiments using 1H homonuclear decoupling sequences to acquire high-resolution 1H NMR spectra for organic solids under magic-angle spinning (MAS). Analogous effects were also observed in numerical simulations of model 13C,1H spin systems under homonuclear decoupling and involving large 13C,1H dipolar couplings. While the heteronuclear coupling is generally assumed to be efficiently suppressed by sample spinning at the magic angle, we show that under conditions typically used in solid-state NMR, there is a significant third-order cross-term from this coupling under the conditions of simultaneous MAS and homonuclear decoupling for spins directly bonded to 1H. This term, which is of the order of 100 Hz under typical conditions, explains the anomalous behaviour observed on both 1H and 13C spins, including the fast dephasing observed in 13C{1H} heteronuclear spin-echo experiments under 1H homonuclear decoupling. Strategies for minimising the impact of this effect are also discussed.

  18. Slow magic-angle rotation 13C NMR studies of solid phosphonium iodides. The interplay of dipolar, shielding, and indirect coupling tensors

    NASA Astrophysics Data System (ADS)

    Harris, Robin K.; Packer, Kenneth J.; Thayer, Ann M.

    High-resolution 13C NMR spectra were recorded for solid [Me 2Ph 2P] +I - and [Me 3PhP] +I - using high-power decoupling, cross-polarization, and magic-angle rotation. Spectra of the ipso carbon, obtained with the nonquaternary suppression (dipolar dephasing) pulse sequence, show an unequal distribution intensity of spinning sidebands for the two peaks split by the isotropic coupling constant 1JPC. This effect is traced to the joint influence of (P, C) dipolar coupling and 13C shielding anisotropy. The existence of scalar coupling enables magic-angle rotation to distinguish the two subspectra which are present. Analysis of the sideband patterns yields values of the NMR parameters. Under certain assumptions, including that the axis of greatest shielding is perpendicular to the PC bond, it is shown that 1JPC is positive. In contrast to traditional methods of determining signs, this conclusion does not rely on knowledge of signs of other coupling constants.

  19. 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.

  20. 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.

  1. 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

  2. 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

  3. 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.

  4. 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.

  5. Electromagnetic non-destructive technique for duplex stainless steel characterization

    NASA Astrophysics Data System (ADS)

    Rocha, João Vicente; Camerini, Cesar; Pereira, Gabriela

    2016-02-01

    Duplex stainless steel (DSS) is a two-phase (ferrite and austenite) material, which exhibits an attractive combination of mechanical properties and high corrosion resistance, being commonly employed for equipment of petrochemical plants, refining units and oil & gas platforms. The best properties of DSS are achieved when the phases are in equal proportions. However, exposition to high temperatures (e.g. welding process) may entail undesired consequences, such as deleterious phases precipitation (e.g. sigma, chi) and different proportion of the original phases, impairing dramatically the mechanical and corrosion properties of the material. A detailed study of the magnetic behavior of DSS microstructure with different ferrite austenite ratios and deleterious phases content was accomplished. The non destructive method evaluates the electromagnetic properties changes in the material and is capable to identify the presence of deleterious phases into DSS microstructure.

  6. 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.

  7. Induction thermography for non-destructive evaluation of adhesive bonds

    NASA Astrophysics Data System (ADS)

    Balaji, L.; Balasubramaniam, Krishnan; Krishnamurthy, C. V.

    2013-01-01

    Adhesive bonding is widely used in automotive industry in the recent times. One of the major problems with adhesive bonds is the lack of a suitable non-destructive evaluation technique for assessing bonding. In this paper, an experimental study was carried out to apply induction thermography technique to evaluate adhesively bonded steel plates. Samples were fabricated with artificial defects such as air gap, foreign material, and improper adhesive filling. Induction thermography technique was found to detect defects and foreign inclusions. The sample specimen was also inspected using standard techniques such as Ultrasonic testing and Radiography testing. Defect detecting capabilities of the three techniques are compared. Induction thermography heating was FE modelled in 3D using COMSOL 3.5a. The simulated Induction thermography model was compared and validated with experimental results.

  8. Non-destructive Raman analyses - polyacetylenes in plants

    NASA Astrophysics Data System (ADS)

    Schrader, Bernhard; Schulz, Hartwig; Baranska, Malgorzata; Andreev, George N.; Lehner, Caroline; Sawatzki, Juergen

    2005-05-01

    Ferdinand Bohlmann has described the isolation, the identification and the structure elucidation of acetylene compounds in many plants, and confirmed it by its synthesis. We have recorded the Raman spectra of most of these plants non-destructively by FT-Raman spectroscopy using radiation at 1064 nm. We could not observe any interfering fluorescence. We found acetylene compounds in some plants, even distinct compounds with different concentration in various parts of it. The distribution of the different compounds over the plant can be observed and their changes during the ontogenesis can be followed by a FT-Raman mapping technique. Of special help is a library of Raman and IR spectra and the structure of the compounds, synthesized by Bohlmann. Thus, the Raman technique allows analyses in a very short time replacing the usual time-consuming separation procedures and avoiding artefacts during clean-up procedures.

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

    NASA Astrophysics Data System (ADS)

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

    2013-08-01

    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.

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

    NASA Astrophysics Data System (ADS)

    Gajdacz, Miroslav; Pedersen, Poul; Mørch, Troels; Hilliard, Andrew; Arlt, Jan; Sherson, Jacob

    2013-05-01

    We investigate non-destructive measurements of ultra-cold atomic clouds based on dark field imaging of spatially resolved Faraday rotation. In particular, we pursue applications to dynamically controlled ultracold atoms. The dependence of the Faraday signal on laser detuning, atomic density and temperature is characterized in a detailed comparison with theory. In particular the destructivity per measurement is extremely low and we illustrate this by imaging the same cloud up to 2000 times. The technique is applied to avoid the effect of shot-to-shot fluctuations in atom number calibration. Adding dynamic changes to system parameters, we demonstrate single-run vector magnetic field imaging and single-run spatial imaging of the system's dynamic behavior. The method can be implemented particularly easily in standard imaging systems by the insertion of an extra polarizing beam splitter. These results are steps towards quantum state engineering using feedback control of ultracold atoms.

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

    PubMed

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

    2013-08-01

    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. PMID:24007051

  12. EVALUATION OF TRANSPORTATION OPTIONS FOR INTERMEDIATE NON DESTRUCTIVE EXAMINATIONS

    SciTech Connect

    Case, Susan; Hoggard, Gary

    2014-07-01

    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.”

  13. Recent developments in solid-state magic-angle spinning, nuclear magnetic resonance of fully and significantly isotopically labelled peptides and proteins.

    PubMed Central

    Straus, Suzana K

    2004-01-01

    In recent years, a large number of solid-state nuclear magnetic resonance (NMR) techniques have been developed and applied to the study of fully or significantly isotopically labelled ((13)C, (15)N or (13)C/(15)N) biomolecules. In the past few years, the first structures of (13)C/(15)N-labelled peptides, Gly-Ile and Met-Leu-Phe, and a protein, Src-homology 3 domain, were solved using magic-angle spinning NMR, without recourse to any structural information obtained from other methods. This progress has been made possible by the development of NMR experiments to assign solid-state spectra and experiments to extract distance and orientational information. Another key aspect to the success of solid-state NMR is the advances made in sample preparation. These improvements will be reviewed in this contribution. Future prospects for the application of solid-state NMR to interesting biological questions will also briefly be discussed. PMID:15306412

  14. {sup 129}Xe magic-angle spinning spectra of xenon in zeolite NaA direct observation of mixed clusters of co-adsorbed species.

    SciTech Connect

    Jameson, A. K.; Jameson, C. J.; de Dios, A. C.; Oldfield, E.; Gerald, R. E., II; Turner, G. L.; Chemical Engineering; Loyola Univ.; Univ. of Illinois at Chicago; Univ. of Illinois; Spectral Data Services, Inc.

    1995-01-01

    We present the first demonstration that the individual {sup 129}Xe resonances corresponding to Xe{sub n} (n = 1-8) clusters inside the {alpha}-cages of zeolite NaA can be narrowed under magic-angle spinning (MAS). Under these high-resolution conditions we also observe upon addition of Kr the individual peaks corresponding to mixed clusters, Xe{sub n}Kr{sub m}, inside the a-cages, which will allow the first direct determination of the distribution of co-adsorbates in a microporous solid. Under MAS the chemical shifts of the Xe{sub n} clusters are shown to be highly sensitive to 'disorder' in the zeolite and provides new, quantitative information about the presence of {alpha}-cages of several types.

  15. Two-Dimensional NMR Study of a Liquid-Crystal Solution under Magic-Angle Spinning. Conformation of Carboxylic Ionophore Lasalocid A Dissolved in a Lyotropic Liquid Crystal

    NASA Astrophysics Data System (ADS)

    Kimura, Atsuomi; Kano, Tetsushi; Fujiwara, Hideaki

    1996-07-01

    The conformation of a carboxylic ionophore, lasalocid A, has been determined in a lyotropic liquid crystal by means of magic-angle spinning (MAS) and two-dimensional NMR experiments. The information extracted from ROESY spectra measured under MAS was analyzed according to the distance-geometry algorithm. The liquid crystal used for the solvent is cesium perfluorooctanoate dissolved in D2O, and the resulting structure of lasalocid A is a cyclic one, indicating cation complexation within a hydrophobic region of the liquid crystal. In this way, the two-dimensional MAS NMR experiment is proved to be a useful technique in conformational studies of complex molecules dissolved in lyotropic liquid crystal which may be regarded as offering a membrane-like environment.

  16. 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. PMID:26367873

  17. Caught in the act: ATP hydrolysis of an ABC-multidrug transporter followed by real-time magic angle spinning NMR.

    PubMed

    Hellmich, Ute A; Haase, Winfried; Velamakanni, Saroj; van Veen, Hendrik W; Glaubitz, Clemens

    2008-10-15

    The ATP binding cassette (ABC) transporter LmrA from Lactococcus lactis transports cytotoxic molecules at the expense of ATP. Molecular and kinetic details of LmrA can be assessed by solid-state nuclear magnetic resonance (ssNMR), if functional reconstitution at a high protein-lipid ratio can be achieved and the kinetic rate constants are small enough. In order to follow ATP hydrolysis directly by 31P-magic angle spinning (MAS) nuclear magnetic resonance (NMR), we generated such conditions by reconstituting LmrA-dK388, a mutant with slower ATP turnover rate, at a protein-lipid ration of 1:150. By analysing time-resolved 31P spectra, protein activity has been directly assessed. These data demonstrate the general possibility to perform ssNMR studies on a fully active full length ABC transporter and also form the foundation for further kinetic studies on LmrA by NMR. PMID:18817774

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

    NASA Astrophysics Data System (ADS)

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

    2011-10-01

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

  19. 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.

  20. 1H high resolution magic-angle coil spinning (HR-MACS) μNMR metabolic profiling of whole Saccharomyces cervisiae cells: a demonstrative study

    PubMed Central

    Wong, Alan; Boutin, Céline; Aguiar, Pedro M.

    2014-01-01

    The low sensitivity and thus need for large sample volume is one of the major drawbacks of Nuclear Magnetic Resonance (NMR) spectroscopy. This is especially problematic for performing rich metabolic profiling of scarce samples such as whole cells or living organisms. This study evaluates a 1H HR-MAS approach for metabolic profiling of small volumes (250 nl) of whole cells. We have applied an emerging micro-NMR technology, high-resolution magic-angle coil spinning (HR-MACS), to study whole Saccharomyces cervisiae cells. We find that high-resolution high-sensitivity spectra can be obtained with only 19 million cells and, as a demonstration of the metabolic profiling potential, we perform two independent metabolomics studies identifying the significant metabolites associated with osmotic stress and aging. PMID:24971307

  1. (1)H high resolution magic-angle coil spinning (HR-MACS) μNMR metabolic profiling of whole Saccharomyces cervisiae cells: a demonstrative study.

    PubMed

    Wong, Alan; Boutin, Céline; Aguiar, Pedro M

    2014-01-01

    The low sensitivity and thus need for large sample volume is one of the major drawbacks of Nuclear Magnetic Resonance (NMR) spectroscopy. This is especially problematic for performing rich metabolic profiling of scarce samples such as whole cells or living organisms. This study evaluates a (1)H HR-MAS approach for metabolic profiling of small volumes (250 nl) of whole cells. We have applied an emerging micro-NMR technology, high-resolution magic-angle coil spinning (HR-MACS), to study whole Saccharomyces cervisiae cells. We find that high-resolution high-sensitivity spectra can be obtained with only 19 million cells and, as a demonstration of the metabolic profiling potential, we perform two independent metabolomics studies identifying the significant metabolites associated with osmotic stress and aging. PMID:24971307

  2. Homonuclear dipolar recoupling under ultra-fast magic-angle spinning: probing 19F-19F proximities by solid-state NMR.

    PubMed

    Wang, Qiang; Hu, Bingwen; Lafon, Olivier; Trébosc, Julien; Deng, Feng; Amoureux, Jean-Paul

    2010-03-01

    We describe dipolar recoupling methods that accomplish, at high magic-angle spinning (MAS) frequencies, the excitation of double-quantum (DQ) coherences between spin-1/2 nuclei. We employ rotor-synchronized symmetry-based pulse sequences which are either gamma-encoded or non-gamma-encoded. The sensitivity and the robustness to both chemical-shift anisotropy and offset are examined. We also compare different techniques to avoid signal folding in the indirect dimension of two-dimensional double-quantum<-->single-quantum (DQ-SQ) spectra. This comprehensive analysis results in the identification of satisfactory conditions for dipolar (19)F-(19)F recoupling at high magnetic fields and high MAS frequencies. The utility of these recoupling methods is demonstrated with high-resolution DQ-SQ NMR spectra, which allow probing (19)F-(19)F proximities in powered fluoroaluminates. PMID:20044288

  3. In situ structural characterization of a recombinant protein in native Escherichia coli membranes with solid-state magic-angle-spinning NMR.

    PubMed

    Fu, Riqiang; Wang, Xingsheng; Li, Conggang; Santiago-Miranda, Adriana N; Pielak, Gary J; Tian, Fang

    2011-08-17

    The feasibility of using solid-state magic-angle-spinning NMR spectroscopy for in situ structural characterization of the LR11 (sorLA) transmembrane domain (TM) in native Escherichia coli membranes is presented. LR11 interacts with the human amyloid precursor protein (APP), a central player in the pathology of Alzheimer's disease. The background signals from E. coli lipids and membrane proteins had only minor effects on the LR11 TM resonances. Approximately 50% of the LR11 TM residues were assigned by using (13)C PARIS data. These assignments allowed comparisons of the secondary structure of the LR11 TM in native membrane environments and commonly used membrane mimics (e.g., micelles). In situ spectroscopy bypasses several obstacles in the preparation of membrane proteins for structural analysis and offers the opportunity to investigate how membrane heterogeneity, bilayer asymmetry, chemical gradients, and macromolecular crowding affect the protein structure. PMID:21774553

  4. Conformational dynamics of phenylene rings in poly(p-phenylene vinylene) as revealed by 13C magic-angle-spinning exchange nuclear magnetic resonance experiments

    NASA Astrophysics Data System (ADS)

    deAzevedo, E. R.; Franco, R. W. A.; Marletta, A.; Faria, R. M.; Bonagamba, T. J.

    2003-08-01

    Poly(p-phenylene vinylene) (PPV) has shown a great potential for electro-optical applications due to its electroluminescent and semiconducting properties. Such properties are directly related with the polymer chain conformation and dynamics. Then, it is important to understand in detail the local chain motions. In this work, three 13C solid-state magic-angle-spinning (MAS) exchange NMR techniques were used to study conformational dynamics of phenylene rings in PPV. The standard 2D MAS exchange experiment was used to identify exchange processes between equivalent and nonequivalent sites. Centerband-only detection of exchange (CODEX) experiments were applied to determine the amplitude of the phenylene ring flips and small-angle oscillations. Additionally, a new version of the CODEX technique, which allows for the selective observation of segments executing exchange between non-equivalent sites, is demonstrated and applied to determine the flipping fractions and the activation energies of the phenylene ring rotations. It was found that, at -15 °C, (26±3)% of the rings undergo 180° flips in the millisecond time scale, with average imprecision of (30±5)° and activation energies of (23±3) kJ/mol. Other (31±10)% of the rings perform only small-angle oscillations with an average amplitude of (9±2)°. These results corroborate previous experimental data and agree with recent ab initio calculations of potential energies barriers in phenylenevinylene oligomers.

  5. 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.

  6. Non-destructive investigation of thermoplastic reinforced composites

    SciTech Connect

    Hassen, Ahmed; Vaidya, Uday

    2016-01-01

    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.

  7. 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.

  8. 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.

  9. 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

  10. 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.

  11. Non-destructive investigation of thermoplastic reinforced composites

    DOE PAGESBeta

    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

  12. 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.

  13. 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. PMID:25824342

  14. 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.

  15. Complex Archaeological Prospection Using Combination of Non-destructive Techniques

    NASA Astrophysics Data System (ADS)

    Faltýnová, M.; Pavelka, K.; Nový, P.; Šedina, J.

    2015-08-01

    This article describes the use of a combination of non-destructive techniques for the complex documentation of a fabulous historical site called Devil's Furrow, an unusual linear formation lying in the landscape of central Bohemia. In spite of many efforts towards interpretation of the formation, its original form and purpose have not yet been explained in a satisfactory manner. The study focuses on the northern part of the furrow which appears to be a dissimilar element within the scope of the whole Devil's Furrow. This article presents detailed description of relics of the formation based on historical map searches and modern investigation methods including airborne laser scanning, aerial photogrammetry (based on airplane and RPAS) and ground-penetrating radar. Airborne laser scanning data and aerial orthoimages acquired by the Czech Office for Surveying, Mapping and Cadastre were used. Other measurements were conducted by our laboratory. Data acquired by various methods provide sufficient information to determine the probable original shape of the formation and proves explicitly the anthropological origin of the northern part of the formation (around village Lipany).

  16. 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.

  17. 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.)

  18. Creating Magic Squares.

    ERIC Educational Resources Information Center

    Lyon, Betty Clayton

    1990-01-01

    One method of making magic squares using a prolongated square is illustrated. Discussed are third-order magic squares, fractional magic squares, fifth-order magic squares, decimal magic squares, and even magic squares. (CW)

  19. 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).

  20. 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

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  2. Non-destructive evaluation of TBC by electrochemical impedance spectroscopy

    NASA Astrophysics Data System (ADS)

    Zhang, Jianqi

    suggested. An alternative electrolyte (trifluoroacetic acid) was investigated using EIS in order to be used as compatible or friendly solution to TBC. A similar characteristic EIS result was found using the alternative electrolyte compared with the commonly used electrolyte [Fe(CN)6]-3/[Fe(CN) 6]-4 in this work. It has indicated that a friendly electrolyte be viable for EIS technique to be used for non-destructive evaluation of TBC. Visualization of a flexible probe for EIS field detection has also been designed. (Abstract shortened by UMI.)

  3. 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.

  4. A Novel High-Resolution and Sensitivity-Enhanced Three-Dimensional Solid-State NMR Experiment Under Ultrafast Magic Angle Spinning Conditions.

    PubMed

    Zhang, Rongchun; Pandey, Manoj Kumar; Nishiyama, Yusuke; Ramamoorthy, Ayyalusamy

    2015-01-01

    Although magic angle spinning (MAS) solid-state NMR is a powerful technique to obtain atomic-resolution insights into the structure and dynamics of a variety of chemical and biological solids, poor sensitivity has severely limited its applications. In this study, we demonstrate an approach that suitably combines proton-detection, ultrafast-MAS and multiple frequency dimensions to overcome this limitation. With the utilization of proton-proton dipolar recoupling and double quantum (DQ) coherence excitation/reconversion radio-frequency pulses, very high-resolution proton-based 3D NMR spectra that correlate single-quantum (SQ), DQ and SQ coherences of biological solids have been obtained successfully for the first time. The proposed technique requires a very small amount of sample and does not need multiple radio-frequency (RF) channels. It also reveals information about the proximity between a spin and a certain other dipolar-coupled pair of spins in addition to regular SQ/DQ and SQ/SQ correlations. Although (1)H spectral resolution is still limited for densely proton-coupled systems, the 3D technique is valuable to study dilute proton systems, such as zeolites, small molecules, or deuterated samples. We also believe that this new methodology will aid in the design of a plethora of multidimensional NMR techniques and enable high-throughput investigation of an exciting class of solids at atomic-level resolution. PMID:26138791

  5. 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.

  6. 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.

  7. 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. PMID:27088924

  8. Quantification of microheterogeneity in glioblastoma multiforme with ex vivo high-resolution magic-angle spinning (HRMAS) proton magnetic resonance spectroscopy.

    PubMed Central

    Cheng, L. L.; Anthony, D. C.; Comite, A. R.; Black, P. M.; Tzika, A. A.; Gonzalez, R. G.

    2000-01-01

    Microheterogeneity is a routinely observed neuropathologic characteristic in brain tumor pathology. Although microheterogeneity is readily documented by routine histologic techniques, these techniques only measure tumor status at the time of biopsy or surgery and do not indicate likely tumor progression. A biochemical screening technique calibrated against pathologic standards would greatly assist in predicting tumor progression from its biological activity. Here we demonstrate for the first time that proton magnetic resonance spectroscopy (1H MRS) with high-resolution magic-angle spinning (HRMAS), a technique introduced in 1997, can preserve tissue histopathologic features while producing well-resolved spectra of cellular metabolites in the identical intact tissue specimens. Observed biochemical alterations and tumor histopathologic characteristics can thus be correlated for the same surgical specimen, obviating the problems caused by tumor microheterogeneity. We analyzed multiple specimens of a single human glioblastoma multiforme surgically removed from a 44-year-old patient. Each specimen was first measured with HRMAS 1H MRS to determine tumor metabolites, then evaluated by quantitative histopathology. The concentrations of lactate and mobile lipids measured with HRMAS linearly reflected the percentage of tumor necrosis. Moreover, metabolic ratios of phosphorylcholine to choline correlated linearly with the percentage of the highly cellular malignant glioma. The quantification of tumor metabolic changes with HRMAS 1H MRS, in conjunction with subsequent histopathology of the same tumor specimen, has the potential to further our knowledge of the biochemistry of tumor heterogeneity during development, and thus ultimately to improve our accuracy in diagnosing, characterizing, and evaluating tumor progression. PMID:11303625

  9. 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. PMID:26604305

  10. Proton-detected solid-state NMR spectroscopy of fully protonated proteins at slow to moderate magic-angle spinning frequencies

    NASA Astrophysics Data System (ADS)

    Mote, Kaustubh R.; Madhu, Perunthiruthy K.

    2015-12-01

    1H -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 1H -1H dipolar coupled network that would otherwise severely broaden resonances, high MAS frequencies (>40 kHz) are often employed. Here, we have explored the alternative of stroboscopic 1H -detection at moderate MAS frequencies of 5-30 kHz using windowed version of supercycled-phase-modulated Lee-Goldburg homonuclear decoupling. We show that improved resolution in the 1H dimension, comparable to that obtainable at high spinning frequencies of 40-60 kHz 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 13C -detection based methods in assignments and characterization through chemical-shift mapping.

  11. Multidimensional High-Resolution Magic Angle Spinning and Solution-State NMR Characterization of (13)C-labeled Plant Metabolites and Lignocellulose.

    PubMed

    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 (13)C-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 (13)C-poplar were measured by high-resolution magic angle spinning NMR spectroscopy, which allows sample analysis without solvent extraction, while lignocellulose components of the (13)C-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 (13)C-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

  12. 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

  13. Recoupling of native homonuclear dipolar couplings in magic-angle-spinning solid-state NMR by the double-oscillating field technique

    NASA Astrophysics Data System (ADS)

    Straasø, Lasse Arnt; Nielsen, Niels Chr.

    2010-08-01

    A new solid-state NMR method, the double-oscillating field technique (DUO), that under magic-angle-spinning conditions produces an effective Hamiltonian proportional to the native high-field homonuclear dipole-dipole coupling operator is presented. The method exploits one part of the radio frequency (rf) field to recouple the dipolar coupling interaction with a relatively high scaling factor and to eliminate offset effects over a reasonable bandwidth while in the recoupling frame, the other part gives rise to a sufficiently large longitudinal component of the residual rf field that averages nonsecular terms and in addition ensures stability toward rf inhomogeneity and rf miscalibration. The capability of the DUO experiment to mediate transfer of polarization is described theoretically and compared numerically and experimentally with finite pulse rf driven recoupling and experimentally with dipolar-assisted rotational resonance. Two-dimensional recoupling experiments were performed on antiparallel amyloid fibrils of the decapeptide SNNFGAILSS with the FGAIL fragment uniformly labeled with C13 and N15.

  14. Trifluoroethanol and 19F magic angle spinning nuclear magnetic resonance as a basic surface hydroxyl reactivity probe for zirconium(IV) hydroxide structures.

    PubMed

    DeCoste, Jared B; Glover, T Grant; Mogilevsky, Gregory; Peterson, Gregory W; Wagner, George W

    2011-08-01

    A novel technique for determining the relative accessibility and reactivity of basic surface hydroxyl sites by reacting various zirconium(IV) hydroxide materials with 2,2,2-trifluoroethanol (TFE) and characterizing the resulting material using (19)F magic angle spinning (MAS) nuclear magnetic resonance (NMR) is presented here. Studied here are three zirconium hydroxide samples, two unperturbed commercial materials, and one commercial material that is crushed by a pellet press. Factors, such as the ratio of bridging/terminal hydroxyls, surface area, and pore size distribution, are examined and found to affect the ability of the zirconium(IV) hydroxide to react with TFE. X-ray diffraction, nitrogen isotherms, and (1)H MAS NMR were used to characterize the unperturbed materials, while thermogravitric analysis with gas chromatography and mass spectrometry along with the (19)F MAS NMR were used to characterize the materials that were reacted with TFE. Zirconium hydroxide materials with a high surface area and a low bridging/terminal hydroxyl ratio were found to react TFE in the greatest amounts. PMID:21699226

  15. 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.

  16. Systematic evaluation of heteronuclear spin decoupling in solid-state NMR at the rotary-resonance conditions in the regime of fast magic-angle spinning.

    PubMed

    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 rCW(ApA), 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 40kHz) 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 (1)H irradiation of ca.195kHz. PMID:27472380

  17. Cross-Correlated Relaxation of Dipolar Coupling and Chemical-Shift Anisotropy in Magic-Angle Spinning R1ρ NMR Measurements: Application to Protein Backbone Dynamics Measurements.

    PubMed

    Kurauskas, Vilius; Weber, Emmanuelle; Hessel, Audrey; Ayala, Isabel; Marion, Dominique; Schanda, Paul

    2016-09-01

    Transverse relaxation rate measurements in magic-angle spinning solid-state nuclear magnetic resonance provide information about molecular motions occurring on nanosecond-to-millisecond (ns-ms) time scales. The measurement of heteronuclear ((13)C, (15)N) relaxation rate constants in the presence of a spin-lock radiofrequency field (R1ρ relaxation) provides access to such motions, and an increasing number of studies involving R1ρ relaxation in proteins have been reported. However, two factors that influence the observed relaxation rate constants have so far been neglected, namely, (1) the role of CSA/dipolar cross-correlated relaxation (CCR) and (2) the impact of fast proton spin flips (i.e., proton spin diffusion and relaxation). We show that CSA/D CCR in R1ρ experiments is measurable and that the CCR rate constant depends on ns-ms motions; it can thus provide insight into dynamics. We find that proton spin diffusion attenuates this CCR due to its decoupling effect on the doublet components. For measurements of dynamics, the use of R1ρ rate constants has practical advantages over the use of CCR rates, and this article reveals factors that have so far been disregarded and which are important for accurate measurements and interpretation. PMID:27500976

  18. 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.

  19. Cross-polarization magic-angle spinning nuclear magnetic resonance study of platinum complexes containing the cis-P2PtC2 fragment.

    PubMed

    Challoner, R; Sebald, A

    1995-01-01

    31P and 195Pt cross-polarization magic-angle spinning nuclear magnetic resonance (CP-MAS NMR) spectra of three platinum complexes of formal oxidation state Pt(0) and Pt(II), respectively, are reported. All three complexes, (Ph3P)2Pt(C2H4) (1), (Et2P-CH2-CH2-PEt2)Pt(C identical to C-H)2 (2) and (Ph2P-CH2-CH2-PPh2)Pt(C identical to C-C(CH3)=CH2)2 (3) contain the square-planar cis-P2PtC2 fragment and show unusual NMR spectroscopic properties insofar that the 195Pt shielding patterns are fairly narrow in relation to what one would generally have to expect for 195Pt in square-planar coordination. Another unexpected NMR property of the cis-P2PtC2 fragment in 1-3 is the absence of spinning frequency-dependent second-order effects in this solid-state ABX spin system. PMID:7894980

  20. Recoupling of chemical shift anisotropies in solid-state NMR under high-speed magic-angle spinning and in uniformly 13C-labeled systems

    NASA Astrophysics Data System (ADS)

    Chan, Jerry C. C.; Tycko, Robert

    2003-05-01

    We demonstrate the possibility of recoupling chemical shift anisotropy (CSA) interactions in solid-state nuclear magnetic resonance (NMR) under high-speed magic-angle spinning (MAS) while retaining a static CSA powder pattern line shape and simultaneously attenuating homonuclear dipole-dipole interactions. CSA recoupling is accomplished by a rotation-synchronized radio-frequency pulse sequence with symmetry properties that permit static CSA line shapes to be obtained. We suggest a specific recoupling sequence, which we call ROCSA, for which the scaling factors for CSA and homonuclear dipole-dipole interactions are 0.272 and approximately 0.05, respectively. This sequence is suitable for high-speed 13C MAS NMR experiments on uniformly 13C-labeled organic compounds, including biopolymers. We demonstrate the ROCSA sequence experimentally by measuring the 13C CSA patterns of the uniformly labeled, polycrystalline compounds L-alanine and N-acetyl-D,L-valine at MAS frequencies of 11 and 20 kHz. We also present experimental data for amyloid fibrils formed by a 15-residue fragment of the β-amyloid peptide associated with Alzheimer's disease, in which four amino acid residues are uniformly labeled, demonstrating the applicability to biochemical systems of high molecular weight and significant complexity. Analysis of the CSA patterns in the amyloid fibril sample demonstrates the utility of ROCSA measurements as probes of peptide and protein conformation in noncrystalline solids.

  1. High-resolution 1H NMR in solids with multiple-pulse sequences and magic-angle sample spinning at 270 MHz

    NASA Astrophysics Data System (ADS)

    Scheler, G.; Haubenreisser, U.; Rosenberger, H.

    A probe suitable for 270-MHz 1H NMR in solids is described, using the combination of the phase-error-compensated WAHUHA multiple-pulse cycle and magic-angle sample spinning (MAS). The experimental results obtained at this frequency are compared with measurements at 60 MHz. Because of the increase of frequency the spectral resolution is improved by a factor of about 5. For a variety of organic and inorganic substances the resolution varies from 0.3 ppm in polycrystalline adamantane to about 2 ppm, sufficient to resolve resonance signals of protons of different molecular groups, such as NH 3, NH 4, olefinic, aromatic, and aliphatic protons. Averaged chemical shifts of a series of selected hydrogen-bonded powder samples are discussed. The residual linewidths were found to be due predominantly to second-order residual dipolar broadening, the cross term between resonance offset and dipolar interaction, nonresolved chemical shifts, and interactions of protons with nuclei which have a strong quadrupolar moment. The resolution is expected to be increased by combining the high-field MAS experiments and more effective multiple-pulse sequences, e.g., the 24-pulse cycle developed recently by Burum and Rhim.

  2. High-Speed Magic-Angle Spinning 13C MAS NMR Spectra of Adamantane: Self-Decoupling of the Heteronuclear Scalar Interaction and Proton Spin Diffusion

    NASA Astrophysics Data System (ADS)

    Ernst, Matthias; Verhoeven, Aswin; Meier, Beat H.

    1998-02-01

    We have investigated the carbon line shape of solid adamantane under high-speed magic-angle sample spinning (MAS) acquired without proton decoupling. The CH-group shows a spinning-speed-dependent line broadening while the CH2-group consists of a spinning-speed-independent sharp component and a spinning-speed-dependent broader part. These phenomena can be explained by self-decoupling of theJ-interaction due to proton spin diffusion. Such a self-decoupling process can be described by a magnetization exchange process between the multiplet lines. Changing the spin-diffusion rate constant by off-resonance irradiation of the protons allows us to observe the full range from slow exchange to coalescence to fast exchange of the carbon spectra. One of the multiplet components in the CH2-group corresponds to a group spin of the protons of zero and therefore does not couple to the other protons. This gives rise to the sharp central line. The magnetization exchange rate constant between the different multiplet lines can be determined from the spectra and is a measure for the spinning-speed-dependent proton spin-diffusion rate constant. Even at an MAS speed of 30 kHz, proton spin diffusion is still observable despite the relatively weak intermolecular proton dipolar-coupling network in adamantane which results in a static proton line width of only 14 kHz (full width at half height).

  3. 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

  4. A Monte Carlo/Simulated Annealing Algorithm for Sequential Resonance Assignment in Solid State NMR of Uniformly Labeled Proteins with Magic-Angle Spinning

    PubMed Central

    Tycko, Robert; Hu, Kan-Nian

    2010-01-01

    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/13Cα 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. Biomolec. NMR, vol. 34, pp. 75-87, 2006) 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. PMID:20547467

  5. Structure of (NH4)3GaF6 investigated by multinuclear magic-angle spinning NMR spectroscopy in comparison with rietveld refinement.

    PubMed

    Krahl, Thoralf; Ahrens, Mike; Scholz, Gudrun; Heidemann, Detlef; Kemnitz, Erhard

    2008-01-21

    The structure of ammonium gallium cryolite (NH(4))(3)GaF(6) was investigated by (19)F and (69,71)Ga magic-angle spinning (MAS) NMR in comparison with X-ray powder diffraction followed by Rietveld refinement. In agreement with previous thermodynamic measurements, NMR experiments on (NH(4))(3)GaF(6) support the model of rigid GaF(6) octahedra. At high spinning speeds (30 kHz), the scalar coupling between the six equivalent (19)F nuclei and (69,71)Ga can be directly observed in the powder spectra. The coupling constants are J(19)F(69)Ga = 197 Hz and J(19)F(71)Ga = 264 Hz. To explain the (71)Ga spectra recorded at 3 kHz a small distribution of quadrupolar frequencies has to be included. The spread of the spinning sidebands hints to a largest nu(Q) value of 28 kHz for (71)Ga. This can be explained by the occurrence of highly symmetric GaF(6) octahedra, which are tilted against the surrounding atoms. In addition, the incomplete motional excitation does not average out the quadrupolar effects. NMR findings are in discrepancy to those of Rietveld refinement. As result it appears that X-ray diffraction is not sensitive enough to deliver proper results. PMID:18069821

  6. 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

  7. 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

  8. 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. PMID:22938251

  9. 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

  10. The molecular origin of a loading-induced black layer in the deep region of articular cartilage at the magic angle

    PubMed Central

    Wang, Nian; Kahn, David; Badar, Farid; Xia, Yang

    2014-01-01

    Purpose To investigate the molecular origin of an unusual low-intensity layer in the deep region of articular cartilage as seen in MRI when the tissue is imaged under compression and oriented at the magic angle. Materials and Methods Microscopic MRI (μMRI) T2 and T1ρ experiments were carried out for both native and degraded (treated with trypsin) 18 specimens. The glycosaminoglycan (GAG) concentrations in the specimens were quantified by both sodium ICP-OES and μMRI Gd(DTPA)2--contrast methods. The mechanical modulus of the specimens was also measured. Results Native tissue shows no load-induced layer, while the trypsin-degraded tissue shows clearly the low-intensity line at the deep part of tissue. The GAG reductions are confirmed by the sodium ICP-OES (from 81.7 ± 5.4 mg/ml to 9.2 ± 3.4 mg/ml), MRI GAG quantification (from 72.4 ± 6.7 mg/ml to 11.2 ± 2.9 mg/ml). The modulus reduction is confirmed by biomechanics (from 4.3 ± 0.7 MPa to 0.3 ± 0.1 MPa). Conclusion Both T2 and T1ρ profiles in native and degraded cartilage show strongly strain-, depth-, and angle-dependent using high resolution MRI. The GAG reduction is responsible for the visualization of a low-intensity layer in deep cartilage when it is loaded and orientated at 55°. PMID:24833266

  11. 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.

  12. 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. PMID:26323547

  13. 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.

  14. 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.

  15. Menu Magic!

    ERIC Educational Resources Information Center

    Smith, Susan H.; Hickey, Bethany

    2003-01-01

    Describes the activity "Menu Magic!" that helps eighth graders review the power of adjectives. Notes that students "eat up this project" that promises to deliver the opportunity to analyze, synthesize, and evaluate while giving students the chance to work in cooperative groups. Describes and gives examples of the "Menu Magic" project. (SG)

  16. A High-Resolution 3D Separated-Local-Field Experiment by Means of Magic-Angle Turning

    PubMed

    Hu; Alderman; Pugmire; Grant

    1997-05-01

    A 3D separated-local-field (SLF) experiment based on the 2D PHORMAT technique is described. In the 3D experiment, the conventional 2D SLF powder pattern for each chemically inequivalent carbon is separated according to their different isotropic chemical shifts. The dipolar coupling constant of a C-H pair, hence the bond distance, and the relative orientation of the chemical-shift tensor to the C-H vector can all be determined for the protonated carbons with a single measurement. As the sample turns at only about 30 Hz in a MAT experiment, the SLF patterns obtained approach those of a stationary sample, and an accuracy in the measurement similar to that obtained on a stationary sample is expected. The technique is demonstrated on 2,6-dimethoxynaphthalene, where the 13 C-1 H separated-local-field powder patterns for the six chemically inequivalent carbons are clearly identified and measured. The observed dipolar coupling for the methoxy carbon is effectively reduced by the fast rotation of the group about its C3 symmetry axis. The average angle between the C-H bond direction and the C3 rotation axis in the OCH3 group is found to be about 66°. PMID:9252281

  17. Characterization of high-tannin fractions from humus by carbon-13 cross-polarization and magic-angle spinning nuclear magnetic resonance.

    PubMed

    Lorenz, Klaus; Preston, Caroline M

    2002-01-01

    Condensed tannins can be found in various parts of many plants. Unlike lignin there has been little study of their fate as they enter the soil organic matter pool and their influence on nutrient cycling, especially through their protein-binding properties. We extracted and characterized tannin-rich fractions from humus collected in 1998 from a black spruce [Picea mariana (Mill.) Britton et al.] forest in Canada where a previous study (1995) showed high levels (3.8% by weight) of condensed tannins. A reference tannin purified from black spruce needles was characterized by solution 13C nuclear magnetic resonance (NMR) as a pure procyanidin with mainly cis stereochemistry and an average chain length of four to five units. The colorimetric proanthocyanidin (PA) assay, standardized against the black spruce tannin, showed that both extracted humus fractions had higher tannin contents than the original humus (2.84% and 11.17% vs. 0.08%), and accounted for 32% of humus tannin content. Consistent with the results from the chemical assay, the aqueous fraction showed higher tannin signals in the 13C cross-polarization and magic-angle spinning (CPMAS) NMR spectrum than the emulsified one. As both tannin-rich humus fractions were depleted in N and high in structures derived from lignin and cutin, they did not have properties consistent with recaldtrant tannin-protein complexes proposed as a mechanism for N sequestration in humus. Further studies are needed to establish if tannin-protein structures in humus can be detected or isolated, or if tannins contribute to forest management problems observed in these ecosystems by binding to and slowing down the activity of soil enzymes. PMID:11931430

  18. 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

  19. 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. PMID:26203019

  20. 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. PMID:25338744

  1. 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.

  2. 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.

  3. 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.

  4. Assessment of a 1H high-resolution magic angle spinning NMR spectroscopy procedure for free sugars quantification in intact plant tissue.

    PubMed

    Delgado-Goñi, Teresa; Campo, Sonia; Martín-Sitjar, Juana; Cabañas, Miquel E; San Segundo, Blanca; Arús, Carles

    2013-08-01

    In most plants, sucrose is the primary product of photosynthesis, the transport form of assimilated carbon, and also one of the main factors determining sweetness in fresh fruits. Traditional methods for sugar quantification (mainly sucrose, glucose and fructose) require obtaining crude plant extracts, which sometimes involve substantial sample manipulation, making the process time-consuming and increasing the risk of sample degradation. Here, we describe and validate a fast method to determine sugar content in intact plant tissue by using high-resolution magic angle spinning nuclear magnetic resonance spectroscopy (HR-MAS NMR). The HR-MAS NMR method was used for quantifying sucrose, glucose and fructose in mesocarp tissues from melon fruits (Cucumis melo var. reticulatus and Cucumis melo var. cantalupensis). The resulting sugar content varied among individual melons, ranging from 1.4 to 7.3 g of sucrose, 0.4-2.5 g of glucose; and 0.73-2.83 g of fructose (values per 100 g fw). These values were in agreement with those described in the literature for melon fruit tissue, and no significant differences were found when comparing them with those obtained using the traditional, enzymatic procedure, on melon tissue extracts. The HR-MAS NMR method offers a fast (usually <30 min) and sensitive method for sugar quantification in intact plant tissues, it requires a small amount of tissue (typically 50 mg fw) and avoids the interferences and risks associated with obtaining plant extracts. Furthermore, this method might also allow the quantification of additional metabolites detectable in the plant tissue NMR spectrum. PMID:23824526

  5. High-resolution magic angle spinning and 1H magnetic resonance spectroscopy reveal significantly altered neuronal metabolite profiles in CLN1 but not in CLN3.

    PubMed

    Sitter, Beathe; Autti, Taina; Tyynelä, Jaana; Sonnewald, Ursula; Bathen, Tone F; Puranen, Johanna; Santavuori, Pirkko; Haltia, Matti J; Paetau, Anders; Polvikoski, Tuomo; Gribbestad, Ingrid S; Häkkinen, Anna-Maija

    2004-09-01

    The neuronal ceroid lipofuscinoses (NCLs) are among the most severe inherited progressive neurodegenerative disorders of children. The purpose of this study was to compare the in vivo 1.5-T 1H magnetic resonance (MR) and ex vivo 14.3-T high-resolution (HR) magic angle spinning (MAS) 1H MR brain spectra of patients with infantile (CLN1) and juvenile (CLN3) types of NCL, to obtain detailed information about the alterations in the neuronal metabolite profiles in these diseases and to test the suitability of the ex vivo HR MAS (1)H MRS technique in analysis of autopsy brain tissue. Ex vivo spectra from CLN1 autopsy brain tissue (n = 9) significantly differed from those of the control (n = 9) and CLN3 (n = 5) groups, although no differences were found between the CLN3 and the control groups. Principal component analysis of ex vivo data showed that decreased levels of N-acetylaspartate (NAA), gamma-aminobutyric acid (GABA), glutamine, and glutamate as well as increased levels of inositols characterized the CLN1 spectra. Also, the intensity ratio of lipid methylene/methyl protons was decreased in spectra of CLN1 brain tissue compared with CLN3 and control brain tissue. In concordance with the ex vivo data, the in vivo spectra of late-stage patients with CLN1 (n = 3) revealed a dramatic decrease of NAA and a proportional increase of myo-inositol and lipids compared with control subjects. Again, the spectra of patients with CLN3 (n = 13) did not differ from those of controls (n = 15). In conclusion, the ex vivo and in vivo spectroscopic findings were in good agreement within all analyzed groups and revealed significant alterations in metabolite profiles in CLN1 brain tissue but not in CLN3 compared with controls. Furthermore, HR MAS 1H MR spectra facilitated refined detection of neuronal metabolites, including GABA, and composition of lipids in the autopsy brain tissue of NCL patients. PMID:15352223

  6. 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. PMID:18498698

  7. Magic angle spinning nuclear magnetic resonance characterization of voltage-dependent anion channel gating in two-dimensional lipid crystalline bilayers.

    PubMed

    Eddy, Matthew T; Andreas, Loren; Teijido, Oscar; Su, Yongchao; Clark, Lindsay; Noskov, Sergei Y; Wagner, Gerhard; Rostovtseva, Tatiana K; Griffin, Robert G

    2015-02-01

    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 (13)C-(13)C 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 (13)C-(13)C 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

  8. Enhanced sensitivity and resolution in (1)H solid-state NMR spectroscopy of paramagnetic complexes under very fast magic angle spinning.

    PubMed

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

    2005-04-27

    High-resolution NMR spectroscopy for paramagnetic complexes in solids has been rarely performed because of its limited sensitivity and resolution due to large paramagnetic shifts and associated technical difficulties. The present study demonstrates that magic angle spinning (MAS) at speeds exceeding 20 kHz provides unusually high sensitivity and excellent resolution in 1H solid-state NMR (SSNMR) for paramagnetic systems. Spinning-speed dependence of 1H MAS spectra showed that very fast MAS (VFMAS) at 24-28 kHz enhanced sensitivity by a factor of 12-18, compared with the sensitivity of 1H SSNMR spectra under moderate MAS at 10 kHz, for Cu(dl-alanine)2.H2O and Mn(acac)3, for which the spectral ranges due to 1H paramagnetic shifts reach 200 and 1000 ppm, respectively. It was theoretically and experimentally confirmed that the absolute sensitivity of 1H VFMAS for small paramagnetic complexes such as Cu(dl-alanine)2 can be an order of magnitude higher than that of equimolar diamagnetic ligands because of short 1H T1 ( approximately 1 ms) of the paramagnetic systems and improved sensitivity under VFMAS. On the basis of this demonstrated high sensitivity, 1H SSNMR micro analysis of paramagnetic systems in a nanomole scale is proposed. Applications were performed on two polymorphs of Cu(II)(8-quinolinol)2, which is a suppressor of human cancer cells. It was demonstrated that 1H VFMAS SSNMR spectra accumulated for 20 nmol of the polycrystalline samples in 10 min enabled one to distinguish alpha- and beta-forms of Cu(II)(8-quinolinol)2 on the basis of shift positions and line widths. PMID:15839671

  9. Application of the Floquet theory to multiple quantum NMR of dipolar-coupled multi-spin systems under magic angle spinning

    NASA Astrophysics Data System (ADS)

    Filip, Claudiu; Bertmer, Marko; Demco, Dan E.; Blümich, Bernhard

    A new analytical Liouville-space representation of the time-propagator under magic angle spinning (MAS) is introduced using the formalized quantum Floquet theory. This approach has the advantage that it is applicable to the analysis of any type of NMR experiment where MAS is combined with multiple-pulse excitation. General relationships describing the spectral parameters in multiple-quantum (MQ) MAS spectra are derived in this representation. Their use is illustrated with an application to double-quantum (DQ) NMR spectra of dipolarcoupled multi-spin systems. Corresponding to the separation of the MAS time-propagator into a rotor modulated and a dephasing component, two distinct mechanisms for DQ excitation are identified. One of them exploits the rotor-modulated component to excite DQ coherences through dipolar-recoupling techniques, which are familiar for spin pairs. Analytical expressions of the integral intensities and linewidths in the resulting DQ sideband pattern are derived in the form of power series expansions of the inverse rotor frequency, of which coefficients depend on structural parameters. In a multi-spin system they can most reliably be extracted in the fast spinning regime. The other mechanism exploits the dephasing component, which is characteristic to multi-spin systems only. This is shown to give rise to DQ coherences by free evolution at full rotor periods. The possibility to exploit it for selective excitation of higher order MQ coherences is discussed. In either case, the dephasing component also leads to residual broadening. The main results of the theoretical developments are demonstrated experimentally on adamantane.

  10. Magic-angle spinning NMR study of deuterium site occupancy and dynamics in ZrNiD1.0 and ZrNiD3.0

    NASA Astrophysics Data System (ADS)

    Adolphi, Natalie L.; Badola, Sharwari; Browder, Lisa A.; Bowman, R. C.

    2002-01-01

    Both static and magic-angle spinning (MAS) 2H nuclear magnetic resonance spectroscopy indicate that two inequivalent sites are occupied in ZrNiD3.0, in a 2:1 ratio, in agreement with previous work. The sites occupied in the trihydride phase have been previously identified as Zr3Ni and Zr3Ni2. In ZrNiD1.0, two well-resolved lines of equal intensity are observed in the MAS spectrum at temperatures<220 K, indicating that two other inequivalent sites are occupied in a 1:1 ratio, in contrast with previous reports that only one type of site (Zr4Ni2) is occupied in the monohydride (β) phase at room temperature and above. The temperature dependences of both MAS and static ZrNiD1.0 spectra indicate that no phase transitions occur over the entire temperature range studied, 160-500 K. The deuterium hopping rate in ZrNiD1.0 is determined from characteristic changes in the MAS spectra as a function of temperature; the motion is consistent with an activation energy Ea≅0.44 eV assuming a rate prefactor 1/τ0~1013 s-1. In ZrNiD3.0, the rate of deuterium motion is determined from signatures of motion in the static and MAS spectra. The motion in ZrNiD3.0 is consistent with an activation energy Ea≅0.62 eV assuming a rate prefactor of ~1013 s-1.

  11. 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 .

  12. High-resolution aluminum-27 solid-state magic-angle sample-spinning nuclear magnetic resonance spectroscopic study of AlCl sub 3 -tetrahydrofuran complexes

    SciTech Connect

    Han, Oc Hee; Oldfield, E. )

    1990-09-19

    The authors have obtained {sup 27}Al solid-state nuclear magnetic resonance (NMR) spectra of several AlCl{sub 3}-THF complexes, using magic-angle sample-spinning (MASS) NMR at high field. The authors results suggest that the isotropic chemical shifts ({delta}{sub i}) occur in relatively well defined regions for 4-, 5-, and 6-coordinate species (AlCl{sub 4}{sup {minus}}, {approximately} 103 ppm; AlCl{sub 3}{center dot}THF, {approximately} 99 ppm; trans-AlCl{sub 3}{center dot}2THF, {approximately} 60 ppM; trans-(AlCl{sub 2}(THF){sub 4}){sup +}, {approximately} 14 ppM), as found previously with aluminum oxo compounds. They also find that theoretically calculated average nuclear quadrupole coupling constants (e{sup 2}qQ/h) (trans-(AlCl{sub 2}(THF){sub 4}){sup +}, {approximately} 6.3 MHz; trans-AlCl{sub 3}{center dot}2THF, {approximately} 4.6 MHz; AlCl{sub 3}{center dot}THF, {approximately} 3.0 MHz; AlCl{sub 4}{sup {minus}}, 0 MHz) are in good accord with experimentally determined nuclear quadrupole coupling constants, determined from computer simulations of the MASS NMR spectra (trans-(AlCl{sub 2}(THF){sub 4}){sup +}, 6.4 MHz; trans-AlCl{sub 3}{center dot}2THF, 4.9 MHz; AlCl{sub 3}{center dot}THF, 4.7 MHz; AlCl{sub 4}{sup {minus}}, 0.3 MHz). Both {sup 27}Al {delta}{sub i} and e{sup 2}qQ/h determinations appear to be useful as probes of structure in these systems, and thus offer a facile means of monitoring various solid-state reactions. 14 refs., 3 figs., 3 tabs.

  13. 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.

  14. Non-destructive characterization of superionic conductor: lithium nitride

    NASA Astrophysics Data System (ADS)

    Yadawa, Pramod Kumar

    2014-12-01

    Higher order elastic constants have been calculated in hexagonally structured superionic conductor Li3N at room temperature using the interaction potential model. The temperature variation of the ultrasonic velocities was evaluated along different angles with z axis (unique axis) of the crystal, using the second order elastic constants. The ultrasonic velocity decreased with the temperature along a particular orientation of the unique axis. Temperature variation of the thermal relaxation time and Debye average velocities was also calculated along the same orientation. The temperature dependency of ultrasonic properties was discussed in correlation with elastic, thermal and electrical properties. It has been found that the thermal conductivity is the main contributor to the behavior of ultrasonic attenuation as a function of temperature and the cause responsible for attenuation is phonon-phonon interaction. The mechanical properties of Li3N at low temperature are better than at high temperature because at low temperature it has low ultrasonic attenuation. Superionic conductor lithium nitride has many industrial applications, such as those used in portable electronic devices.

  15. Non-destructive Measurement of Residual Stress Depth Profile in Laser-peened Steel at SPring-8

    SciTech Connect

    Sato, Masugu; Kajiwara, Kentaro; Sano, Yuji; Tanaka, Hirotomo; Akita, Koichi

    2007-01-19

    We investigated the residual stress depth profile near the surface of steel treated by laser peening without coating using X-ray diffraction at SPring-8. This investigation was carried out using a constant penetration depth sin2{psi} method. In this method, the sin2{psi} diagram is measured controlling both the {psi} angle and the X-ray penetration depth simultaneously with a combination of the {omega} and {chi} axes of the 4-circle goniometer. This method makes it possible to evaluate the residual stress and its depth profile in material with a stress gradient precisely and non-destructively. As a result, we confirmed that a compressive residual stress was successfully formed all over the range of the depth profile in the steel treated properly by laser peening without coating.

  16. Non-destructive Measurement of Residual Stress Depth Profile in Laser-peened Steel at SPring-8

    NASA Astrophysics Data System (ADS)

    Sato, Masugu; Sano, Yuji; Kajiwara, Kentaro; Tanaka, Hirotomo; Akita, Koichi

    2007-01-01

    We investigated the residual stress depth profile near the surface of steel treated by laser peening without coating using X-ray diffraction at SPring-8. This investigation was carried out using a constant penetration depth sin2ψ method. In this method, the sin2ψ diagram is measured controlling both the ψ angle and the X-ray penetration depth simultaneously with a combination of the ω and χ axes of the 4-circle goniometer. This method makes it possible to evaluate the residual stress and its depth profile in material with a stress gradient precisely and non-destructively. As a result, we confirmed that a compressive residual stress was successfully formed all over the range of the depth profile in the steel treated properly by laser peening without coating.

  17. Comparisons of lipid dynamics and packing in fully interdigitated monoarachidoylphosphatidylcholine and non-interdigitated dipalmitoylphosphatidylcholine bilayers: cross polarization/magic angle spinning 13C-NMR studies.

    PubMed

    Wu, W G; Chi, L M

    1990-07-24

    13C-NMR spectra have been obtained at 50.3 MHz for monoarachidoylphosphatidylcholine (MAPC) and dipalmitoylphosphatidylcholine (DPPC) dispersions from 25 degrees C to 55 degrees C and for DPPC polycrystals at 25 degrees C using the cross polarization/magic angle spinning technique. Differential scanning calorimetric studies on DPPC and MAPC dispersions show comparable lipid phase transitions with transition temperatures at 41 degrees C and 45 degrees C, respectively, and thus enable the comparison of thermal, structural and dynamic differences between these two systems at corresponding temperatures. Conformational-dependent 13C chemical shift studies on DPPC dispersions demonstrate not only the coexistence of the tilted gel (L beta') and liquid-crystalline (L alpha) phases in the rippled gel (P beta') phase, but also the presence of an intermediate third microscopic phase as evidenced by three resolvable peaks for omega - 1 methylene carbon signals at the temperature interval between Tp and Tm. By comparing chemical shifts of MAPC in the hydrocarbon chain region with those of DPPC at similar reduced temperatures, it can be concluded that the packings are perturbed markedly in the middle segment of the fatty acyl chain during the lamellar to micellar transition. However, terminal methylene and methyl groups of interdigitated MAPC lamellae were found to be more ordered than those of non-interdigitated DPPC bilayers in the gel state. Interestingly, the terminal methyl groups of MAPC in the micelles remain to be relatively ordered; in fact, they are more ordered than the corresponding acyl chain end of DPPC in the liquid-crystalline state. Analysis of data obtained from rotating frame proton spin-lattice relaxation measurements shows a highly mobile phosphocholine headgroup, a rigid carbonyl group and an ordered hydrocarbon chain for lamellar MAPC in the interdigitated state. Furthermore, results suggest that free rotations of the glycerol C2-C3 bond within MAPC

  18. 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.

    PubMed

    Eliav, U; Haimovich, A; Goldbourt, A

    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 (7)Li-(13)C distances in a complex of lithium, glycine, and water. Discussion

  19. 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

  20. Sensitivity enhanced (14)N/(14)N correlations to probe inter-beta-sheet interactions using fast magic angle spinning solid-state NMR in biological solids.

    PubMed

    Pandey, Manoj Kumar; Amoureux, Jean-Paul; Asakura, Tetsuo; Nishiyama, Yusuke

    2016-08-10

    (14)N/(14)N correlations are vital for structural studies of solid samples, especially those in which (15)N isotopic enrichment is challenging, time-consuming and expensive. Although (14)N nuclei have high isotopic abundance (99.6%), there are inherent difficulties in observing (14)N/(14)N correlations due to limited resolution and sensitivity related to: (i) low (14)N gyromagnetic ratio (γ), (ii) large (14)N quadrupolar couplings, (iii) integer (14)N spin quantum number (I = 1), and (iv) very weak (14)N-(14)N dipolar couplings. Previously, we demonstrated a proton-detected 3D (14)N/(14)N/(1)H correlation experiment at fast magic angle spinning (MAS) on l-histidine·HCl·H2O utilizing a through-bond (J) and residual dipolar-splitting (RDS) based heteronuclear multiple quantum correlation (J-HMQC) sequence mediated through (1)H/(1)H radio-frequency driven recoupling (RFDR). As an extension of our previous work, in this study we show the utility of dipolar-based HMQC (D-HMQC) in combination with (1)H/(1)H RFDR mixing to obtain sensitivity enhanced (14)N/(14)N correlations in more complex biological solids such as a glycyl-l-alanine (Gly-l-Ala) dipeptide, and parallel (P) and antiparallel (AP) β-strand alanine tripeptides (P-(Ala)3 and AP-(Ala)3, respectively). These systems highlight the mandatory necessity of 3D (14)N/(14)N/(1)H measurements to get (14)N/(14)N correlations when the amide proton resonances are overlapped. Moreover, the application of long selective (14)N pulses, instead of short hard ones, is shown to improve the sensitivity. Globally, we demonstrate that replacing J-scalar with dipolar interaction and hard- with selective-(14)N pulses allows gaining a factor of ca. 360 in experimental time. On the basis of intermolecular NH/NH distances and (14)N quadrupolar tensor orientations, (14)N/(14)N correlations are effectively utilized to make a clear distinction between the parallel and antiparallel arrangements of the β-strands in (Ala)3 through the

  1. 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].

  2. Exploring the conformational energy landscape of glassy disaccharides by cross polarization magic angle spinning 13C nuclear magnetic resonance and numerical simulations. II. Enhanced molecular flexibility in amorphous trehalose

    NASA Astrophysics Data System (ADS)

    Lefort, Ronan; Bordat, Patrice; Cesaro, Attilio; Descamps, Marc

    2007-01-01

    This paper uses chemical shift surfaces to simulate experimental C13 cross polarization magic angle spinning spectra for amorphous solid state disaccharides, paying particular attention to the glycosidic linkage atoms in trehalose, sucrose, and lactose. The combination of molecular mechanics with density functional theory/gauge invariant atomic orbital ab initio methods provides reliable structural information on the conformational distribution in the glass. The results are interpreted in terms of an enhanced flexibility that trehalose possesses in the amorphous solid state, at least on the time scale of C13 nuclear magnetic resonance measurements. Implications of these findings for the fragility of trehalose glass and bioprotectant action are discussed.

  3. 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.

  4. Edward's sword? - A non-destructive study of a medieval king's sword

    NASA Astrophysics Data System (ADS)

    Segebade, Chr.

    2013-04-01

    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.

  5. Non destructive evaluation of adhesively bonded carbon fiber reinforced composite lap joints with varied bond quality

    NASA Astrophysics Data System (ADS)

    Vijayakumar, R. L.; Bhat, M. R.; Murthy, C. R. L.

    2012-05-01

    Structural adhesive bonding is widely used to execute assemblies in automobile and aerospace structures. The quality and reliability of these bonded joints must be ensured during service. In this context non destructive evaluation of these bonded structures play an important role. Evaluation of adhesively bonded composite single lap shear joints has been attempted through experimental approach. Series of tests, non-destructive as well as destructive were performed on different sets of carbon fiber reinforced polymer (CFRP) composite lap joint specimens with varied bond quality. Details of the experimental investigations carried out and the outcome are presented in this paper.

  6. Time Domain Terahertz Non-Destructive Evaluation of Aeroturbine Blade Thermal Barrier Coatings

    NASA Astrophysics Data System (ADS)

    White, Jeffrey; Fichter, G.; Chernovsky, A.; Whitaker, John F.; Das, D.; Pollock, Tresa M.; Zimdars, David

    2009-03-01

    Time domain terahertz (TD-THz) non destructive evaluation (NDE) imaging is used to two-dimensionally map the thickness of yttria stabilized zirconia (YSZ) thermal barrier coatings (TBC) on aircraft engine turbine blades. Indications of thermal degradation can be seen. The method is non-contact, rapid, and requires no special preparation of the blade.

  7. The non-destructive identification of early Chinese porcelain by PIXE

    NASA Astrophysics Data System (ADS)

    Cheng, H. S.; Zhang, Z. Q.; Zhang, B.; Yang, F. J.

    2004-06-01

    PIXE is used for the non-destructive differentiation of early precious Chinese blue and white porcelain made in Yuan (AD 1206-1368), Ming (AD 1368-1644) Dynasty in Jingdezhen from imitations. Also, ancient celadon made in Song Dynasty (AD 960-1279) is identified by measuring the trace elements contained in the glazes.

  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

    2015-03-01

    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. PMID:25589230

  9. 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.

  10. Rapid, Non-Destructive Estimation of Leaf Area on Field-Grown Vitis labruscana Grapevines

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Three potential variables, shoot basal diameter, leaf count per shoot and shoot length, were examined as potential rapid, non-destructive methods for estimating leaf area per shoot, a frequent component of estimates of leaf area per vine. The metrics were recorded in large field-grown vines over fi...

  11. Non-destructive freeze damage detection in oranges using machine vision and ultraviolet fluorescence

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A non-contact, non-destructive, and rapid method of detecting freeze damaged oranges based on ultraviolet (UV) fluorescence of the peel oil constituents visible on the peel surface was investigated. The visual appearance is different from oleocellosis in that freeze damaged oranges exhibit a fine pa...

  12. 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.

  13. Development of non-destructive inspection method for the performance of thermal barrier coating.

    PubMed

    Morinaga, M; Takahashi, T

    2001-05-01

    This paper shows that our proprietary non-destructive inspection method can be used to effectively measure the thermal barrier performance of the thermal barrier coating used to coat gas turbine hot parts by the results of numerical analysis and laboratory experiments. PMID:11460665

  14. 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…

  15. 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)

  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. 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)

  18. Light-driven supramolecular chiral materials: photoinduced control of liquid-crystalline helical structures and non-destructive erasable molecular memory for photonic applications

    NASA Astrophysics Data System (ADS)

    Kawamoto, Masuki; Shiga, Natsuki; Takaishi, Kazuto; Sassa, Takafumi; Yamashita, Takashi; Ito, Yoshihiro

    2013-09-01

    Light-driven supramolecular chiral materials containing an azobenzene moiety as a photoresponsive part and binaphthyl moiety as a chiral part were designed. We found that the dynamic molecular twisting motion of the binaphthyl moiety could be achieved by irradiation of UV or visible light to cause photoisomerization of the azobenzene moiety. The twisting motion induced by the photochromic reaction gave rise to large change in the molecular structure and the value of optical rotation. The chiral materials were demonstrated to behave uniquely as photomodulation of liquid-crystalline helical structures and non-destructive erasable chiroptical memory through photoinduced switching of the dihedral angle of the binaphthyl moiety.

  19. Quality parameters of mango and potential of non-destructive techniques for their measurement - a review.

    PubMed

    Jha, S N; Narsaiah, K; Sharma, A D; Singh, M; Bansal, S; Kumar, R

    2010-01-01

    The king of fruits "Mango" (Mangifera indica L.) is very nutritious and rich in carotenes. India produces about 50% of the total world's mango. Many researchers have reported the maturity indices and quality parameters for determination of harvesting time and eating quality. The methods currently used for determination of quality of mango are mostly based on the biochemical analysis, which leads to destruction of the fruits. Numerous works are being carried out to explore some non-destructive methods such as Near Infrared (NIR), Nuclear Magnetic Resonance (NMR), X-ray and Computed Tomography (CT), electronic nose, machine vision and ultrasound for quality determination of fruits. This paper deals with some recent work reported on quality parameters, harvesting and post-harvest treatments in relation to quality of mango fruits and reviews on some of the potential non-destructive techniques that can be explored for quality determination of mango cultivars. PMID:23572595

  20. 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.

  1. Non-destructive missile seeker flight testing: HWIL in the sky

    NASA Astrophysics Data System (ADS)

    Clements, Jim; Robinson, Joe; Robinson, Richard M.

    2010-04-01

    Surface to air missile development programs typically utilize hardware-in-the-loop (HWIL) simulations when available to provide a non-destructive high volume test environment for what are typically very expensive guidance sections. The HWIL, while invaluable, hasn't been able to obviate the need for missile flight tests. Because of the great expense of these missiles the designers are only allowed to perform a fraction of the desired tests. Missile Airframe Simulation Testbed (MAST) is a program conceived by US Army Aviation and Missile Research Development and Engineering Center (AMRDEC) that blends the non-destructive nature of HWIL with the confidence gained from flight tests to expand the knowledge gained while reducing the development schedule of new missile programs.

  2. 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.

  3. Non-destructive imaging of buried electronic interfaces using a decelerated scanning electron beam.

    PubMed

    Hirohata, Atsufumi; Yamamoto, Yasuaki; Murphy, Benedict A; Vick, Andrew J

    2016-01-01

    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

  4. Inhomogeneous light shift effects on atomic quantum state evolution in non-destructive measurements

    NASA Astrophysics Data System (ADS)

    Windpassinger, Patrick J.; Oblak, Daniel; Busk Hoff, Ulrich; Appel, Jürgen; Kjærgaard, Niels; Polzik, Eugene S.

    2008-05-01

    Various parameters of a trapped collection of cold and ultracold atoms can be determined non-destructively by measuring the phase shift of an off-resonant probe beam, caused by the state-dependent index of refraction of the atoms. The dispersive light-atom interaction, however, gives rise to a differential light shift (ac Stark shift) between the atomic states which, for a non-uniform probe intensity distribution, causes an inhomogeneous dephasing between the atoms. In this paper, we investigate the effects of this inhomogeneous light shift in non-destructive measurement schemes in cold caesium. We interpret our experimental data on dispersively probed Rabi oscillations and Ramsey fringes in terms of a simple light shift model which is shown to describe the observed behavior well. Furthermore, we show that by using spin echo techniques, the inhomogeneous phase shift distribution between the two clock levels can be reversed.

  5. Evaluation of Damage in Steels Subjected to Exploitation Loading - Destructive and Non-Destructive Methods

    NASA Astrophysics Data System (ADS)

    Kowalewski, Zbigniew L.; Mackiewicz, Sławomir; Szelążek, Jacek; Pietrzak, Krystyna; Augustyniak, Bolesław

    Damage due to creep and plastic flow is assessed using destructive and non-destructive methods in steels (40HNMA and P91). In the destructive methods the standard tension tests were carried out after prestraining and variations of the selected tension parameters were taken into account for damage identification. In order to assess a damage development during the creep and plastic deformation the tests for both steels were interrupted for a range of the selected strain magnitudes. The ultrasonic and magnetic techniques were used as the non-destructive methods for damage evaluation. The last step of the experimental programme contained microscopic observations. A very promising correlation between parameters of methods for damage development evaluation was achieved. It is well proved for the ultimate tensile stress and birefringence coefficient.

  6. 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.

  7. 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.

  8. 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.

  9. Non-destructive analysis in a study of the religious art objects

    NASA Astrophysics Data System (ADS)

    Vornicu, Nicoleta; Geba, Maria; Bibire, Cristina

    2009-08-01

    The icon Descending of the Saint Spirit from Bucium Church, dating in the year 1814 and was done in tempera on wood technology. The characterization of cultural heritage materials is essential for the comprehension of their degradation mechanisms. The present study aims at identifying the pigments in the various layers, establishing the possible existence of an organic binder and scientifically evaluating the state of preservation. To this end, were used non-destructive methods, as: microscopic (SEM), XRF and spectroscopic (FTIR).

  10. Rotational magnetic flux sensor with neural network for non-destructive testing

    SciTech Connect

    Enokizono, M.; Todaka, T.; Akita, M. . Faculty of Engineering); Nagata, S. . Faculty of Engineering)

    1993-11-01

    This paper presents a new non-destructive testing (NDT) method which utilizes rotational magnetic flux. In this system, the magnitude and phase value are measured and used to obtain information about defect. These values include the information about the shape or position of an unknown defect. The authors employ the neural network technique for estimation of a defect shape. The experimental results show the validity of the method.

  11. 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

  12. 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.

  13. 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. PMID:26628124

  14. 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.

  15. Non-destructive estimation of root pressure using sap flow, stem diameter measurements and mechanistic modelling

    PubMed Central

    De Swaef, Tom; Hanssens, Jochen; Cornelis, Annelies; Steppe, Kathy

    2013-01-01

    Background Upward water movement in plants via the xylem is generally attributed to the cohesion–tension theory, as a response to transpiration. Under certain environmental conditions, root pressure can also contribute to upward xylem water flow. Although the occurrence of root pressure is widely recognized, ambiguity exists about the exact mechanism behind root pressure, the main influencing factors and the consequences of root pressure. In horticultural crops, such as tomato (Solanum lycopersicum), root pressure is thought to cause cells to burst, and to have an important impact on the marketable yield. Despite the challenges of root pressure research, progress in this area is limited, probably because of difficulties with direct measurement of root pressure, prompting the need for indirect and non-destructive measurement techniques. Methods A new approach to allow non-destructive and non-invasive estimation of root pressure is presented, using continuous measurements of sap flow and stem diameter variation in tomato combined with a mechanistic flow and storage model, based on cohesion–tension principles. Key Results Transpiration-driven sap flow rates are typically inversely related to stem diameter changes; however, this inverse relationship was no longer valid under conditions of low transpiration. This decoupling between sap flow rates and stem diameter variations was mathematically related to root pressure. Conclusions Root pressure can be estimated in a non-destructive, repeatable manner, using only external plant sensors and a mechanistic model. PMID:23211757

  16. 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

  17. Giant Magnetoresistance Sensors: A Review on Structures and Non-Destructive Eddy Current Testing Applications.

    PubMed

    Rifai, Damhuji; Abdalla, Ahmed N; Ali, Kharudin; Razali, Ramdan

    2016-01-01

    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

  18. [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. PMID:26964242

  19. Study of the ferroelastic phase transition in the tetraethylammonium compound [N(C2H5)4]2ZnBr4 by magic-angle spinning and static NMR

    NASA Astrophysics Data System (ADS)

    Lim, Ae Ran

    2016-03-01

    The ferroelastic phase transition of tetraethylammonium compound [N(C2H5)4]2ZnBr4 at the phase transition temperature (TC) = 283 K was characterized by magic-angle spinning (MAS) and static nuclear magnetic resonance (NMR), and confirmed by optical polarizing spectroscopy. The structural geometry near TC was studied in terms of the chemical shifts and the spin-lattice relaxation times T1ρ in the rotating frame for 1H MAS NMR and 13C cross-polarization (CP)/MAS NMR. The two inequivalent ethyl groups were distinguishable in the 13C NMR spectrum, and the T1ρ results indicate that they undergo tumbling motion above TC in a coupled manner. From the 14N NMR results, the two nitrogen nuclei in the N(C2H5)4+ ions were distinguishable above TC, and the splitting in the spectra below TC was related to the ferroelastic domains with different orientations.

  20. A study of conformational stability of poly(L-alanine), poly(L-valine), and poly(L-alanine)/poly(L-valine) blends in the solid state by (13)C cross-polarization/magic angle spinning NMR.

    PubMed

    Murata, Katsuyoshi; Kuroki, Shigeki; Kimura, Hideaki; Ando, Isao

    2002-06-01

    13C cross-polarization/magic angle spinning (CP/MAS) NMR and (1)H T(1rho) experiments of poly(L-alanine) (PLA), poly(L-valine) (PLV), and PLA/PLV blends have been carried out in order to elucidate the conformational stability of the polypeptides in the solid state. These were prepared by adding a trifluoroacetic acid (TFA) solution of the polymer with a 2.0 wt/wt % of sulfuric acid (H(2)SO(4)) to alkaline water. From these experimental results, it is clarified that the conformations of PLA and PLV in their blends are strongly influenced by intermolecular hydrogen-bonding interactions that cause their miscibility at the molecular level. PMID:11948439

  1. 27Al magic-angle spinning nuclear magnetic resonance satellite transition spectroscopy of glasses in the system K2O-Al2O3-SiO2.

    PubMed

    Mundus, C; Müller-Warmuth, W

    1995-10-01

    27Al magic-angle spinning nuclear magnetic resonance satellite transition spectroscopy at 78 MHz has been applied to determine (true) chemical shift and quadrupole coupling parameters of glasses in the system K2O-Al2O3-SiO2 with 60-80 mol% SiO2 and K2O concentrations between 0 and 24 mol%. The powdered crystalline aluminosilicates andalusite and sillimanite have also been examined. In the glasses, all Al appears to be tetrahedrally bound in the aluminosilicate network unless x = mol% K2O:mol% Al2O3 becomes extremely small. Upon decreasing x the distortion of the tetrahedral Al(OSi)4 units increases in steps, and possible explanations are discussed. Six-coordinated aluminum observed for x < 0.2 is connected with the occurrence of interstitial Al3+ ions which charge-compensate the AlO4 units in addition to K+. PMID:8748646

  2. Non-destructive inspection of ferromagnetic pipes based on the discrete Fourier coefficients of magnetic flux leakage

    NASA Astrophysics Data System (ADS)

    Nara, T.; Fujieda, M.; Gotoh, Y.

    2014-05-01

    For non-destructive inspection of ferromagnetic pipes using magnetic flux leakage (MFL), a sensor consisting of two coils to measure the discrete Fourier sine and cosine coefficients of MFL is developed. The position of a crack in a pipe can be estimated from the squared sum and the ratio of the voltages induced in the two coils. Each coil has sixteen elemental coils with 78 permalloy cores which are placed along a circle with a radius of 6.3 mm and connected in series. The number of turns comprising an elemental coil at an angle ϕ is proportional to sinϕ in one coil and proportional to cosϕ in the other. It was experimentally shown that a circular crack 4 mm in diameter in a ferromagnetic pipe with diameter 21.6 mm was localized. The proposed structure is suitable for narrow pipe inspection where the sensitivity of our previous sensor composed of two coaxial crescent-shaped coils decreases.

  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. 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

  5. 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. PMID:23307024

  6. 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

  7. A non-destructive metrology solution for detailed measurements of imprint templates and media

    NASA Astrophysics Data System (ADS)

    Roberts, Jeffrey; Hu, Linlin; Eriksson, Torbjörn; Thulin, Kristian; Heidari, Babak

    2009-10-01

    This study investigates a non-destructive optical metrology technique, that furnishes measurement solutions for hard drive discrete track recording (DTR) and bit patterned media (BPM) templates and imprints. From the measurement and analysis of polarized reflectance and transmittance, feature height and profile of DTR and BPM templates and imprints, as well as residual layer thickness of imprints, are accurately determined, and uniformity maps of these parameters are produced in a fraction of a minute. Simulations of theoretical polarized reflectance and transmittance, relating to next generation structures, demonstrate that the optical metrology solution has capability for future products.

  8. 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.

  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. 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.

  11. 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.

  12. 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.

  13. Non-destructive high-resolution thermal imaging techniques to evaluate wildlife and delicate biological samples

    NASA Astrophysics Data System (ADS)

    Lavers, C.; Franklin, P.; Franklin, P.; Plowman, A.; Sayers, G.; Bol, J.; Shepard, D.; Fields, D.

    2009-07-01

    Thermal imaging cameras now allows routine monitoring of dangerous yet endangered wildlife in captivity. This study looks at the potential applications of radiometrically calibrated thermal data to wildlife, as well as providing parameters for future materials applications. We present a non-destructive active testing technique suitable for enhancing imagery contrast of thin or delicate biological specimens yielding improved thermal contrast at room temperature, for analysis of sample thermal properties. A broad spectrum of animals is studied with different textured surfaces, reflective and emissive properties in the infra red part of the electromagnetic spectrum. Some surface features offer biomimetic materials design opportunities.

  14. 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.

  15. A new facility for non-destructive assay using a 252Cf source.

    PubMed

    Stevanato, L; Caldogno, M; Dima, R; Fabris, D; Hao, Xin; Lunardon, M; Moretto, S; Nebbia, G; Pesente, S; Pino, F; Sajo-Bohus, L; Viesti, G

    2013-03-01

    A new laboratory facility for non-destructive analysis (NDA) using a time-tagged (252)Cf source is presented. The system is designed to analyze samples having maximum size of about 20 × 25 cm(2), the material recognition being obtained by measuring simultaneously total and energy dependent transmission of neutrons and gamma rays. The equipment technical characteristics and performances of the NDA system are presented, exploring also limits due to the sample thickness. Some recent applications in the field of cultural heritage are presented. PMID:23276691

  16. Non-destructive evaluation of cylindrical composite structures using photothermal radiometry

    NASA Astrophysics Data System (ADS)

    Wang, C.; Mandelis, A.; Liu, Y.

    2005-06-01

    Thermal-wave diagnostics by means of infrared photothermal radiometry (PTR) has been used for quantitative non-destructive evaluation of cylindrical composite structures. To quantitatively evaluate the thermal-wave field of a cylindrical composite material, the Green function corresponding to the composite structure has been developed and subsequently the thermal-wave field has been derived. Furthermore, the characteristics of the thermal-wave field for a cylindrical material with a surface coating are discussed. Experimental results from a stainless steel (AISI 302) tube are used to validate the theoretical model.

  17. Second harmonic generation for contactless non-destructive characterization of silicon on insulator wafers

    NASA Astrophysics Data System (ADS)

    Damianos, D.; Pirro, L.; Soylu, G.; Ionica, I.; Nguyen, V.; Vitrant, G.; Kaminski, A.; Blanc-Pelissier, D.; Onestas, L.; Changala, J.; Kryger, M.; Cristoloveanu, S.

    2016-01-01

    In this work we investigate a non-invasive, non-destructive characterization technique for monitoring the quality of film, oxide and interfaces in silicon-on-insulator (SOI) wafers. This technique is based on optical Second Harmonic Generation (SHG). The principles of SHG and the experimental setup will be thoroughly described. The experimental parameters best suited for testing SOI wafers with SHG are identified. SOI geometry, as well as the passivation of the top surface, both have an impact on the observed SHG signal. The back-gate bias applied on the substrate is shown to modulate the SHG signal.

  18. 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.

  19. Non-destructive evaluation of metal-to-metal adhesive joints using vibration analysis: experimental results

    NASA Astrophysics Data System (ADS)

    Pandurangan, Pradeep; Buckner, Gregory D.

    2006-03-01

    Vibration based non-destructive evaluation shows promise for damage detection in metal-to-metal adhesive joints. This research investigates an experimental technique to diagnose damage in single-lap adhesive joints subject to cyclical tensile loading. Vibration analysis reveals that damage can be correlated with changes in identified modal damping ratios. Constant amplitude forcing functions are employed to eliminate amplitude-dependent nonlinearities in the dynamic response profiles. Damping estimates obtained from time-domain analyses correlate well with damage magnitudes. Finite element modal analysis of the lap joints supports the experimental results.

  20. Photothermal Analysis Applied To Non-Destructive Evaluation Of Paint On Polymer Substrates

    NASA Astrophysics Data System (ADS)

    Vergne, D.; Busse, G.

    1988-10-01

    The decoration and protection quality of coatings on polymers is of considerable interest for industrial applications. However, at present there is no non-destructive (NDE) method to monitor the quality of these coatings during the manufacturing process or while they are in use. As an approach for such a method we use photothermal analysis where the propagation and reflection of optically generated thermal waves is investigated. We found that one can monitor the drying process, the effect of surface temperature treatment, and coating thickness (accuracy + 2 μm in 50 μm thickness). The information obtained with this remote NDE method is adequate for most industrial applications, eg car manufacturing.

  1. 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.

  2. MAGIC highlights

    NASA Astrophysics Data System (ADS)

    López-Coto, Rubén

    2016-07-01

    The present generation of Imaging Air Cherenkov Telescopes (IACTs) has greatly improved our knowledge on the Very High Energy (VHE) side of our Universe. The MAGIC IACTs operate since 2004 with one telescope and since 2009 as a two telescope stereoscopic system. I will outline a few of our latest and most relevant results: the discovery of pulsed emission from the Crab pulsar at VHE, recently found to extend up to 400 GeV and along the "bridge" of the light curve, the measurement of the Crab nebula spectrum over three decades of energy, the discovery of VHE γ-ray emission from the PWN 3C 58, the very rapid emission of IC 310, in addition to dark matter studies. The results that will be described here and the planned deep observations in the next years will pave the path for the future generation of IACTs.

  3. 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.

  4. Non-Destructive Evaluation of Grain Structure Using Air-Coupled Ultrasonics

    SciTech Connect

    Belvin, A. D.; Burrell, R. K.; Cole, E.G.

    2009-08-01

    Cast material has a grain structure that is relatively non-uniform. There is a desire to evaluate the grain structure of this material non-destructively. Traditionally, grain size measurement is a destructive process involving the sectioning and metallographic imaging of the material. Generally, this is performed on a representative sample on a periodic basis. Sampling is inefficient and costly. Furthermore, the resulting data may not provide an accurate description of the entire part's average grain size or grain size variation. This project is designed to develop a non-destructive acoustic scanning technique, using Chirp waveforms, to quantify average grain size and grain size variation across the surface of a cast material. A Chirp is a signal in which the frequency increases or decreases over time (frequency modulation). As a Chirp passes through a material, the material's grains reduce the signal (attenuation) by absorbing the signal energy. Geophysics research has shown a direct correlation with Chirp wave attenuation and mean grain size in geological structures. The goal of this project is to demonstrate that Chirp waveform attenuation can be used to measure grain size and grain variation in cast metals (uranium and other materials of interest). An off-axis ultrasonic inspection technique using air-coupled ultrasonics has been developed to determine grain size in cast materials. The technique gives a uniform response across the volume of the component. This technique has been demonstrated to provide generalized trends of grain variation over the samples investigated.

  5. Non-destructive investigation of a time capsule using neutron radiography and X-ray fluorescence

    NASA Astrophysics Data System (ADS)

    MacDonald, B. L.; Vanderstelt, J.; O'Meara, J.; McNeill, F. E.

    2016-01-01

    Non-destructive analytical techniques are becoming increasingly important for the study of objects of cultural heritage interest. This study applied two techniques: X-ray fluorescence and neutron radiography, for the investigation of a capped, tubular metal object recovered from an urban construction site in Gore Park, Hamilton, Canada. The site is an urban park containing a World War I commemorative monument that underwent renovation and relocation. Historical documentation suggested that the object buried underneath the monument was a time capsule containing a paper document listing the names of 1800 Canadians who died during WWI. The purpose of this study was to assess the condition of the object, and to verify if it was what the historical records purported. XRF analysis was used to characterize the elemental composition of the metal artifact, while neutron radiography revealed that its contents were congruent with historical records and remained intact after being interred for 91 years. Results of this study demonstrate the value of non-destructive techniques for the analysis and preservation of cultural heritage.

  6. 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. PMID:26117369

  7. 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.

  8. Non-Destructive Techniques in the Tacis and Phare Nuclear Safety Programmes

    SciTech Connect

    Bieth, Michel

    2002-07-01

    Decisions regarding the verification of design plant lifetime and potential license renewal periods involve a determination of the component and circuit condition. In Service Inspection of key reactor components becomes a crucial consideration for continued safe plant operation. The determination of the equipment properties by Non Destructive Techniques during periodic intervals is an important aspect of the assessment of fitness-for-service and safe operation of nuclear power plants The Tacis and Phare were established since 1991 by the European Union as support mechanisms through which projects could be identified and addressed satisfactorily. In Nuclear Safety, the countries mainly concerned are Russia, Ukraine, Armenia, and Kazakhstan for the Tacis programme, and Bulgaria, Czech Republic, Hungary, Slovak Republic, Lithuania, Romania and Slovenia for the Phare programme. The Tacis and Phare programs concerning the Nuclear Power Plants consist of: - On Site Assistance and Operational Safety, - Design Safety, - Regulatory Authorities, - Waste management, and are focused on reactor safety issues, contributing to the improvement in the safety of East European reactors and providing technology and safety culture transfer. The main parts of these programmes are related to the On-Site Assistance and to the Design Safety of VVER and RBMK Nuclear power plants where Non Destructive Techniques for In Service Inspection of the primary circuit components are addressed. (authors)

  9. 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.

  10. 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.

  11. 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. PMID:25967902

  12. 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.

  13. 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. PMID:23351273

  14. 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. PMID:25789964

  15. 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.

  16. 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. PMID:26150966

  17. Non-destructive quantification of pharmaceutical tablet coatings using terahertz pulsed imaging and optical coherence tomography

    NASA Astrophysics Data System (ADS)

    Zhong, Shuncong; Shen, Yao-Chun; Ho, Louise; May, Robert K.; Zeitler, J. Axel; Evans, Mike; Taday, Philip F.; Pepper, Michael; Rades, Thomas; Gordon, Keith C.; Müller, Ronny; Kleinebudde, Peter

    2011-03-01

    Optical coherence tomography (OCT) and terahertz pulsed imaging (TPI) are two powerful techniques allowing high quality cross-sectional images from within scattering media to be obtained non-destructively. In this paper, we report experimental results of using OCT and TPI for quantitatively characterizing pharmaceutical tablet coatings in the thickness range of 10-140 μm. We found that the spectral OCT system developed in-house has an axial resolution of 0.9 μm, and is capable of quantifying very thin coatings in the range of 10-60 μm. The upper limit of 60 μm within the tablet coating and core is owed to the strong scattering of OCT light, which has relatively short wavelengths in the range of 0.5-1.0 μm. On the other hand, TPI utilizes terahertz radiation that has substantially long wavelengths in the range of hundreds of microns, and thus is less prone to the scattering problem. Consequently TPI has been demonstrated to be able to quantify thicker coatings in the range of 40-140 μm and beyond. We concluded that OCT and TPI are two complementary analytical techniques for non-destructive and quantitative characterization of pharmaceutical tablet coatings.

  18. 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.

  19. 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.

  20. 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. PMID:22302428

  1. Checking collagen preservation in archaeological bone by non-destructive studies (Micro-CT and IBA)

    NASA Astrophysics Data System (ADS)

    Beck, L.; Cuif, J.-P.; Pichon, L.; Vaubaillon, S.; Dambricourt Malassé, A.; Abel, R. L.

    2012-02-01

    The material to be studied is a piece of human skull discovered (1999) in Pleistocene sediments from the Orsang river (Gujarat state, India). From anatomical view point, this skull is highly composite: modern Homo sapiens characters are associated to undoubtedly more ancient features. Absolute dating by 14C is critical to understand this discovery. Prior to dating measurements, non-destructive studies have been carried out. Micro-CT reconstruction (X-ray microtomography) and Ion Beam Analysis (IBA) have been undertaken to check the structural preservation of the fossil and the collagen preservation. PIXE elemental map was used to select well-preserved bone area. RBS/EBS and NRA were used for light element quantification, in particular C, N and O contents. We also demonstrate that the PIXE-RBS/EBS combination is a effective tool for the whole characterization of archaeological and recent bones by analysing in one experiment both mineral and organic fractions. We have shown that the archaeological bone, a fragment of the potentially oldest modern Indian, is enough preserved for radiocarbon dating. We propose that Elastic Backscattering Spectrometry (EBS) using 3 MeV protons could be a good non destructive alternative to conventional CHN method using Carbon-Hydrogen-Nitrogen analyzer for measuring C and N before 14C dating.

  2. Neural network and principal component regression in non-destructive soluble solids content assessment: a comparison*

    PubMed Central

    Chia, Kim-seng; Abdul Rahim, Herlina; Abdul Rahim, Ruzairi

    2012-01-01

    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. PMID:22302428

  3. 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. PMID:23022426

  4. 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.

  5. Non-destructive on-line monitoring of MIC (microbially influenced corrosion)

    SciTech Connect

    White, D.C. Tennessee Univ., Knoxville, TN ); Nivens, D.E.; Mittelman, M.W. . Inst. for Applied Microbiology); Chambers, J.Q. . Dept. of Chemistry); King, J.M.H. . Center for Environmental Biotechnology); Sayler, G.S. (Tennessee Univ., Knoxville, TN

    1990-01-01

    The formation of microbial biofilms on metal surfaces with the subsequent increase in heat transfer resistance and the induction of microbially influenced corrosion (MIC) is being increasingly recognized as an extremely important economic and safety problem for industrial water systems. The development of sufficiently rugged and accurate monitoring devices by which biofilm formation and activity of microbial biofilms can be monitored non-destructively, directly in water systems is the goal of this research. This on-line systems would allow the effective utilization of minimal levels of biocides and inhibitors as well as permit in situ testing of materials for MIC resistance. Several non-destructive technologies such as the quartz crystal microbalance (QCM), the attenuated total reflectance-Fourier transforming infrared spectrometer (ATR-FT/IR), and a genetically engineered bacterium containing the lux gene cassette in which its bioluminescence can be used to define its presence on coupons are on-line devices which accurately measure biofilm formation. Corrosion activity can be estimated by electrochemical impedance. 12 refs., 8 figs.

  6. 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.

  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. 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

  9. A semi-automatic non-destructive method to quantify grapevine downy mildew sporulation.

    PubMed

    Peressotti, Elisa; Duchêne, Eric; Merdinoglu, Didier; Mestre, Pere

    2011-02-01

    The availability of fast, reliable and non-destructive methods for the analysis of pathogen development contributes to a better understanding of plant-pathogen interactions. This is particularly true for the genetic analysis of quantitative resistance to plant pathogens, where the availability of a method allowing a precise quantification of pathogen development allows the reliable detection of different genomic regions involved in the resistance. Grapevine downy mildew, caused by the biotrophic Oomycete Plasmopara viticola, is one of the most important diseases affecting viticulture. Here we report the development of a simple image analysis-based semi-automatic method for the quantification of grapevine downy mildew sporulation, requiring just a compact digital camera and the open source software ImageJ. We confirm the suitability of the method for the analysis of the interaction between grapevine and downy mildew by performing QTL analysis of resistance to downy mildew as well as analysis of the kinetics of downy mildew infection. The non-destructive nature of the method will enable comparison between the phenotypic and molecular data obtained from the very same sample, resulting in a more accurate description of the interaction, while its simplicity makes it easily adaptable to other plant-pathogen interactions, in particular those involving downy mildews. PMID:21167874

  10. Assesment of uniaxial compressive strenght of repair mortars by using in situ non destructive techniques

    NASA Astrophysics Data System (ADS)

    Szemerey-Kiss, Balázs; Török, Ákos

    2014-05-01

    The present paper provides information on the strength assessment of restoration mortars by using ultrasonic pulse velocity. The aims of the tests were to determine the compressive strength of the mortars by using non destructive test methods. Four commercially available types of restoration mortars were tested. Besides the pure mortars, specimens with 30 and 50 wt% of limestone sand aggregate (from Sóskút quarry) were also made. The material properties of the tested mortars have been described in details previously (Szemerey-Kiss et al. 2013). Cubic test specimens of 3cm x 3cm x 3cm were prepared from the mortars and after casting and consolidation 10 cubes of each mortar type were tested. Ultrasonic pulse velocity was measured according to the guidelines given by EN 14579:2005. Uniaxial compressive strength of test specimens were measured following the instructions of EN 1015-11:2000. An exponential mathematical formula was outlined that describes the uniaxial compressive strength of mortars based on ultrasonic pulse velocity data. The best fit was found for two mortars while the formula with different constants could be also used for other mortars, too. These experiments have proved that non destructive tests can be used in the assessment of the strength of historic mortars. References: Szemerey-Kiss, B., Török, Á., Siegesmund S 2013. The influence of binder/aggregate ratio on the properties and strength of repair mortars. Environmental Earth Sciences, 69:1439-1449.

  11. 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.

  12. 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. PMID:25924926

  13. Investigation of the application of phase contrast imaging using a point X-ray source to industrial non-destructive testing.

    PubMed

    Suzuki, Kazuaki; Haig, Ian

    2014-03-01

    X-Tek Systems, a division of Nikon Metrology UK, designs, develops and manufactures microfocus X-ray radiography and computed tomography systems for industrial non-destructive testing. The range of X-ray acceleration voltages of its current standard products is 130-450 kV. It is widely known that X-ray images can be created using phase contrast formed by the natural propagation of X-rays. Simulation of the natural propagation of X-rays through a cylindrical test sample predicted a small contrast peak at the boundary between the cylinder material and air. Comparison data were obtained using an X-ray source with acceleration voltage above 100 kV. The simulation results correlated well with the experimental data. A further practical example (a 'magic mirror' amulet from an old Japanese shrine) is introduced and discussed. In this specimen, we detected intensity variation including the effect of phase contrast in the operating region above 100 kV. In summary, natural propagation phase contrast was observed in radiographic images from a standard point X-ray source with acceleration voltages exceeding 100 kV. PMID:24470417

  14. Photonic non-destructive measurement methods for investigating the evolution of polar firn and ice

    NASA Astrophysics Data System (ADS)

    Breton, Daniel James

    When snow falls on glaciers or ice sheets, it persists for many tens, hundreds and sometimes thousands of years before becoming ice. The granular material in between fresh snow and glacial ice is known as firn and is generally 50 to 100 m thick over polar ice sheets. The compaction mechanism of firn into ice (called densification) has important glaciological ramifications in determination of ice sheet stability and related sea level rise effects via remote sensing altimetry. Firn densification is also important for correctly interpreting ice core paleoclimate records, especially those analyzing gases trapped in air bubbles within the glacial ice. Densification is thought to depend strongly on microstructure: the sizes, shapes, orientations and inter-particle bonds of the ice grains that make up polar firn. Microstructure-dependent densification is poorly understood and occurs in the region where two-thirds of the overall densification takes place. This work focuses on developing non-destructive methods for simultaneously evaluating changes in both the bulk density and microstructure of polar firn to better understand structure- dependent densification processes. The first method is an automated density gauge which uses gamma-ray transmission methods to non-destructively produce high resolution (3.3 mm) and high precision (+/-4 kg m-3) density profiles of firn and ice cores. This instrument was used to collect a density profile for the first 160 m of the West Antarctic Ice Sheet Divide WDCO6A deep ice core. The second method involves optical scattering measurements on firn and ice cores to determine the important microstructural parameters of ice grain and air bubble size and air-ice interface surface area. These measurements are modeled using both Monte Carlo radiative transfer and ray-tracing geometric optics methods, and are then tested against experiment using digital photography of the WDC06A core. Combining the results of both bulk density and optical

  15. Non-destructive infrared analyses: a method for provenance analyses of sandstones

    NASA Astrophysics Data System (ADS)

    Bowitz, Jörg; Ehling, Angela

    2008-12-01

    Infrared spectroscopy (IR spectroscopy) is commonly applied in the laboratory for mineral analyses in addition to XRD. Because such technical efforts are time and cost consuming, we present an infrared-based mobile method for non-destructive mineral and provenance analyses of sandstones. IR spectroscopy is based on activating chemical bonds. By irradiating a mineral mixture, special bonds are activated to vibrate depending on the bond energy (resonance vibration). Accordingly, the energy of the IR spectrum will be reduced thereby generating an absorption spectrum. The positions of the absorption maxima within the spectral region indicate the type of the bonds and in many cases identify minerals containing these bonds. The non-destructive reflection spectroscopy operates in the near infrared region (NIR) and can detect all common clay minerals as well as sulfates, hydroxides and carbonates. The spectra produced have been interpreted by computer using digital mineral libraries that have been especially collected for sandstones. The comparison of all results with XRD, RFA and interpretations of thin sections demonstrates impressively the accuracy and reliability of this method. Not only are different minerals detectable, but also differently ordered kaolinites and varieties of illites can be identified by the shape and size of the absorption bands. Especially clay minerals and their varieties in combination with their relative contents form the characteristic spectra of sandstones. Other components such as limonite, hematite and amorphous silica also influence the spectra. Sandstones, similar in colour and texture, often can be identified by their characteristic reflectance spectra. Reference libraries with more than 60 spectra of important German sandstones have been created to enable entirely computerized interpretations and identifications of these dimension stones. The analysis of infrared spectroscopy results is demonstrated with examples of different sandstones

  16. The Versatile Magic Square.

    ERIC Educational Resources Information Center

    Watson, Gale A.

    2003-01-01

    Demonstrates the transformations that are possible to construct a variety of magic squares, including modifications to challenge students from elementary grades through algebra. Presents an example of using magic squares with students who have special needs. (YDS)

  17. Non-destructive fraud detection in rosehip oil by MIR spectroscopy and chemometrics.

    PubMed

    Santana, Felipe Bachion de; Gontijo, Lucas Caixeta; Mitsutake, Hery; Mazivila, Sarmento Júnior; Souza, Leticia Maria de; Borges Neto, Waldomiro

    2016-10-15

    Rosehip oil (Rosa eglanteria L.) is an important oil in the food, pharmaceutical and cosmetic industries. However, due to its high added value, it is liable to adulteration with other cheaper or lower quality oils. With this perspective, this work provides a new simple, fast and accurate methodology using mid-infrared (MIR) spectroscopy and partial least squares discriminant analysis (PLS-DA) as a means to discriminate authentic rosehip oil from adulterated rosehip oil containing soybean, corn and sunflower oils in different proportions. The model showed excellent sensitivity and specificity with 100% correct classification. Therefore, the developed methodology is a viable alternative for use in the laboratory and industry for standard quality analysis of rosehip oil since it is fast, accurate and non-destructive. PMID:27173556

  18. PREDICTION OF DISSOLVER LIFETIMES THROUGH NON-DESTRUCTIVE EVALUATION AND LABORATORY TESTING

    SciTech Connect

    Mickalonis, J.; Woodsmall, T.; Hinz, W.; Edwards, T.

    2011-10-03

    Non-destructive evaluation was used as the primary method of monitoring the corrosion degradation of nuclear material dissolvers and assessing the remaining lifetimes. Materials were typically processed in nitric acid based (4-14M) solutions containing fluoride concentrations less than 0.2 M. The primary corrosion issue for the stainless steel dissolvers is the occurrence of localized corrosion near the tank bottom and the heat affected zones of the welds. Laboratory data for a range of operational conditions, including solution chemistry and temperature, was used to assess the impact of processing changes on the dissolver corrosion rate. Experimental and NDE-based general corrosion rates were found to be in reasonable agreement for standard dissolution chemistries consisting of nitric acid with fluorides and at temperatures less than 95 C. Greater differences were observed when chloride was present as an impurity and temperatures exceeded 100 C.

  19. Rapid, non-destructive evaluation of ultrathin WSe{sub 2} using spectroscopic ellipsometry

    SciTech Connect

    Eichfeld, Sarah M.; Lin, Yu-Chuan; Hossain, Lorraine; Eichfeld, Chad M.; Robinson, Joshua A.

    2014-09-01

    The utilization of tungsten diselenide (WSe{sub 2}) in electronic and optoelectronic devices depends on the ability to understand and control the process-property relationship during synthesis. We demonstrate that spectroscopic ellipsometry is an excellent technique for accurate, non-destructive determination of ultra-thin (<30 nm) WSe{sub 2} properties. The refractive index (n) and extinction coefficient (k) were found to be independent of thickness down to 1.3 nm, and were used to determine film thickness, which was confirmed to be within 9% of values found via atomic force microscopy. Finally, the optical bandgap was found to closely correlate with thickness, ranging from 1.2 to 1.55 eV as the WSe{sub 2} is thinned to the equivalent of 2 atomic layers.

  20. Monitoring ground anchor using non-destructive ground anchor integrity test (NDT-GRANIT)

    NASA Astrophysics Data System (ADS)

    Robbany, Z.; Handayani, G.

    2015-09-01

    Monitoring at ground anchor commonly uses a pull out test method, therefor we developing a non-destructive ground anchor integrity testing (NDT-GRANIT). NDT-GRANIT using the principle of seismic waves that have been modified into form of sweep signal, the signal will be demodulated, filtered, and Fourier transformation (inverse discrete Fourier transform) so the data can be interpreted reflected wave from the ground anchor. The method was applied to determine whether the ground anchor still gripped in the subsurface by looking the attenuation of the wave generated sources. From the result we can see that ground anchor does not grip. To validate the results of the comparison method of measurement used pile integrity test.

  1. MCNP ESTIMATE OF THE SAMPLED VOLUME IN A NON-DESTRUCTIVE IN SITU SOIL CARBON ANALYSIS.

    SciTech Connect

    WIELOPOLSKI, L.; DIOSZEGI, I.; MITRA, S.

    2004-05-03

    Global warming, promoted by anthropogenic CO{sub 2} emission into the atmosphere, is partially mitigated by the photosynthesis processes of the terrestrial echo systems that act as atmospheric CO{sub 2} scrubbers and sequester carbon in soil. Switching from till to no till soils management practices in agriculture further augments this process. Carbon sequestration is also advanced by putting forward a carbon ''credit'' system whereby these can be traded between CO{sub 2} producers and sequesters. Implementation of carbon ''credit'' trade will be further promulgated by recent development of a non-destructive in situ carbon monitoring system based on inelastic neutron scattering (INS). Volumes and depth distributions defined by the 0.1, 1.0, 10, 50, and 90 percent neutron isofluxes, from a point source located at either 5 or 30 cm above the surface, were estimated using Monte Carlo calculations.

  2. Non-destructive evaluation of depth of surface cracks using ultrasonic frequency analysis.

    PubMed

    Her, Shiuh-Chuan; Lin, Sheng-Tung

    2014-01-01

    Ultrasonic is one of the most common uses of a non-destructive evaluation method for crack detection and characterization. The effectiveness of the acoustic-ultrasound Structural Health Monitoring (SHM) technique for the determination of the depth of the surface crack was presented. A method for ultrasonic sizing of surface cracks combined with the time domain and frequency spectrum was adopted. The ultrasonic frequency spectrum was obtained by Fourier transform technique. A series of test specimens with various depths of surface crack ranging from 1 mm to 8 mm was fabricated. The depth of the surface crack was evaluated using the pulse-echo technique. In this work, three different longitudinal waves with frequencies of 2.25 MHz, 5 MHz and 10 MHz were employed to investigate the effect of frequency on the sizing detection of surface cracks. Reasonable accuracies were achieved with measurement errors less than 7%. PMID:25225875

  3. In-situ and non-destructive focus determination device for high-precision laser applications

    NASA Astrophysics Data System (ADS)

    Armbruster, Oskar; Naghilou, Aida; Pöhl, Hannes; Kautek, Wolfgang

    2016-09-01

    A non-destructive, in-line, and low-cost focusing device based on an image sensor has been developed and demonstrated. It allows an in situ focus determination for a broad variety of laser types (e.g. cw and pulsed lasers). It provides stringent focusing conditions with high numerical apertures. This approach does not require sub-picosecond and/or auxiliary lasers, or high fluences above damage thresholds. Applications of this system include, but are not limited to the laser-illumination of micro-electrodes, pump-probe microscopy on thin films, and laser ablation of small samples without sufficient surface area for focus determination by ablation. An uncertainty of the focus position by an order of magnitude less than the respective Rayleigh length could be demonstrated.

  4. High-resolution thermal imaging methodology for non-destructive evaluation of historic structures

    NASA Astrophysics Data System (ADS)

    Hess, Michael; Vanoni, David; Petrovic, Vid; Kuester, Falko

    2015-11-01

    This paper presents a methodology for automated, portable thermography, for the acquisition of high-resolution thermal image mosaics supporting the non-destructive evaluation of historic structures. The presented approach increases the spatial resolution of thermal surveys to a level of detail needed for building scale analysis. The integration of a robotic camera platform enables automated alignment of multiple images into a high-resolution thermal image mosaic giving a holistic view of the structure while maintaining a level of detail equaling or exceeding that of traditional spot surveys using existing cameras. Providing a digital workflow for automated data and metadata recording increases the consistency and accuracy of surveys regardless of the location or operator. An imaging workflow and instrumentation are shown for a case-study on buildings in Florence, Italy demonstrating the effectiveness of this methodology for structural diagnostics.

  5. Evaluation and correction of readout artifacts from flat panel detectors for non-destructive testing purposes

    NASA Astrophysics Data System (ADS)

    Burtzlaff, S.; Voland, V.; Salamon, M.; Hofmann, Th.; Uhlmann, N.

    2009-08-01

    Flat panel detectors are commonly used for non-destructive testing purposes using X-ray technology. During a series of measurements with high absorbing objects, we observed an unknown kind of artifacts especially apparent with high contrast edges. These artifacts lead to unwanted results in radioscopic and computed tomography inspection. Given the object is fully occupying the lower part and half of the upper part of the detector. Looking at the image with high contrast visualization, it can be seen that the covered upper part of the detector is brighter than the covered lower half. The horizontal border of the detector tile is clearly recognizable. Furthermore, the uncovered area directly above the object is darker than next to the edge. In this area the vertical border of the edge below can be localized. We examined and evaluated the effect and developed a correction algorithm. The effect and its correction results are presented.

  6. Non-destructive research methods applied on materials for the new generation of nuclear reactors

    NASA Astrophysics Data System (ADS)

    Bartošová, I.; Slugeň, V.; Veterníková, J.; Sojak, S.; Petriska, M.; Bouhaddane, A.

    2014-06-01

    The paper is aimed on non-destructive experimental techniques applied on materials for the new generation of nuclear reactors (GEN IV). With the development of these reactors, also materials have to be developed in order to guarantee high standard properties needed for construction. These properties are high temperature resistance, radiation resistance and resistance to other negative effects. Nevertheless the changes in their mechanical properties should be only minimal. Materials, that fulfil these requirements, are analysed in this work. The ferritic-martensitic (FM) steels and ODS steels are studied in details. Microstructural defects, which can occur in structural materials and can be also accumulated during irradiation due to neutron flux or alpha, beta and gamma radiation, were analysed using different spectroscopic methods as positron annihilation spectroscopy and Barkhausen noise, which were applied for measurements of three different FM steels (T91, P91 and E97) as well as one ODS steel (ODS Eurofer).

  7. Transient elastodynamic model for beam defect interaction: application to non-destructive testing

    PubMed

    Raillon; Lecoeur-Taibi

    2000-03-01

    Modeling tools have been developed at the French Atomic Energy Commission (CEA) for the simulation of ultrasonic non-destructive testing inspections. In this paper the model for the prediction of echoes arising from defects within a piece (Mephisto) is presented and some examples are given and compared with experimental results. The model for computing wave defect interaction is based on Kirchhoff's approximation, and uses the principle of reciprocity and a mode-by-mode (between the transducer and the defect) calculation of the echoes. It accounts for possible mode conversions. These approximations and other approximations for the radiated field incident on the defect allow us to obtain a formulation of the echo received at the transducer, which is able to be computed rapidly. PMID:10829719

  8. Portable generator-based XRF instrument for non-destructive analysis at crime scenes

    NASA Astrophysics Data System (ADS)

    Schweitzer, Jeffrey S.; Trombka, Jacob I.; Floyd, Samuel; Selavka, Carl; Zeosky, Gerald; Gahn, Norman; McClanahan, Timothy; Burbine, Thomas

    2005-12-01

    Unattended and remote detection systems find applications in space exploration, telemedicine, teleforensics, homeland security and nuclear non-proliferation programs. The National Institute of Justice (NIJ) and the National Aeronautics and Space Administration's (NASA) Goddard Space Flight Center (GSFC) have teamed up to explore the use of NASA developed technologies to help criminal justice agencies and professionals investigate crimes. The objective of the program is to produce instruments and communication networks that have application within both NASA's space program and NIJ, together with state and local forensic laboratories. A general-purpose X-ray fluorescence system has been built for non-destructive analyses of trace and invisible material at crime scenes. This portable instrument is based on a generator that can operate to 60 kV and a Schottky CdTe detector. The instrument has been shown to be successful for the analysis of gunshot residue and a number of bodily fluids at crime scenes.

  9. Three-dimensional non-destructive testing (NDT) in the infrared spectrum

    NASA Astrophysics Data System (ADS)

    Akhloufi, Moulay A.; Guyon, Yannis; Bendada, Abdelhakim; Castenado, Clemente-Ibarra

    2015-05-01

    Three-dimensional (3D) vision scanning for metrology and inspection applications is an area that knows an increasing interest in the industry. This interest is driven by the recent advances in 3D technologies, permitting to attain high precision measurements at an affordable cost. 3D vision allows for the modelling and inspection of the visible surface of objects. When it is necessary to detect subsurface defects, active infrared (IR) thermography is one of the most used tools today for non-destructive testing (NDT) of materials. Fusion of these two modalities allows the simultaneous detection of surface and subsurface defects and to visualize these defects overlaid on a 3D model of the scanned and modelled parts or their 3D computer-aided design (CAD) models. In this work, we present a framework for automatically fusing 3D data (scanned or CAD) with the infrared thermal images for an NDT process in 3D space.

  10. A modified positron lifetime spectrometer as method of non-destructive testing in materials

    NASA Astrophysics Data System (ADS)

    Chen, Z. Q.; Shi, J. J.; Jiang, J.; Liu, X. B.; Wang, R. S.; Wu, Y. C.

    2015-02-01

    This paper aims to develop a new non-destructive testing (NDT) method using positron annihilation spectroscopy, a powerful tool to detect vacancy-type defects and defect's chemical environment. A positron NDT system was designed and constructed by modifying the "sandwich" structure of sample-source-sample in the conventional positron lifetime spectrometer. The positron lifetime spectra of one single sample can be measured and analyzed by subtracting the contribution of a reference sample. The feasibility and reliability of the positron NDT system have been tested by analyzing nondestructively deformation damage caused by mechanical treatment in metals and steels. This system can be used for detecting defects and damage in thick or large-size samples without cutting off the sample materials, as well as for detecting two-dimensional distribution of defects.

  11. Non-Destructive Evaluation of Depth of Surface Cracks Using Ultrasonic Frequency Analysis

    PubMed Central

    Her, Shiuh-Chuan; Lin, Sheng-Tung

    2014-01-01

    Ultrasonic is one of the most common uses of a non-destructive evaluation method for crack detection and characterization. The effectiveness of the acoustic-ultrasound Structural Health Monitoring (SHM) technique for the determination of the depth of the surface crack was presented. A method for ultrasonic sizing of surface cracks combined with the time domain and frequency spectrum was adopted. The ultrasonic frequency spectrum was obtained by Fourier transform technique. A series of test specimens with various depths of surface crack ranging from 1 mm to 8 mm was fabricated. The depth of the surface crack was evaluated using the pulse-echo technique. In this work, three different longitudinal waves with frequencies of 2.25 MHz, 5 MHz and 10 MHz were employed to investigate the effect of frequency on the sizing detection of surface cracks. Reasonable accuracies were achieved with measurement errors less than 7%. PMID:25225875

  12. System and method for non-destructive evaluation of surface characteristics of a magnetic material

    DOEpatents

    Jiles, David C.; Sipahi, Levent B.

    1994-05-17

    A system and a related method for non-destructive evaluation of the surface characteristics of a magnetic material. The sample is excited by an alternating magnetic field. The field frequency, amplitude and offset are controlled according to a predetermined protocol. The Barkhausen response of the sample is detected for the various fields and offsets and is analyzed. The system produces information relating to the frequency content, the amplitude content, the average or RMS energy content, as well as count rate information, for each of the Barkhausen responses at each of the excitation levels applied during the protocol. That information provides a contiguous body of data, heretofore unavailable, which can be analyzed to deduce information about the surface characteristics of the material at various depths below the surface.

  13. Interferometric system for non-destructive testing based on large diameter bacteriorhodopsin films

    NASA Astrophysics Data System (ADS)

    Juchem, Thorsten; Hampp, Norbert

    2000-08-01

    A system for holographic interferometry using bacteriorhodopsin films as an erasable optical recording medium is presented. Bacteriorhodopsin is a photochromic protein found in archaebacteria. Bacteriorhodopsin films with an aperture of 90×90 mm are used for high-resolution lensless recording (5000 lines/mm). The holograms are recorded in reflection-type geometry in order to achieve a compact design. A frequency-doubled Nd : YVO 4 laser, emitting at 532 nm, is used for recording and incoherent blue light is employed for photochemical erasure. The system is suitable for a variety of different interferometric techniques like double-exposure, time-averaging and real-time interferometry. As an example for the application of the BR-based non-destructive testing system the inspection of ceramic motor valves, made from silicone nitride (Si 3N 4), under mechanical load is reported.

  14. Non-destructive testing of an original XVI century painting on wood by ESPI system

    NASA Astrophysics Data System (ADS)

    Arena, G.; Paturzo, M.; Fatigati, G.; Grilli, M.; Pezzati, L.; Ferraro, P.

    2015-03-01

    Electronic Speckle Pattern Interferometry (ESPI), a non-contact and non-destructive optical techniques, was employed for assessing the conservation state of a XVI Century painting on wood (72x88x1,9 cm). By a long term analysis, the whole structure alterations, induced by the room temperature and relative humidity variations, were evaluated. Measurement of the whole painting structural bends was achieved. Local flaws and hidden detachments of pictorial layers from the support, which cannot be recognized by traditional art-restorer methods, were also revealed. This work was prevalently aimed at achieving a simple approach, in the laboratory practice, to get an intuitively user-friendly method for art conservators, not accustomed to high-tech or math based methods. The results demonstrate that ESPI can largely improve the traditional art conservation survey techniques.

  15. Could non-destructive methodologies enhance the microbiologically influenced corrosion (MIC) in pipeline systems?

    NASA Astrophysics Data System (ADS)

    Al-Abbas, F.; Kakpovbia, A.; Mishra, B.; Olson, D.; Spear, J.

    2013-01-01

    Stringent corrosion management programs are being deployed by oil and gas industry to ensure the integrity of pipeline systems. Parts of this program are the corrosion protection systems and inspection detection methods included non-destructive techniques. Those measures induce remnant magnetic field (RMF) in the pipeline steel. Potentially the RMF could affect the corrosion process in the pipeline including microbiologically influenced corrosion (MIC). Microorganisms in pipelines have surface charges and produce a wide variety of metabolic products. Consequently, when they are exposed to RMF generated at the linepipe steel surface by the aforementioned sources there will be potential effects. This sequentially will increase the likelihood of biofilm formation and hence enhance/promote MIC. This study investigates the potential effects of RFM on the MIC by sulfate reducing bacteria (SRB).

  16. Design of ERL Spoke Cavity For Non-Destructive Assay Research

    NASA Astrophysics Data System (ADS)

    Sawamura, M.; Nagai, R.; Nishimori, N.; Hajima, R.

    2015-10-01

    We are proposing non-destructive assay system of nuclear materials with laser Compton scattering combined with an energy-recovery linac (ERL) and a laser. Since constructing accelerator system for nuclear safe guard and security requires small cavities, spoke cavities have many advantages such as shortening the distance between cavities, small frequency detune due to micro-phonics and easy adjustment of field distribution for strong cell coupling. Calculations of optimized cavity shape and HOM coupler shape have been performed and rf properties with aluminum spoke cavity model have been also measured. Considering refrigerator system required for superconducting accelerator, we are planning to develop 325MHz spoke cavity which can be practically operated with 4K liquid helium. We have started to fabricate the niobium one-spoke cavity.

  17. Template synthesis of test tube nanoparticles using non-destructive replication.

    PubMed

    Wagner, Jonathan; Yao, Jingyuan; Rodgers, David; Hinds, Bruce

    2013-03-01

    Nano test tubes are a promising delivery vehicle for a range of therapeutics, including small molecule drugs and biologics. However, current template synthesis methods of producing nano test tubes are prohibitively expensive and time consuming. Here, non-destructive template replication was used to increase nano test tube yield from porous alumina by more than a hundredfold. We demonstrate how to produce nano test tubes of several sizes and compositions, including hybrid tubes with different inner and outer surfaces for targeted surface chemistry. Nano test tubes were readily suspended and stored in aqueous solutions without the need for chemical treatment. These nano test tubes should find application as delivery vehicles for therapeutics, particularly for processive 'bionanoreactors' loaded with enzymes. PMID:23376956

  18. Non-destructive testing of mid-IR optical fiber using infrared imaging

    NASA Astrophysics Data System (ADS)

    Gagnon, Marc-André; Fortin, Vincent; Vallée, Réal; Farley, Vincent; Lagueux, Philippe; Guyot, Éric; Marcotte, Frédérick

    2016-05-01

    Optical fiber lasers offers the advantage of being relatively compact and efficient. However, the materials such as fluoride and chalcogenide glasses used for their fabrication must be exempt of defects in order to make efficient laser systems. However, most existing quality control techniques are not compatible with chalcogenide fibers because of their limited transparency in the visible spectral range. For this reason, the Université Laval's Centre d'optique, photonique et laser (COPL), in Quebec City, Canada, has developed a novel non-destructive testing (NDT) methodology based on infrared imaging to address this problem. The results show how this simple screening technique eases the selection of high-quality fibers for the design of high-power mid-IR lasers.

  19. Evaluation of thermal cameras for non-destructive thermal testing applications

    NASA Astrophysics Data System (ADS)

    Chrzanowski, K.; Park, S. N.

    2001-04-01

    Thermal cameras are nowadays often used in industry and science for non-destructive thermal testing (NDTT). There have been published, by the American Society for Testing of Materials, two standards that present detailed measurement procedures of the minimum resolvable temperature difference (MRTD) and the minimum detectable temperature difference (MDTD) of commercial thermal cameras for NDTT applications. However, the standards provide only very general guidelines about the use of the measured MRTD and MDTD values for evaluation of thermal cameras for NDTT applications. Precise methods that enable evaluation of a thermal imager for NDTT application on the basis of measurement results of the MRTD and the MDTD are presented in this paper. The methods enable estimation of probabilities of detection, orientation, recognition and identification of thermal anomalies generated by flaws in the materials imaged.

  20. Prediction of Service Life of Cordierite-Mullite Refractory Materials by Non-Destructive Methods

    NASA Astrophysics Data System (ADS)

    Boccaccini, D. N.; Kamseu, Elie; Volkov-Husoviæ, T. D.; Cannio, M.; Romagnoli, M.; Veronesi, P.; Dlouhy, I.; Boccaccini, A. R.; Leonelli, C.

    2008-02-01

    Ultrasonic pulse velocity testing was used to perform non-destructive quality control of refractory plates used as substrates in fast firing of porcelain whitewares. The measurement of the ultrasonic velocity was used to asses the presence of internal voids or cracks originated from the manufacturing procedure. Image analysis was used to predict thermal stability of the refractory materials. Two cordierite-mullite compositions were investigated that are characterized by different microstructure morphologies and crack propagation behaviour. A brief discussion about the correlation between microstructure, crack propagation behaviour and thermal shock resistance is presented. Moreover, empirical models were developed to predict the service life of refractory plates from measured values of ultrasonic velocities in plates in the as-received state.

  1. Gigahertz time-domain spectroscopy and imaging for non-destructive materials research and evaluation

    NASA Astrophysics Data System (ADS)

    Bulgarevich, Dmitry S.; Shiwa, Mitsuharu; Furuya, Takashi; Tani, Masahiko

    2016-06-01

    By using optical sampling with repetition frequency modulation of pump/probe laser pulses on photoconductive emitter/detector antennas, the high-speed time/frequency domain gigahertz imaging is reported due to the absence of opto-mechanical delay line in this optical scheme. The clear contrast for a 3-cm wide metal plate, which was placed behind a 5-cm thick concrete block, was observed with a 1 × 1 mm image pixilation. On average, it took only ~0.75 s per pixel/waveform acquisition/assignment with a 675 ps time-domain window. This could become a valuable non-destructive evaluation technique in gigahertz spectral range with all benefits of time-domain spectroscopy.

  2. Gigahertz time-domain spectroscopy and imaging for non-destructive materials research and evaluation.

    PubMed

    Bulgarevich, Dmitry S; Shiwa, Mitsuharu; Furuya, Takashi; Tani, Masahiko

    2016-01-01

    By using optical sampling with repetition frequency modulation of pump/probe laser pulses on photoconductive emitter/detector antennas, the high-speed time/frequency domain gigahertz imaging is reported due to the absence of opto-mechanical delay line in this optical scheme. The clear contrast for a 3-cm wide metal plate, which was placed behind a 5-cm thick concrete block, was observed with a 1 × 1 mm image pixilation. On average, it took only ~0.75 s per pixel/waveform acquisition/assignment with a 675 ps time-domain window. This could become a valuable non-destructive evaluation technique in gigahertz spectral range with all benefits of time-domain spectroscopy. PMID:27302877

  3. Extracting Entanglement Entropy Via Non-Destructive Imaging of an Ultracold Atomic Gas

    NASA Astrophysics Data System (ADS)

    Price, Craig; Liu, Qi; Gemelke, Nathan

    2015-03-01

    Entanglement plays an important role in determining the thermodynamic ground state of many many-body quantum systems, and recent theoretical studies have provided evidence that broad classes of quantum critical and topologically ordered states may be characterized by the scaling properties of their entanglement entropy (EE). We describe how EE can be extracted in a QND imaging process, in which information is transferred from one quantum gas to another using pairwise entangling schemes, and how the subsequent non-local thermal back-action of detection may be used to probe pre-existing entanglement in the sample. We discuss related applications of quantum collisional microscopy, including minimally destructive imaging of non-equilibrium quantum gases, and the algorithmic cooling of a Mott-insulator by non-destructive detection and removal of thermal defects.

  4. Yucca Mountain project container fabrication, closure and non-destructive evaluation development activities; Summary and viewgraphs

    SciTech Connect

    Russell, E.W.; Nelson, T.A.

    1989-06-01

    In this presentation, container fabrication, closure, and non-destructive evaluation (NDE) process development activities are described. All of these activities are interrelated, and will contribute to the metal barrier selection activity. The plan is to use a corrosion-resistant material in the form of a cylinder with a wall thickness of {approximately}1cm (2cm for pure copper.) The materials under consideration include the three austenitic alloys: stainless steel-304L, stainless steel-316L and alloy 825, as well as the three copper alloys: CDA 102, CDA 613, and CDA 715. This document reviews the recommended procedures and processes for fabricating, closing and evaluating each of the candidate materials. (KGD)

  5. Gigahertz time-domain spectroscopy and imaging for non-destructive materials research and evaluation

    PubMed Central

    Bulgarevich, Dmitry S.; Shiwa, Mitsuharu; Furuya, Takashi; Tani, Masahiko

    2016-01-01

    By using optical sampling with repetition frequency modulation of pump/probe laser pulses on photoconductive emitter/detector antennas, the high-speed time/frequency domain gigahertz imaging is reported due to the absence of opto-mechanical delay line in this optical scheme. The clear contrast for a 3-cm wide metal plate, which was placed behind a 5-cm thick concrete block, was observed with a 1 × 1 mm image pixilation. On average, it took only ~0.75 s per pixel/waveform acquisition/assignment with a 675 ps time-domain window. This could become a valuable non-destructive evaluation technique in gigahertz spectral range with all benefits of time-domain spectroscopy. PMID:27302877

  6. In situ non-destructive measurement of biofilm thickness and topology in an interferometric optical microscope.

    PubMed

    Larimer, Curtis; Suter, Jonathan D; Bonheyo, George; Addleman, Raymond Shane

    2016-06-01

    Biofilms are ubiquitous and impact the environment, human health, dental hygiene, and a wide range of industrial processes. Biofilms are difficult to characterize when fully hydrated, especially in a non-destructive manner, because of their soft structure and water-like bulk properties. Herein a method of measuring and monitoring the thickness and topology of live biofilms of using white light interferometry is described. Using this technique, surface morphology, surface roughness, and biofilm thickness were measured over time without while the biofilm continued to grow. The thickness and surface topology of a P. putida biofilm were monitored growing from initial colonization to a mature biofilm. Measured thickness followed expected trends for bacterial growth. Surface roughness also increased over time and was a leading indicator of biofilm growth. PMID:26992071

  7. Non-Destructive Evaluation of Thermal Spray Coating Interface Quality By Eddy Current Method

    SciTech Connect

    B. Mi; G. Zhao; R. Bayles

    2006-08-10

    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 various surface preparation conditions or spray process parameters. A quad-frequency eddy current probe was used to manually scan over the coating surface to evaluate the bonding quality. Experimental results show that different surface preparation conditions and varied process parameters can be successfully differentiated by the impedance value observed from the eddy current probe. The measurement is fairly robust and consistent. This non-contact, nondestructive, easy-to-use technique has the potential for evaluating the coating quality immediately after its application so that any defects can be corrected immediately.

  8. Template synthesis of test tube nanoparticles using non-destructive replication

    PubMed Central

    Wagner, Jonathan; Yao, Jingyuan; Rodgers, David; Hinds, Bruce

    2013-01-01

    Nano test tubes are a promising delivery vehicle for a range of therapeutics including small molecule drugs and biologics. However, current template synthesis methods of producing nano test tubes are prohibitively expensive and time consuming. Here, non-destructive template replication was used to increase nano test tube yield from porous alumina by more than a hundredfold. We demonstrate how to produce nano test tubes of several sizes and compositions including hybrid tubes with different inner and outer surfaces for targeted surface chemistry. Nano test tubes were readily suspended and stored in aqueous solutions without the need for chemical treatment. These nano test tubes should find application as delivery vehicles for therapeutics, particularly for processive “bionanoreactors” loaded with enzymes. PMID:23376956

  9. Wavelet Processing of Continuous Scanning Laser Doppler Vibrometry data in Non-Destructive Testing

    NASA Astrophysics Data System (ADS)

    Chiariotti, P.; Revel, G. M.; Martarelli, M.

    2015-11-01

    The present paper proposes a novel non-destructive testing procedure based on the exploitation of the simultaneous time and spatial sampling provided by Continuous Scanning Laser Doppler Vibrometry (CSLDV) and the feature extraction capabilities of wavelet-based processing. Two criteria for selecting in an objective way the mother-wavelet to be used in the decomposition procedure, the Relative Wavelet Energy and Energy to Shannon Entropy Ratio, are compared in terms of capability of best locating the damage. The paper demonstrates the applicability of the procedure for the identification of superficial and in-depth defects in simulated and real test cases when an area scan is performed over the test sample. The method shows promising results, since defects are identified in different severity conditions.

  10. Prediction of Service Life of Cordierite-Mullite Refractory Materials by Non-Destructive Methods

    SciTech Connect

    Boccaccini, D. N.; Kamseu, Elie; Cannio, M.; Romagnoli, M.; Veronesi, P.; Leonelli, C.; Volkov-Husoviae, T. D.; Dlouhy, I.; Boccaccini, A. R.

    2008-02-15

    Ultrasonic pulse velocity testing was used to perform non-destructive quality control of refractory plates used as substrates in fast firing of porcelain whitewares. The measurement of the ultrasonic velocity was used to asses the presence of internal voids or cracks originated from the manufacturing procedure. Image analysis was used to predict thermal stability of the refractory materials. Two cordierite-mullite compositions were investigated that are characterized by different microstructure morphologies and crack propagation behaviour. A brief discussion about the correlation between microstructure, crack propagation behaviour and thermal shock resistance is presented. Moreover, empirical models were developed to predict the service life of refractory plates from measured values of ultrasonic velocities in plates in the as-received state.

  11. Contribution to the improvement of heritage mural painting non-destructive testing by stimulated infrared thermography

    NASA Astrophysics Data System (ADS)

    Bodnar, Jean-Luc; Mouhoubi, Kamel; Di Pallo, Luigi; Detalle, Vincent; Vallet, Jean-Marc; Duvaut, Thierry

    2013-10-01

    Non-destructive testing of heritage mural paintings by means of stimulated infrared thermography has now become rather efficient [1-14]. However, pigments, which form a pictorial layer, have contrasting radiative properties possibly leading to artifact detection. In this paper, attempts to alleviate this difficulty are presented. Based on the spectroscopic study of different paint layers, one can argue that, in the medium infrared field, this radiative disparity decreases significantly. Then, with similar settings, it can be shown that ceramic radiative sources allow reaching this wavelength band. Finally, on the basis of a study carried out on an academic sample and a partial copy of a fresco from the cathedral of Angers, combining ceramic heat sources with a laboratory SAMMTHIR experimental setup enables to make real headway in terms of defects' detection.

  12. Magnetic non-destructive evaluation of ruptures of tensile armor in oil risers

    NASA Astrophysics Data System (ADS)

    Pérez-Benitez, J. A.; Padovese, L. R.

    2012-04-01

    Risers are flexible multilayered pipes formed by an inner flexible metal structure surrounded by polymer layers and spiral wound steel ligaments, also known as armor wires. Since these risers are used to link subsea pipelines to floating oil and gas production installations, and their failure could produce catastrophic consequences, some methods have been proposed to monitor the armor integrity. However, until now there is no practical method that allows the automatic non-destructive detection of individual armor wire rupture. In this work we show a method using magnetic Barkhausen noise that has shown high efficiency in the detection of armor wire rupture. The results are examined under the cyclic and static load conditions of the riser. This work also analyzes the theory behind the singular dependence of the magnetic Barkhausen noise on the applied tension in riser armor wires.

  13. Monitoring ground anchor using non-destructive ground anchor integrity test (NDT-GRANIT)

    SciTech Connect

    Robbany, Z. Handayani, G.

    2015-09-30

    Monitoring at ground anchor commonly uses a pull out test method, therefor we developing a non-destructive ground anchor integrity testing (NDT-GRANIT). NDT-GRANIT using the principle of seismic waves that have been modified into form of sweep signal, the signal will be demodulated, filtered, and Fourier transformation (inverse discrete Fourier transform) so the data can be interpreted reflected wave from the ground anchor. The method was applied to determine whether the ground anchor still gripped in the subsurface by looking the attenuation of the wave generated sources. From the result we can see that ground anchor does not grip. To validate the results of the comparison method of measurement used pile integrity test.

  14. Non-destructive quantitative analysis of risperidone in film-coated tablets.

    PubMed

    Orkoula, M G; Kontoyannis, C G

    2008-07-15

    A simple, non-destructive, methodology based on FT-Raman spectroscopy was developed for the quantitative analysis of risperidone in commercially available film-coated tablets. A simple linear regression model was constructed based on standard tablets, prepared using the same manufacturing process as the commercially available. The tablets contained 0.27, 0.54, 1.08, 1.62, 2.16, 3.24 and 4.32 wt% risperidone. The most prominent Raman vibration of the active pharmaceutical ingredient at 1533 cm(-1), recorded using a home-made rotating system, was plotted against concentration. The model was tested on commercial film-coated tablets. The results were compared against those obtained by application of HPLC on the same samples. PMID:18359600

  15. Non-destructive Ripeness Sensing by Using Proton NMR [Nuclear Magnetic Resonance

    DOE R&D Accomplishments Database

    Cho, Seong In; Krutz, G. W.; Stroshine, R. L.; Bellon, V.

    1990-01-01

    More than 80 kinds of fruits and vegetables are available in the United States. But only about 6 of them have their quality standards (Dull, 1986). In the 1990 Fresh Trends survey (Zind, 1990), consumers were asked to rate 16 characteristics important to their decision to purchase fresh produce. The four top ranking factors were ripeness/freshness, taste/flavor, appearance/condition and nutritional value. Of these surveyed, 96% rated ripeness/freshness as extremely important or very important. Therefore, the development of reliable grading or sorting techniques for fresh commodities is essential. Determination of fruit quality often involves cutting and tasting. Non-destructive quality control in fruit and vegetables is a goal of growers and distributors, as well as the food processing industry. Many nondestructive techniques have been evaluated including soft x-ray, optical transmission, near infrared radiation, and machine vision. However, there are few reports of successful non-destructive measurement of sugar content directly in fruit. Higher quality fruit could be harvested and available to consumers if a nondestructive sensor that detects ripeness level directly by measuring sugar content were available. Using proton Nuclear Magnetic Resonance (NMR) principle is the possibility. A nondestructive ripeness (or sweetness) sensor for fruit quality control can be developed with the proton NMR principle (Cho, 1989). Several feasibility studies were necessary for the ripeness sensor development. Main objectives in this paper was to investigate the feasibilities (1) to detect ripeness (or sweetness level) of raw fruit tissue with an high resolution proton NMR spectroscopy (200 MHz) and (2) to measure sugar content of intact fruit with a low resolution proton NMR spectroscopy (10 MHz).

  16. Monitoring fungal growth on brown rice grains using rapid and non-destructive hyperspectral imaging.

    PubMed

    Siripatrawan, U; Makino, Y

    2015-04-16

    This research aimed to develop a rapid, non-destructive, and accurate method based on hyperspectral imaging (HSI) for monitoring spoilage fungal growth on stored brown rice. Brown rice was inoculated with a non-pathogenic strain of Aspergillus oryzae and stored at 30 °C and 85% RH. Growth of A. oryzae on rice was monitored using viable colony counts, expressed as colony forming units per gram (CFU/g). The fungal development was observed using scanning electron microscopy. The HSI system was used to acquire reflectance images of the samples covering the visible and near-infrared (NIR) wavelength range of 400-1000 nm. Unsupervised self-organizing map (SOM) was used to visualize data classification of different levels of fungal infection. Partial least squares (PLS) regression was used to predict fungal growth on rice grains from the HSI reflectance spectra. The HSI spectral signals decreased with increasing colony counts, while conserving similar spectral pattern during the fungal growth. When integrated with SOM, the proposed HSI method could be used to classify rice samples with different levels of fungal infection without sample manipulation. Moreover, HSI was able to rapidly identify infected rice although the samples showed no symptoms of fungal infection. Based on PLS regression, the coefficient of determination was 0.97 and root mean square error of prediction was 0.39 log (CFU/g), demonstrating that the HSI technique was effective for prediction of fungal infection in rice grains. The ability of HSI to detect fungal infection at early stage would help to prevent contaminated rice grains from entering the food chain. This research provides scientific information on the rapid, non-destructive, and effective fungal detection system for rice grains. PMID:25662486

  17. Non-destructive in situ mapping of macroholes, cracks and inhomogeneities of stalagmites in cave environments

    NASA Astrophysics Data System (ADS)

    Hegymegi, Erika; Gyöngy, Miklós; Bodolai, Tamás; Divós, Ferenc; Barta, Edit; Gribovszki, Katalin; Bokelmann, Götz; Hegymegi, Csaba; Lednická, Markéta; Kovács, Károly

    2016-04-01

    Intact and vulnerable, candle-stick type stalagmites can be used as prehistoric-earthquake indicators during seismic-hazard analysis of a given region, because they are old enough to survive several earthquakes. The continued intactness of the stalagmites indicates a lack of earthquakes that had the strength to destroy them. To make sure that the stalagmites are intact, we have to image their internal structure in order to estimate the steadiness more accurate and potential failure in the last few thousand years, during their evolution. These stalagmites play an important indicator role and carry fundamental information; however, legally they are strictly protected natural objects in Europe. Therefore it is impossible to examine them in the laboratory by conventional equipment such as computer tomography (CT) or X-ray, because this would require taking samples. With the presented non-destructive methods (ultrasound and acoustic tomography) we tried to detect macroholes, cracks and velocity anomalies inside the stalagmites on the mm scale in situ, in the cave. The acoustic tomography applied in the current work is an existing method in forest research. Forest researchers use it to non-destructively detect the size and location of decayed or hollow parts in the trunk and this technique is able to detect the velocity changing of wave propagation and anomalies in the stalagmites as well. The other method that we use is ultrasound imaging, which uses (and is able to calculate) the velocity of sound propagation. Here, the frequency used is much higher (typically 250 kHz to 5 MHz), which increases resolution but at the same time decreases penetration depth compared to acoustic tomography. In this latter work, through transmission and TOFD (time-of-flight-diffraction) ultrasound methods are using thickness-mode ultrasound transducers (Panametrics, Olympus). Such equipment is well-adapted to the cave environment and this is the first time that it has been used for these

  18. Non-destructive ripeness sensing by using proton NMR (Nuclear Magnetic Resonance)

    SciTech Connect

    Cho, Seong In; Krutz, G.W.; Stroshine, R.L. . Dept. of Agricultural Engineering); Bellon, V. , 34 - Montpellier )

    1990-01-01

    More than 80 kinds of fruits and vegetables are available in the United States. But only about 6 of them have their quality standards (Dull, 1986). In the 1990 Fresh Trends survey (Zind, 1990), consumers were asked to rate 16 characteristics important to their decision to purchase fresh produce. The four top ranking factors were ripeness/freshness, taste/flavor, appearance/condition and nutritional value. Of these surveyed, 96% rated ripeness/freshness as extremely important or very important. Therefore, the development of reliable grading or sorting techniques for fresh commodities is essential. Determination of fruit quality often involves cutting and tasting. Non-destructive quality control in fruit and vegetables is a goal of growers and distributors, as well as the food processing industry. Many nondestructive techniques have been evaluated including soft x-ray, optical transmission, near infrared radiation, and machine vision. However, there are few reports of successful non-destructive measurement of sugar content directly in fruit. Higher quality fruit could be harvested and available to consumers if a nondestructive sensor that detects ripeness level directly by measuring sugar content were available. Using proton Nuclear Magnetic Resonance (NMR) principle is the possibility. A nondestructive ripeness (or sweetness) sensor for fruit quality control can be developed with the proton NMR principle (Cho, 1989). Several feasibility studies were necessary for the ripeness sensor development. Main objectives in this paper was to investigate the feasibilities (1) to detect ripeness (or sweetness level) of raw fruit tissue with an high resolution proton NMR spectroscopy (200 MHz) and (2) to measure sugar content of intact fruit with a low resolution proton NMR spectroscopy (10 MHz). 7 refs., 4 figs.

  19. NON-DESTRUCTIVE TBC SPALLATION DETECTION BY A MICRO-INDENTATION METHOD

    SciTech Connect

    J. M. Tannenbaum; B.S.-J. Kang; M.A. Alvin

    2010-06-18

    In this research, a load-based depth-sensing micro-indentation method for spallation detection and damage assessment of thermal barrier coating (TBC) materials is presented. A non-destructive multiple loading/partial unloading testing methodology was developed where in stiffness responses of TBC coupons subjected to various thermal cyclic loading conditions were analyzed to predict the spallation site and assess TBC degradation state. The measured stiffness responses at various thermal loading cycles were used to generate time-series color maps for correlation with accumulation of TBC residual stress states. The regions with higher stiffness responses can be linked to a rise in out-of-plane residual stress located near or at the yttria stabilized zirconia (YSZ)/thermally grown oxide (TGO) interface, which is ultimately responsible for initiating TBC spallation failure. A TBC thermal exposure testing plan was carried out where time-series cross-sectional microstructural analyses of damage accumulation and spallation failure associated with the evolution of bond coat/TGO/top coat composite (e.g. thickness, ratcheting, localized oxidations, etc.) of air plasma sprayed (APS) TBCs were evaluated and correlated to the measured stiffness responses at various thermal cycles. The results show that the load-based micro-indentation test methodology is capable of identifying the spallation site(s) before actual occurrence. This micro-indentation technique can be viewed as a viable non-destructive evaluation (NDE) technique for determining as-manufactured and process-exposed TBCs. This technique also shows promise for the development of a portable instrument for on-line, in-situ spallation detection/prediction of industrial-size TBC turbine components.

  20. μ-XRF analysis of glasses: a non-destructive utility for Cultural Heritage applications.

    PubMed

    Vaggelli, G; Cossio, R

    2012-02-01

    This paper presents a μ-XRF analytical approach for a non-destructive study of Cultural Heritage glass finds. This technique can be used for quantitative analysis of small volumes of solid samples, with a sensitivity that is superior to the electron microprobe but inferior to an ICP-MS system. An experimental set-up with natural and synthetic glass standards is proposed here for the quantitative analyses of major and trace elements on glass objects which cannot be sampled such as small archaeological or historical artefacts from Cultural Heritage. The described method, performed by means of the commercial μ-XRF Eagle III-XPL, was applied to Islamic glass specimens of Sasanian production (III-VII century A.D.) previously analyzed by ICP-MS and SEM-EDS techniques (P. Mirti, M. Pace, M. Negro Ponzi and M. Aceto, Archaeometry, 2008, 50(3), 429-450; P. Mirti, M. Pace, M. Malandrino and M. Negro Ponzi, J. Archaeol. Sci., 36, 1061-1069; and M. Gulmini, M. Pace, G. Ivaldi, M. Negro Ponzi and P. Mirti, J. Non-Cryst. Solids, 2009, 355, 1613-1621) and coming from the archaeological site of Veh Ardasir in modern Iraq. Major elements (Na, Mg, Al, Si, K, Ca, Fe) of glass specimens show an accuracy better than 5%. Trace elements (Cr, Mn, Sr and Zr) display an accuracy better than 5% when the checked elements have a concentration >100 ppm by weight, whereas it is around 10% with a concentration <100 ppm by weight. μ-XRF is, therefore, a suitable elemental analysis technique for the non-destructive study of small glass finds due to its relatively good accuracy, reproducibility and low detection limits (∼tens ppm). PMID:22163367

  1. Portable 1,5 MeV X-Band Linac For Non-destructive Radiography

    NASA Astrophysics Data System (ADS)

    Saversky, A. J.; Rodionov, A. E.; Shaltyrev, A. P.; Shchedrin, I. S.

    1997-05-01

    Portable linear electron accelerator Y-34 developed in Small Accelerator Laboratory of MEPhI for non-destructive industrial radiography. This Linac is a fully self-contained device with the exception of external electric power 220Vx50Gz, 1 phase, 5 kVA. Full mass of Linac Y-34 - less than 300 kg. The Radiographic parameters: Nominal Energy - 1,5 MeV; Energy Range - 0,7...1,8 MeV; Maximum pulse current - 100 mA; Maximum Intensity - 15 R/min@m; Focal spot size - less than 2 mm. The Linac is comprised of 4 subassemblies. The X-ray head with weight less than 100 kg, dimensions: 0,7x0,7x1,0 m contains the traveling-wave accelerating structure with lens 0,4 m, electron gun, vacuum pump, tungsten target and RF-system with 500-kW magnetron. The permanent magnets focusing system provides focal spot less than 2 mm. The high voltage power unit consist of a line-type magnetron/electron gun modulator 2 kW power supply, the weight is equal 70 kg. The self-contained cooling water supply provides temperature controlled water for accelerator structure and magnetron. The control console allows convenient monitoring of critical system and Linac parameters by manual or remote computer. Portable X-band Linac Y-34 is the effective X - ray and/or electron beam source for such applications as non-destructive examination of nuclear reactor systems, solid rocket motors, technology research.

  2. Perception, Illusion, and Magic.

    ERIC Educational Resources Information Center

    Solomon, Paul R.

    1980-01-01

    Describes a psychology course in which magical illusions were used for teaching the principles of sensation and perception. Students read psychological, philosophical, historical, and magical literature on illusion, performed a magical illusion, and analyzed the illusion in terms of the psychological principles involved. (Author/KC)

  3. Shortening spin-lattice relaxation using a copper-chelated lipid at low-temperatures - A magic angle spinning solid-state NMR study on a membrane-bound protein.

    PubMed

    Yamamoto, Kazutoshi; Caporini, Marc A; Im, Sangchoul; Waskell, Lucy; Ramamoorthy, Ayyalusamy

    2013-12-01

    Inherent low sensitivity of NMR spectroscopy has been a major disadvantage, especially to study biomolecules like membrane proteins. Recent studies have successfully demonstrated the advantages of performing solid-state NMR experiments at very low and ultralow temperatures to enhance the sensitivity. However, the long spin-lattice relaxation time, T1, at very low temperatures is a major limitation. To overcome this difficulty, we demonstrate the use of a copper-chelated lipid for magic angle spinning solid-state NMR measurements on cytochrome-b5 reconstituted in multilamellar vesicles. Our results on multilamellar vesicles containing as small as 0.5mol% of a copper-chelated lipid can significantly shorten T1 of protons, which can be used to considerably reduce the data collection time or to enhance the signal-to-noise ratio. We also monitored the effect of slow cooling on the resolution and sensitivity of (13)C and (15)N signals from the protein and (13)C signals from lipids. PMID:24246881

  4. Stochastic molecular motions in the nematic, smectic-A, and solid phases of p,p{sup '}-di-n-heptyl-azoxybenzene as seen by quasielastic neutron scattering and {sup 13}C cross-polarization magic-angle-spinning NMR

    SciTech Connect

    ZajaPc, Wojciech; Urban, Stanislaw; Domenici, Valentina; Geppi, Marco; Veracini, Carlo Alberto; Telling, Mark T. F.; Gabrys, Barbara J.

    2006-05-15

    Molecular rotational dynamics in p,p{sup '}-di-n-heptyl-azoxybenzene was studied by means of quasielastic neutron scattering (QENS) and {sup 13}C cross-polarization magic-angle-spinning (CPMAS) NMR. Fast reorientation of the hydrogen nuclei was observed by QENS in the two liquid crystalline (LC) phases nematic and smectic A, as well as in the crystalline phase. The latter could not be restricted to the -CH{sub 3} rotations alone, and a clear indication was found of some other reorientation motions persisting in the crystal. Two Lorentz-type components convoluted with the resolution function gave an excellent fit to the QENS spectra in both LC phases. The narrow (slow) component was attributed to the reorientation of the whole molecule around the long axis. The corresponding characteristic time of {approx}130 ps agreed well with the values obtained in recent dielectric relaxation and {sup 2}H NMR studies. The full width at half maximum of the broader (fast) component shows a quadratic Q dependence (Q is the momentum transfer). Hence the corresponding motions could be described by a stretched exponential correlation function and were interpreted as various ''crankshaft-type'' motions within the alkyl tails. The {sup 13}C CPMAS experiments fully corroborated the QENS results, sometimes considered ambiguous in complex systems.

  5. Stochastic molecular motions in the nematic, smectic-A, and solid phases of p,p'-di-n-heptyl-azoxybenzene as seen by quasielastic neutron scattering and 13C cross-polarization magic-angle-spinning NMR.

    PubMed

    Zajac, Wojciech; Urban, Stanisław; Domenici, Valentina; Geppi, Marco; Veracini, Carlo Alberto; Telling, Mark T F; Gabryś, Barbara J

    2006-05-01

    Molecular rotational dynamics in p,p'-di-n-heptyl-azoxybenzene was studied by means of quasielastic neutron scattering (QENS) and 13C cross-polarization magic-angle-spinning (CPMAS) NMR. Fast reorientation of the hydrogen nuclei was observed by QENS in the two liquid crystalline (LC) phases nematic and smectic A, as well as in the crystalline phase. The latter could not be restricted to the -CH3 rotations alone, and a clear indication was found of some other reorientation motions persisting in the crystal. Two Lorentz-type components convoluted with the resolution function gave an excellent fit to the QENS spectra in both LC phases. The narrow (slow) component was attributed to the reorientation of the whole molecule around the long axis. The corresponding characteristic time of approximately 130 ps agreed well with the values obtained in recent dielectric relaxation and 2H NMR studies. The full width at half maximum of the broader (fast) component shows a quadratic Q dependence (Q is the momentum transfer). Hence the corresponding motions could be described by a stretched exponential correlation function and were interpreted as various "crankshaft-type" motions within the alkyl tails. The 13C CPMAS experiments fully corroborated the QENS results, sometimes considered ambiguous in complex systems. PMID:16802951

  6. {sup 13}C, {sup 1}H, {sup 6}Li magic-angle spinning nuclear magnetic resonance, electron paramagnetic resonance, and Fourier transform infrared study of intercalation electrodes based in ultrasoft carbons obtained below 3100 K

    SciTech Connect

    Alcantara, R.; Madrigal, F.J.F.; Lavela, P.; Tirado, J.L.; Mateos, J.M.J.; Stoyanova, R.; Zhecheva, E.

    1999-01-01

    The past decade has seen an important development of materials for high-performance energy storage systems. Particularly, the field of electrode materials for advanced lithium batteries has attracted the interest of numerous researchers. Petroleum coke samples of different origins and heat treated at different temperatures below 3100 K have been studied by spectroscopic and electrochemical procedures. According to {sup 13}C and {sup 1}H magic-angle spinning (MAS) nuclear magnetic resonance (NMR), infrared (IR), and electron paramagnetic resonance (EPR) data, aromatic compounds and surface OH groups are present in green coke samples. The preparation of CMB (combustible) sample from 1673 K leads to a low-temperature graphitization process, as shown by the occurrence of multiphase products containing both turbostatic and graphitized solid. This process is accompanied by the loss of aromatic compounds and surface hydroxyls. The optimization of the lithium intercalation electrodes based in the green coke materials was carried out by thermal treatment at 1023 K under dynamic vacuum conditions. Such pretreatment of the electrode material leads to marked enhancement of reversible capacities without the higher temperatures usually required for other soft carbon materials. Finally, the results of {sup 6}Li MAS NMR and EPR have been correlated with the experimental determination of lithium diffusion coefficients and surface properties. On the basis of these results, spin resonance spectroscopies are found to be a powerful tool to discern between the different petroleum coke samples to select the active electrode material with best performance.

  7. Shortening Spin-lattice Relaxation Using a Copper-Chelated lipid at Low-Temperatures – A Magic Angle Spinning Solid-State NMR Study on a Membrane-Bound Protein

    PubMed Central

    Yamamoto, Kazutoshi; Caporini, Marc; Im, Sangchoul; Waskell, Lucy; Ramamoorthy, Ayyalusamy

    2013-01-01

    Inherent low sensitivity of NMR spectroscopy has been a major disadvantage, especially to study biomolecules like membrane proteins. Recent studies have successfully demonstrated the advantages of performing solid-state NMR experiments at very low and ultralow temperatures to enhance the sensitivity. However, the long spin-lattice relaxation time, T1, at very low temperatures is a major limitation. To overcome this difficulty, we demonstrate the use of a copper-chelated lipid for magic angle spinning solid-state NMR measurements on cytochrome-b5 reconstituted in multilamellar vesicles. Our results on multilamellar vesicles containing as small as 0.5 mole % of a copper-chelated lipid can significantly shorten T1 of protons, which can be used to considerably reduce the data collection time or to enhance the signal-to-noise ratio. We also monitored the effect of slow cooling on the resolution and sensitivity of 13C and 15N signals from the protein and 13C signals from lipids. PMID:24246881

  8. Non-destructive testing for the structures and civil infrastructures characterization

    NASA Astrophysics Data System (ADS)

    Capozzoli, L.; Rizzo, E.

    2012-04-01

    infrared thermography and sonic testing. Finally, we investigated a radiant floor by GPR (900 MHz to 2000 MHz antennas) and long-wave infrared camera. Non-destructive diagnostic techniques allow to investigate a building structure in reinforced concrete or masonry without altering the characteristics of the element investigated. For this reason, geo-electrical and electromagnetic surveys of masonry are a suitable non-destructive tool for the diagnosis of a deteriorated concrete structure. Moreover, the integration of different NDT techniques (conventional and no-conventional) is a very powerful to maximize the capabilities and to compensate for the limitations of each method.

  9. Fast solver for large scale eddy current non-destructive evaluation problems

    NASA Astrophysics Data System (ADS)

    Lei, Naiguang

    Eddy current testing plays a very important role in non-destructive evaluations of conducting test samples. Based on Faraday's law, an alternating magnetic field source generates induced currents, called eddy currents, in an electrically conducting test specimen. The eddy currents generate induced magnetic fields that oppose the direction of the inducing magnetic field in accordance with Lenz's law. In the presence of discontinuities in material property or defects in the test specimen, the induced eddy current paths are perturbed and the associated magnetic fields can be detected by coils or magnetic field sensors, such as Hall elements or magneto-resistance sensors. Due to the complexity of the test specimen and the inspection environments, the availability of theoretical simulation models is extremely valuable for studying the basic field/flaw interactions in order to obtain a fuller understanding of non-destructive testing phenomena. Theoretical models of the forward problem are also useful for training and validation of automated defect detection systems. Theoretical models generate defect signatures that are expensive to replicate experimentally. In general, modelling methods can be classified into two categories: analytical and numerical. Although analytical approaches offer closed form solution, it is generally not possible to obtain largely due to the complex sample and defect geometries, especially in three-dimensional space. Numerical modelling has become popular with advances in computer technology and computational methods. However, due to the huge time consumption in the case of large scale problems, accelerations/fast solvers are needed to enhance numerical models. This dissertation describes a numerical simulation model for eddy current problems using finite element analysis. Validation of the accuracy of this model is demonstrated via comparison with experimental measurements of steam generator tube wall defects. These simulations generating two

  10. Direct, non-destructive, and rapid evaluation of developmental cotton fibers by ATR FT-IR spectroscopy

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Chemical, compositional, and structural differences within the fibers at different growth stages have been investigated considerably through a number of methodologies. Due to its direct, non-destructive, and rapid attribute, this study reports the utilization of attenuated total reflection Fourier t...

  11. Development of vibrational spectroscopic methods to rapidly and non-destructively assess quality of chicken breast meat

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Development of Vibrational Spectroscopic Methods to Rapidly and Non-Destructively Assess Quality of Chicken Breast Meat H. Zhuang1, M. Sohn2, S. Trabelsi1 and K. Lawrence1 1Quality and Safety Assessment Research Unit, ARS-USDA, 950 College Station Road, Athens, GA 30605 2University of Georgia, De...

  12. A new facility for Non-Destructive Assay with a time-tagged {sup 252}Cf source

    SciTech Connect

    Stevanato, L.; Caldogno, M.; Hao Xin; Dima, R.; Fabris, D.; Nebbia, G.; Lunardon, M.; Moretto, S.; Pesente, S.; Viesti, G.; Sajo-Bohus, L.

    2010-08-04

    A new facility for non-destructive assay using a time-tagged {sup 252}Cf source is presented. The system is designed to analyze samples having maximum size of about 15x20 cm{sup 2}, the material recognition being obtained by measuring simultaneously transmission of neutrons and gamma rays.

  13. Development of non-destructive quality measurement technique for cabbage seed (Brassica campestris L) using hyperspectral reflectance imaging

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cabbage (Brassica campestris L) is an important crop for Asian countries especially in Korea, Japan and China. In order to achieve uniform and high-yield rate of cabbage product, the seed lot quality needs to be controlled. Non-destructive evaluation of seed viability is an important technique for i...

  14. Non-destructive quantification of alignment of nanorods embedded in uniaxially stretched polymer films

    NASA Astrophysics Data System (ADS)

    Stoenescu, Stefan; Truong, Vo-Van; Packirisamy, Muthukumaran

    2014-03-01

    Among several methods developed for uniaxial alignment of metallic nanorods for optical applications, alignment by film stretching consists in embedding the rods in a transparent thin film of thermoplastic polymer, followed by simultaneous heating and uniaxial stretching of the composite film. As to the quantification of the resulting alignment, it has been limited to statistical calculations based on microscopic examination, which is incomplete, subject to errors due to geometric distortions of the scanning electron microscope images and destructive, since it involves cutting of samples. In contrast, we present in this paper a non-destructive quantification of the average orientation of the rods, based on a probabilistic approach combined with numerical simulations of absorbance spectra and spectrometric characterization of the composite film. Assuming electromagnetically non-interacting rods, we consider the longitudinal absorbance peak of their ensemble to consist of the superposition of their individual spectra that we obtain by numerical simulation using the size and shape adapted dielectric function of the metal and the finite difference time domain method. The accuracy of the solution depends on the number of discretization intervals, the accuracy of the numerical simulations, and the accurate knowledge of the polydispersity of the rods. For the sake of concreteness, we used nanorods to describe the quantification steps but the method is equally valid for any dichroic particles.

  15. Recent advances in rapid and non-destructive assessment of meat quality using hyperspectral imaging

    NASA Astrophysics Data System (ADS)

    Tao, Feifei; Ngadi, Michael

    2016-05-01

    Meat is an important food item in human diet. Its production and consumption has greatly increased in the last decades with the development of economies and improvement of peoples' living standards. However, most of the traditional methods for evaluation of meat quality are time-consuming, laborious, inconsistent and destructive to samples, which make them not appropriate for a fast-paced production and processing environment. Development of innovative and non-destructive optical sensing techniques to facilitate simple, fast, and accurate evaluation of quality are attracting increasing attention in the food industry. Hyperspectral imaging is one of the promising techniques. It integrates the combined merits of imaging and spectroscopic techniques. This paper provides a comprehensive review on recent advances in evaluation of the important quality attributes of meat including color, marbling, tenderness, pH, water holding capacity, and also chemical composition attributes such as moisture content, protein content and fat content in pork, beef and lamb. In addition, the future potential applications and trends of hyperspectral imaging are also discussed in this paper.

  16. Non-destructive in-situ method and apparatus for determining radionuclide depth in media

    DOEpatents

    Xu, X. George; Naessens, Edward P.

    2003-01-01

    A non-destructive method and apparatus which is based on in-situ gamma spectroscopy is used to determine the depth of radiological contamination in media such as concrete. An algorithm, Gamma Penetration Depth Unfolding Algorithm (GPDUA), uses point kernel techniques to predict the depth of contamination based on the results of uncollided peak information from the in-situ gamma spectroscopy. The invention is better, faster, safer, and/cheaper than the current practice in decontamination and decommissioning of facilities that are slow, rough and unsafe. The invention uses a priori knowledge of the contaminant source distribution. The applicable radiological contaminants of interest are any isotopes that emit two or more gamma rays per disintegration or isotopes that emit a single gamma ray but have gamma-emitting progeny in secular equilibrium with its parent (e.g., .sup.60 Co, .sup.235 U, and .sup.137 Cs to name a few). The predicted depths from the GPDUA algorithm using Monte Carlo N-Particle Transport Code (MCNP) simulations and laboratory experiments using .sup.60 Co have consistently produced predicted depths within 20% of the actual or known depth.

  17. Assessment of the non-destructive nature of PASD on wire insulation integrity.

    SciTech Connect

    Lockner, Thomas Ramsbeck; Peña, Gary Edward; Schneider, Larry X.; Higgins, Matthew B.; Glover, Steven Frank

    2003-09-01

    The potential of a new cable diagnostic known as Pulse-Arrested Spark Discharge technique (PASD) is being studied. Previous reports have documented the capability of the technique to locate cable failures using a short high voltage pulse. This report will investigate the impact of PASD on the sample under test. In this report, two different energy deposition experiments are discussed. These experiments include the PASD pulse ({approx}6 mJ) and a high energy discharge ({approx}600 mJ) produced from a charged capacitor source. The high energy experiment is used to inflict detectable damage upon the insulators and to make comparisons with the effects of the low energy PASD pulse. Insulator breakdown voltage strength before and after application of the PASD pulse and high energy discharges are compared. Results indicate that the PASD technique does not appear to degrade the breakdown strength of the insulator or to produce visible damage. However, testing of the additional materials, including connector insulators, may be warranted to verify PASDs non-destructive nature across the full spectrum of insulators used in commercial aircraft wiring systems.

  18. Non-Destructive Evaluation of Wind Turbine Blades Using an Infrared Camera

    SciTech Connect

    Beattie, A.G.; Rumsey, M.

    1998-12-17

    The use of a digital infrared as a non-destructive evaluation thermography camera (NDE) tool was ex- plored in two separate wind turbine blade fatigue tests. The fwst test was a fatigue test of part of a 13.1 meter wood-epoxy-composite blade. The second test was on a 4.25 meter pultruded fiber glass blade section driven at several mechanical resonant frequencies. The digital infrared camera can produce images of either the static temperature distribution on the surface of the specimen, or the dynamic temperature distribution that is in phase with a specific frequency on a vibrating specimen. The dynamic temperature distribution (due to thermoplastic effects) gives a measure of the sum of the principal stresses at each point on the surface. In the wood- epoxy-composite blade fatigue test, the point of ultimate failure was detected long before failure occurred. The mode shapes obtained with the digital infrared camera, from the resonant blade tests, were in very good agree- ment with the finite-element calculations. In addition, the static temperature images of the resonating blade showed two areas that contained cracks. Close-up dy- namic inf%red images of these areas showed the crack structure that agreed with subsequent dye-penetrant analysis.

  19. Non-Destructive Optical Monitoring of Grape Maturation by Proximal Sensing

    PubMed Central

    Ben Ghozlen, Naïma; Cerovic, Zoran G.; Germain, Claire; Toutain, Sandrine; Latouche, Gwendal

    2010-01-01

    A new, commercial, fluorescence-based optical sensor for plant constituent assessment was recently introduced. This sensor, called the Multiplex® (FORCE-A, Orsay, France), was used to monitor grape maturation by specifically monitoring anthocyanin accumulation. We derived the empirical anthocyanin content calibration curves for Champagne red grape cultivars, and we also propose a general model for the influence of the proportion of red berries, skin anthocyanin content and berry size on Multiplex® indices. The Multiplex® was used on both berry samples in the laboratory and on intact clusters in the vineyard. We found that the inverted and log-transformed far-red fluorescence signal called the FERARI index, although sensitive to sample size and distance, is potentially the most widely applicable. The more robust indices, based on chlorophyll fluorescence excitation ratios, showed three ranges of dependence on anthocyanin content. We found that up to 0.16 mg cm−2, equivalent to approximately 0.6 mg g−1, all indices increase with accumulation of skin anthocyanin content. Excitation ratio-based indices decrease with anthocyanin accumulation beyond 0.27 mg cm−2. We showed that the Multiplex® can be advantageously used in vineyards on intact clusters for the non-destructive assessment of anthocyanin content of vine blocks and can now be tested on other fruits and vegetables based on the same model. PMID:22163456

  20. Laser ultrasound and simulated time reversal on bulk waves for non destructive control

    NASA Astrophysics Data System (ADS)

    Diot, G.; Walaszek, H.; Kouadri-David, A.; Guégan, S.; Flifla, J.

    2014-06-01

    Laser welding of aluminium generally creates embedded welding defects, such as porosities or cracks. Non Destructive Inspection (NDI) after processing may ensure an acceptable weld quality by defect detection. Nowadays, NDI techniques used to control the inside of a weld are mainly limited to X-Rays or ultrasonics. The current paper describes the use of a Laser Ultrasound (LU) technique to inspect porosities in 2 and 4-mm thick sheet lap welds. First experimentations resulted in the detection of 0.5-mm drilled holes in bulk aluminium sheets. The measurement of the depth of these defects is demonstrated too. Further experimentations shows the applicability of the LU technique to detect porosities in aluminium laser welds. However, as the interpretation of raw measures is limiting the detection capacity of this technique, we developed a signal processing using Time-Reversal capabilities to enhance detection capacities. Furthermore, the signal processing output is a geometrical image of the material's inner state, increasing the ease of interpretation. It is based on a mass-spring simulation which enables the back-propagation of the acquired ultrasound signal. The spring-mass simulation allows the natural generation of all the different sound waves and thus enables the back-propagation of a raw signal without any need of filtering or wave identification and extraction. Therefore the signal processing uses the information contained in the compression wave as well as in the shear wave.

  1. Quantitative impact characterization of aeronautical CFRP materials with non-destructive testing methods

    SciTech Connect

    Kiefel, Denis E-mail: Rainer.Stoessel@airbus.com; Stoessel, Rainer E-mail: Rainer.Stoessel@airbus.com; Grosse, Christian

    2015-03-31

    In recent years, an increasing number of safety-relevant structures are designed and manufactured from carbon fiber reinforced polymers (CFRP) in order to reduce weight of airplanes by taking the advantage of their specific strength into account. Non-destructive testing (NDT) methods for quantitative defect analysis of damages are liquid- or air-coupled ultrasonic testing (UT), phased array ultrasonic techniques, and active thermography (IR). The advantage of these testing methods is the applicability on large areas. However, their quantitative information is often limited on impact localization and size. In addition to these techniques, Airbus Group Innovations operates a micro x-ray computed tomography (μ-XCT) system, which was developed for CFRP characterization. It is an open system which allows different kinds of acquisition, reconstruction, and data evaluation. One main advantage of this μ-XCT system is its high resolution with 3-dimensional analysis and visualization opportunities, which enables to gain important quantitative information for composite part design and stress analysis. Within this study, different NDT methods will be compared at CFRP samples with specified artificial impact damages. The results can be used to select the most suitable NDT-method for specific application cases. Furthermore, novel evaluation and visualization methods for impact analyzes are developed and will be presented.

  2. How clean is clean: Non-destructive/direct methods of flux, residue detection

    NASA Astrophysics Data System (ADS)

    Welch, C. S.; Ray, U.; Stallard, B. R.; Watkins, R. D.; Koch, M. W.; Moya, M. M.

    The feasibility of three different non-destructive and direct methods of evaluating PCB (printed circuit boards) cleanliness was demonstrated. The detection limits associated with each method were established. In addition, the pros and cons of these methods as routine quality control inspection tools were discussed. OSEE (Optically Stimulated Electron Emission) was demonstrated to be a sensitive technique for detection of low levels of flux residues on insulating substances. However, future work including development of rugged OSEE instrumentation will determine whether the PCB industry can accept this technique in a production environment. FTIR (Fourier Transform Infrared) microscopy is a well established technique with well known characteristics. The inability of FTIR to discriminate an organic contaminant from an organic substrate limits its usefulness as a PCB line inspection tool, but it will still remain a technique for the QC/QA laboratory. One advantage of FTIR over the other two techniques described here is its ability to identify the chemical nature of the residue, which is important in Failure Mode Analysis. Optical imaging using sophisticated pattern recognition algorithms was found to be limited to high concentrations of residue. Further work on improved sensor techniques is necessary.

  3. Static characterization of a soft elastomeric capacitor for non destructive evaluation applications

    SciTech Connect

    Saleem, Hussam; Laflamme, Simon; Zhang, Huanhuan; Geiger, Randall; Kessler, Michael; Rajan, Krishna

    2014-02-18

    A large and flexible strain transducer consisting of a soft elastomeric capacitor (SEC) has been proposed by the authors. Arranged in a network setup, the sensing strategy offers tremendous potential at conducting non-destructive evaluation of large-scale surfaces. In prior work, the authors have demonstrated the performance of the sensor at tracking strain history, localizing cracks, and detecting vibration signatures. In this paper, we characterize the static performance of the proposed SEC. The characterization includes sensitivity of the signal, and temperature and humidity dependences. Tests are conducted on a simply supported aluminum beam subjected to bending as well as on a free standing sensor. The performance of the SEC is compared against off-the-shelf resistance-based strain gauges with resolution of 1 με. A sensitivity of 1190 pF/ε is obtained experimentally, in agreement with theory. Results also show the sensor linearity over the given level of strain, showing the promise of the SEC at monitoring of surface strain.

  4. Thermal history sensors for non-destructive temperature measurements in harsh environments

    SciTech Connect

    Pilgrim, C. C.; Heyes, A. L.; Feist, J. P.

    2014-02-18

    The operating temperature is a critical physical parameter in many engineering applications, however, can be very challenging to measure in certain environments, particularly when access is limited or on rotating components. A new quantitative non-destructive temperature measurement technique has been proposed which relies on thermally induced permanent changes in ceramic phosphors. This technique has several distinct advantages over current methods for many different applications. The robust ceramic material stores the temperature information allowing long term thermal exposures in harsh environment to be measured at a convenient time. Additionally, rare earth dopants make the ceramic phosphorescent so that the temperature information can be interpreted by automated interrogation of the phosphorescent light. This technique has been demonstrated by application of YAG doped with dysprosium and europium as coatings through the air-plasma spray process. Either material can be used to measure temperature over a wide range, namely between 300°C and 900°C. Furthermore, results show that the material records the peak exposure temperature and prolonged exposure at lower temperatures would have no effect on the temperature measurement. This indicates that these materials could be used to measure peak operating temperatures in long-term testing.

  5. Non-Destructive Current Sensing for Energy Efficiency Monitoring in Buildings with Environmental Certification

    PubMed Central

    Mota, Lia Toledo Moreira; Mota, Alexandre de Assis; Coiado, Lorenzo Campos

    2015-01-01

    Nowadays, buildings environmental certifications encourage the implementation of initiatives aiming to increase energy efficiency in buildings. In these certification systems, increased energy efficiency arising from such initiatives must be demonstrated. Thus, a challenge to be faced is how to check the increase in energy efficiency related to each of the employed initiatives without a considerable building retrofit. In this context, this work presents a non-destructive method for electric current sensing to assess implemented initiatives to increase energy efficiency in buildings with environmental certification. This method proposes the use of a sensor that can be installed directly in the low voltage electrical circuit conductors that are powering the initiative under evaluation, without the need for reforms that result in significant costs, repair, and maintenance. The proposed sensor consists of three elements: an air-core transformer current sensor, an amplifying/filtering stage, and a microprocessor. A prototype of the proposed sensor was developed and tests were performed to validate this sensor. Based on laboratory tests, it was possible to characterize the proposed current sensor with respect to the number of turns and cross-sectional area of the primary and secondary coils. Furthermore, using the Least Squares Method, it was possible to determine the efficiency of the air core transformer current sensor (the best efficiency found, considering different test conditions, was 2%), which leads to a linear output response. PMID:26184208

  6. PHOTOACOUSTIC NON-DESTRUCTIVE EVALUATION AND IMAGING OF CARIES IN DENTAL SAMPLES

    SciTech Connect

    Li, T.; Dewhurst, R. J.

    2010-02-22

    Dental caries is a disease wherein bacterial processes damage hard tooth structure. Traditional dental radiography has its limitations for detecting early stage caries. In this study, a photoacoustic (PA) imaging system with the near-infrared light source has been applied to postmortem dental samples to obtain 2-D and 3-D images. Imaging results showed that the PA technique can be used to image human teeth caries. For non-destructive photoacoustic evaluation and imaging, the induced temperature and pressure rises within biotissues should not cause physical damage to the tissue. For example, temperature rises above 5 deg. C within live human teeth will cause pulpal necrosis. Therefore, several simulations based on the thermoelastic effect have been applied to predict temperature and pressure fields within samples. Predicted temperature levels are below corresponding safety limits, but care is required to avoid nonlinear absorption phenomena. Furthermore, PA imaging results from the phantom provide evidence for high sensitivity, which shows the imaging potential of the PA technique for detecting early stage disease.

  7. Robotic path planning for non-destructive testing of complex shaped surfaces

    NASA Astrophysics Data System (ADS)

    Mineo, Carmelo; Pierce, Stephen Gareth; Wright, Ben; Nicholson, Pascual Ian; Cooper, Ian

    2015-03-01

    The requirement to increase inspection speeds for non-destructive testing (NDT) of composite aerospace parts is common to many manufacturers. The prevalence of complex curved surfaces in the industry provides significant motivation for the use of 6 axis robots for deployment of NDT probes in these inspections. A new system for robot deployed ultrasonic inspection of composite aerospace components is presented. The key novelty of the approach is through the accommodation of flexible robotic trajectory planning, coordinated with the NDT data acquisition. Using a flexible approach in MATLAB, the authors have developed a high level custom toolbox that utilizes external control of an industrial 6 axis manipulator to achieve complex path planning and provide synchronization of the employed ultrasonic phase array inspection system. The developed software maintains a high level approach to the robot programming, in order to ease the programming complexity for an NDT inspection operator. Crucially the approach provides a pathway for a conditional programming approach and the capability for multiple robot control (a significant limitation in many current off-line programming applications). Ultrasonic and experimental data has been collected for the validation of the inspection technique. The path trajectory generation for a large, curved carbon-fiber-reinforced polymer (CFRP) aerofoil component has been proven and is presented. The path error relative to a raster-scan tool-path, suitable for ultrasonic phased array inspection, has been measured to be within + 2mm over the 1.6 m2 area of the component surface.

  8. Non-Destructive Measurement of Vascular Tissue Development in Stems of Miniature Tomato Using Acoustic Method

    NASA Astrophysics Data System (ADS)

    Kageyama, Kensuke; Watanabe, Eiko; Kato, Hiroshi

    The guided wave effect resembling that of annual rings found in woods and the cortical region of bones is believed to be observable in vascular tissues of herbaceous plants. The properties of acoustic waves traveling through the vascular tissue in the stem of a miniature tomato were measured using a piezoelectric pulser and receiver. The thickness of the vascular tissues and the stem's water content were measured. The detected acoustic waves showed a guided wave effect. The apparent sound velocity, va, was related to the vascular tissue thickness, tv. These results reveal that the detected acoustic waves traveled along the vascular tissues in stems. The maximum peak intensity of the detected acoustic waves, Imax was also related to t. Furthermore, wilting of the examined plants decreased the Imax, although va was not changed. The decrease in Imax might result from cavitations and embolisms with a subsequent increase in air pores in xylem tissues. These results demonstrate that the measurement of acoustic waves traveling through vascular tissue is a useful tool for the non-destructive evaluation of vascular tissue development and embolism density in xylem tissues.

  9. Non-Destructive Current Sensing for Energy Efficiency Monitoring in Buildings with Environmental Certification.

    PubMed

    Mota, Lia Toledo Moreira; Mota, Alexandre de Assis; Coiado, Lorenzo Campos

    2015-01-01

    Nowadays, buildings environmental certifications encourage the implementation of initiatives aiming to increase energy efficiency in buildings. In these certification systems, increased energy efficiency arising from such initiatives must be demonstrated. Thus, a challenge to be faced is how to check the increase in energy efficiency related to each of the employed initiatives without a considerable building retrofit. In this context, this work presents a non-destructive method for electric current sensing to assess implemented initiatives to increase energy efficiency in buildings with environmental certification. This method proposes the use of a sensor that can be installed directly in the low voltage electrical circuit conductors that are powering the initiative under evaluation, without the need for reforms that result in significant costs, repair, and maintenance. The proposed sensor consists of three elements: an air-core transformer current sensor, an amplifying/filtering stage, and a microprocessor. A prototype of the proposed sensor was developed and tests were performed to validate this sensor. Based on laboratory tests, it was possible to characterize the proposed current sensor with respect to the number of turns and cross-sectional area of the primary and secondary coils. Furthermore, using the Least Squares Method, it was possible to determine the efficiency of the air core transformer current sensor (the best efficiency found, considering different test conditions, was 2%), which leads to a linear output response. PMID:26184208

  10. An x ray scatter approach for non-destructive chemical analysis of low atomic numbered elements

    NASA Technical Reports Server (NTRS)

    Ross, H. Richard

    1993-01-01

    A non-destructive x-ray scatter (XRS) approach has been developed, along with a rapid atomic scatter algorithm for the detection and analysis of low atomic-numbered elements in solids, powders, and liquids. The present method of energy dispersive x-ray fluorescence spectroscopy (EDXRF) makes the analysis of light elements (i.e., less than sodium; less than 11) extremely difficult. Detection and measurement become progressively worse as atomic numbers become smaller, due to a competing process called 'Auger Emission', which reduces fluorescent intensity, coupled with the high mass absorption coefficients exhibited by low energy x-rays, the detection and determination of low atomic-numbered elements by x-ray spectrometry is limited. However, an indirect approach based on the intensity ratio of Compton and Rayleigh scattered has been used to define light element components in alloys, plastics and other materials. This XRS technique provides qualitative and quantitative information about the overall constituents of a variety of samples.

  11. Non-destructive Evaluation of Bonds Between Fiberglass Composite and Metal

    NASA Technical Reports Server (NTRS)

    Zhao, Selina; Sonta, Kestutis; Perey, Daniel F.; Cramer, K. E.; Berger, Libby

    2015-01-01

    To assess the integrity and reliability of an adhesive joint in an automotive composite component, several non-destructive evaluation (NDE) methodologies are correlated to lap shear bond strengths. A glass-fabric-reinforced composite structure was bonded to a metallic structure with a two-part epoxy adhesive. Samples were subsequently cut and tested in shear, and flaws were found in some areas. This study aims to develop a reliable and portable NDE system for service-level adhesive inspection in the automotive industry. The results of the experimental investigation using several NDE methods are presented and discussed. Fiberglass-to-metal bonding is the ideal configuration for NDE via thermography using excitation with induction heating, due to the conductive metal and non-conductive glass-fiber-reinforced composites. Excitation can be either by a research-grade induction heater of highly defined frequency and intensity, or by a service-level heater, such as would be used for sealing windshields in a body shop. The thermographs thus produced can be captured via a high-resolution infrared camera, with principal component analysis and 2D spatial Laplacian processing. Alternatively, the thermographs can be captured by low resolution thermochromic microencapsulated liquid crystal film imaging, which needs no post-processing and can be very inexpensive. These samples were also examined with phased-array ultrasound. The NDE methods are compared to the lap shear values and to each other for approximate cost, accuracy, and time and level of expertise needed.

  12. Guided ultrasonic waves for non-destructive monitoring of the stress levels in prestressed steel strands.

    PubMed

    Chaki, S; Bourse, G

    2009-02-01

    The safety of prestressed civil structures such as bridges, dams, nuclear power plants, etc. directly involves the security of both environment and users. Health monitoring of the tensioning components, such as strands, tendons, bars, anchorage bolts, etc. is an important research topic and a challenging task bringing together the non-destructive evaluation (NDE) and civil engineering communities. This paper deals with a guided ultrasonic wave procedure for monitoring the stress levels in seven-wire steel strands (15.7 mm in diameter). The mechanical and geometrical characteristics of the prestressed strands were taken into account for optimizing the measurement configuration and then the choice of the guided ultrasonic mode at a suitable frequency. Simplified acoustoelastic formulations were derived from the acoustoelasticity theory according to either calibration test or in situ measurement. The results from acoustoelastic measurements on the seven-wire steel strands are presented and discussed in the case of calibration tests and industrially prestressed strands. They show the potential and the suitability of the proposed guided wave method for evaluating the stress levels in the tested seven-wire steel strands. PMID:18804832

  13. Ultra-portable, wireless smartphone spectrometer for rapid, non-destructive testing of fruit ripeness

    PubMed Central

    Das, Anshuman J.; Wahi, Akshat; Kothari, Ishan; Raskar, Ramesh

    2016-01-01

    We demonstrate a smartphone based spectrometer design that is standalone and supported on a wireless platform. The device is inherently low-cost and the power consumption is minimal making it portable to carry out a range of studies in the field. All essential components of the device like the light source, spectrometer, filters, microcontroller and wireless circuits have been assembled in a housing of dimensions 88 mm × 37 mm × 22 mm and the entire device weighs 48 g. The resolution of the spectrometer is 15 nm, delivering accurate and repeatable measurements. The device has a dedicated app interface on the smartphone to communicate, receive, plot and analyze spectral data. The performance of the smartphone spectrometer is comparable to existing bench-top spectrometers in terms of stability and wavelength resolution. Validations of the device were carried out by demonstrating non-destructive ripeness testing in fruit samples. Ultra-Violet (UV) fluorescence from Chlorophyll present in the skin was measured across various apple varieties during the ripening process and correlated with destructive firmness tests. A satisfactory agreement was observed between ripeness and fluorescence signals. This demonstration is a step towards possible consumer, bio-sensing and diagnostic applications that can be carried out in a rapid manner. PMID:27606927

  14. Development of a neutron measurement system in unified non-destructive assay for the PRIDE facility

    NASA Astrophysics Data System (ADS)

    Seo, Hee; Park, Se-Hwan; Won, Byung-Hee; Ahn, Seong-Kyu; Shin, Hee-Sung; Na, Sang-Ho; Song, Dae-Yong; Kim, Ho-Dong; Lee, Seung Kyu

    2013-12-01

    The Korea Atomic Energy Research Institute (KAERI) has made an effort to develop pyroprocessing technology to resolve an on-going problem in Korea, i.e., the management of spent nuclear fuels. To this end, a test-bed facility for pyroprocessing, called PRIDE (PyRoprocessing Integrated inactive DEmonstration facility), is being constructed at KAERI. The main objective of PRIDE is to evaluate the performance of the unit processes, remote operation, maintenance, and proliferation resistance. In addition, integrating all unit processes into a one-step process is also one of the main goals. PRIDE can also provide a good opportunity to test safeguards instrumentations for a pyroprocessing facility such as nuclear material accounting devices, surveillance systems, radiation monitoring systems, and process monitoring systems. In the present study, a non-destructive assay (NDA) system for the testing of nuclear material accountancy of PRIDE was designed by integrating three different NDA techniques, i.e., neutron, gamma-ray, and mass measurements. The developed neutron detection module consists of 56 3He tubes and 16 AMPTEK A111 signal processing circuits. The amplifiers were matched in terms of the gain and showed good uniformity after a gain-matching procedure (%RSD=0.37%). The axial and the radial efficiency distributions within the cavity were then measured using a 252Cf neutron source and were compared with the MCNPX calculation results. The measured efficiency distributions showed excellent agreement with the calculations, which confirmed the accuracy of the MCNPX model of the system.

  15. Wavelet-based subsurface defect characterization in pulsed phase thermography for non-destructive evaluation

    NASA Astrophysics Data System (ADS)

    Zauner, G.; Mayr, G.; Hendorfer, G.

    2009-02-01

    Active infrared thermography is a method for non-destructive testing (NDT) of materials and components. In pulsed thermography (PT), a brief and high intensity flash is used to heat the sample. The decay of the sample surface temperature is detected and recorded by an infrared camera. Any subsurface anomaly (e.g. inclusion, delamination, etc.) gives rise to a local temperature increase (thermal contrast) on the sample surface. Conventionally, in Pulsed Phase Thermography (PPT) the analysis of PT time series is done by means of Discrete Fourier Transform producing phase images which can suppress unwanted physical effects (due to surface emissivity variations or non-uniform heating). The drawback of the Fourier-based approach is the loss of temporal information, making quantitative inversion procedures tricky (e.g. defect depth measurements). In this paper the complex Morlet-Wavelet transform is used to preserve the time information of the signal and thus provides information about the depth of a subsurface defect. Additionally, we propose to use the according phase contrast value to derive supplementary information about the thermal reflection properties at the defect interface. This provides additional information (e.g. about the thermal mismatch factor between the specimen and the defect) making interpretation of PPT results easier and perhaps unequivocal.

  16. Image pixel guided tours: a software platform for non-destructive x-ray imaging

    NASA Astrophysics Data System (ADS)

    Lam, K. P.; Emery, R.

    2009-02-01

    Multivariate analysis seeks to describe the relationship between an arbitrary number of variables. To explore highdimensional data sets, projections are often used for data visualisation to aid discovering structure or patterns that lead to the formation of statistical hypothesis. The basic concept necessitates a systematic search for lower-dimensional representations of the data that might show interesting structure(s). Motivated by the recent research on the Image Grand Tour (IGT), which can be adapted to view guided projections by using objective indexes that are capable of revealing latent structures of the data, this paper presents a signal processing perspective on constructing such indexes under the unifying exploratory frameworks of Independent Component Analysis (ICA) and Projection Pursuit (PP). Our investigation begins with an overview of dimension reduction techniques by means of orthogonal transforms, including the classical procedure of Principal Component Analysis (PCA), and extends to an application of the more powerful techniques of ICA in the context of our recent work on non-destructive testing technology by element specific x-ray imaging.

  17. Non-destructive testing techniques for the forensic engineering investigation of reinforced concrete buildings.

    PubMed

    Hobbs, Brian; Tchoketch Kebir, Mohamed

    2007-04-11

    This study describes in detail the results of a laboratory investigation where the compressive strength of 150mm side-length cubes was evaluated. Non-destructive testing (NDT) was carried out using ultrasonic pulse velocity (UPV) and impact rebound hammer (IRH) techniques to establish a correlation with the compressive strengths of compression tests. To adapt the Schmidt hammer apparatus and the ultrasonic pulse velocity tester to the type of concrete used in Algeria, concrete mix proportions that are recommended by the Algerian code were chosen. The resulting correlation curve for each test is obtained by changing the level of compaction, water/cement ratio and concrete age of specimens. Unlike other works, the research highlights the significant effect of formwork material on surface hardness of concrete where two different mould materials for specimens were used (plastic and wood). A combined method for the above two tests, reveals an improvement in the strength estimation of concrete. The latter shows more improvement by including the concrete density. The resulting calibration curves for strength estimation were compared with others from previous published literature. PMID:16904854

  18. Non-destructive quantification of alignment of nanorods embedded in uniaxially stretched polymer films

    SciTech Connect

    Stoenescu, Stefan Packirisamy, Muthukumaran; Truong, Vo-Van

    2014-03-21

    Among several methods developed for uniaxial alignment of metallic nanorods for optical applications, alignment by film stretching consists in embedding the rods in a transparent thin film of thermoplastic polymer, followed by simultaneous heating and uniaxial stretching of the composite film. As to the quantification of the resulting alignment, it has been limited to statistical calculations based on microscopic examination, which is incomplete, subject to errors due to geometric distortions of the scanning electron microscope images and destructive, since it involves cutting of samples. In contrast, we present in this paper a non-destructive quantification of the average orientation of the rods, based on a probabilistic approach combined with numerical simulations of absorbance spectra and spectrometric characterization of the composite film. Assuming electromagnetically non-interacting rods, we consider the longitudinal absorbance peak of their ensemble to consist of the superposition of their individual spectra that we obtain by numerical simulation using the size and shape adapted dielectric function of the metal and the finite difference time domain method. The accuracy of the solution depends on the number of discretization intervals, the accuracy of the numerical simulations, and the accurate knowledge of the polydispersity of the rods. For the sake of concreteness, we used nanorods to describe the quantification steps but the method is equally valid for any dichroic particles.

  19. Nitrogen Concentration Estimation in Tomato Leaves by VIS-NIR Non-Destructive Spectroscopy

    PubMed Central

    Ulissi, Valentina; Antonucci, Francesca; Benincasa, Paolo; Farneselli, Michela; Tosti, Giacomo; Guiducci, Marcello; Tei, Francesco; Costa, Corrado; Pallottino, Federico; Pari, Luigi; Menesatti, Paolo

    2011-01-01

    Nitrogen concentration in plants is normally determined by expensive and time consuming chemical analyses. As an alternative, chlorophyll meter readings and N-NO3 concentration determination in petiole sap were proposed, but these assays are not always satisfactory. Spectral reflectance values of tomato leaves obtained by visible-near infrared spectrophotometry are reported to be a powerful tool for the diagnosis of plant nutritional status. The aim of the study was to evaluate the possibility and the accuracy of the estimation of tomato leaf nitrogen concentration performed through a rapid, portable and non-destructive system, in comparison with chemical standard analyses, chlorophyll meter readings and N-NO3 concentration in petiole sap. Mean reflectance leaf values were compared to each reference chemical value by partial least squares chemometric multivariate methods. The correlation between predicted values from spectral reflectance analysis and the observed chemical values showed in the independent test highly significant correlation coefficient (r = 0.94). The utilization of the proposed system, increasing efficiency, allows better knowledge of nutritional status of tomato plants, with more detailed and sharp information and on wider areas. More detailed information both in space and time is an essential tool to increase and stabilize crop quality levels and to optimize the nutrient use efficiency. PMID:22163962

  20. Research Based on Optical Non-Destructive Testing of Pigment Identification.

    PubMed

    Wang, Jigang; Hao, Shengcai; Zhou, Wenhua; Qi, Xiaokun; Shi, Jilong

    2016-04-01

    Optical Non-Destructive Testing (ONDT) can be applied as penetrating elemental and structure analysis technology in the Pigments identification field. Three-dimensional video microscopy, Raman microscopy and energy dispersive X-ray fluorescence spectroscopy are employed to measure the materials based on a Qing Dynasty meticulous painting. The results revealed that the dark yellow area within the decorative patterns was presented due to the interaction of Emerald green and hematite, and the bright yellow edge area was delineated by Cu-Zn-Pb composition. The interesting thing is that an artificial synthetic ultramarine blue was checked in the painting. According to the first synthesized time of ultramarine blue and Paris green, the time limit of the painting completion can be identified. The principle of Pigment subtractive colorant and nitikaset method were employed to interpreting the results. Optical testing combined with the area of cultural relic identification can be a potential method to build an expert identification system successfully. This work also help lay the optical method groundwork for further cultural relic identification, sterilization, and preservation. PMID:27451669

  1. Nitrogen concentration estimation in tomato leaves by VIS-NIR non-destructive spectroscopy.

    PubMed

    Ulissi, Valentina; Antonucci, Francesca; Benincasa, Paolo; Farneselli, Michela; Tosti, Giacomo; Guiducci, Marcello; Tei, Francesco; Costa, Corrado; Pallottino, Federico; Pari, Luigi; Menesatti, Paolo

    2011-01-01

    Nitrogen concentration in plants is normally determined by expensive and time consuming chemical analyses. As an alternative, chlorophyll meter readings and N-NO(3) concentration determination in petiole sap were proposed, but these assays are not always satisfactory. Spectral reflectance values of tomato leaves obtained by visible-near infrared spectrophotometry are reported to be a powerful tool for the diagnosis of plant nutritional status. The aim of the study was to evaluate the possibility and the accuracy of the estimation of tomato leaf nitrogen concentration performed through a rapid, portable and non-destructive system, in comparison with chemical standard analyses, chlorophyll meter readings and N-NO(3) concentration in petiole sap. Mean reflectance leaf values were compared to each reference chemical value by partial least squares chemometric multivariate methods. The correlation between predicted values from spectral reflectance analysis and the observed chemical values showed in the independent test highly significant correlation coefficient (r = 0.94). The utilization of the proposed system, increasing efficiency, allows better knowledge of nutritional status of tomato plants, with more detailed and sharp information and on wider areas. More detailed information both in space and time is an essential tool to increase and stabilize crop quality levels and to optimize the nutrient use efficiency. PMID:22163962

  2. Non-destructive inspection of drilled holes in reinforced honeycomb sandwich panels using active thermography

    NASA Astrophysics Data System (ADS)

    Usamentiaga, R.; Venegas, P.; Guerediaga, J.; Vega, L.; López, I.

    2012-11-01

    The aerospace industry is in constant need of ever-more efficient inspection methods for quality control. Product inspection is also essential to maintain the safe operation of aircraft components designed to perform for decades. This paper proposes a method for non-destructive inspection of drilled holes in reinforced honeycomb sandwich panels. Honeycomb sandwich panels are extensively employed in the aerospace industry due to their high strength and stiffness to weight ratios. In order to attach additional structures to them, panels are reinforced by filling honeycomb cells and drilling holes into the reinforced areas. The proposed procedure is designed to detect the position of the holes within the reinforced area and to provide a robust measurement of the distance between each hole and the boundary of the reinforced area. The result is a fast, safe and clean inspection method for drilled holes in reinforced honeycomb sandwich panels that can be used to robustly assess a possible displacement of the hole from the center of the reinforced area, which could have serious consequences. The proposed method is based on active infrared thermography, and uses state of the art methods for infrared image processing, including signal-to-nose ratio enhancement, hole detection and segmentation. Tests and comparison with X-ray inspections indicate that the proposed system meets production needs.

  3. Non-destructive testing of ceramic balls using high frequency ultrasonic resonance spectroscopy.

    PubMed

    Petit, S; Duquennoy, M; Ouaftouh, M; Deneuville, F; Ourak, M; Desvaux, S

    2005-12-01

    Although ceramic balls are used more and more for bearings in the aerospace and space industries, defects in this type of ceramic material could be dangerous, particularly if such defects are located close to the surface. In this paper, we propose a non-destructive testing method for silicon nitride balls, based on ultrasonic resonance spectroscopy. Through the theoretical study of their elastic vibrations, it is possible to characterize the balls using a vibration mode that is similar to surface wave propagation. The proposed methodology can both excite spheroidal vibrations in the ceramic balls and detect such vibrations over a large frequency range. Studying their resonance spectrums allows the balls' elastic parameters be characterized. Ours is an original method that can quickly estimate the velocity of surface waves using high frequency resonances, which permits surface and sub-surface areas to be tested specifically. Two applications are described in this paper. Both use velocity measurements to achieve their different goals, the first to differentiate between flawless balls from different manufacturing processes, and the second to detect small defects, such as cracks. Our method is rapid and permits the entire ceramic ball to be tested in an industrial context. PMID:16083931

  4. Non-destructive state detection for quantum logic spectroscopy of molecular ions.

    PubMed

    Wolf, Fabian; Wan, Yong; Heip, Jan C; Gebert, Florian; Shi, Chunyan; Schmidt, Piet O

    2016-02-25

    Precision laser spectroscopy of cold and trapped molecular ions is a powerful tool in fundamental physics--used, for example, in determining fundamental constants, testing for their possible variation in the laboratory, and searching for a possible electric dipole moment of the electron. However, the absence of cycling transitions in molecules poses a challenge for direct laser cooling of the ions, and for controlling and detecting their quantum states. Previously used state-detection techniques based on photodissociation or chemical reactions are destructive and therefore inefficient, restricting the achievable resolution in laser spectroscopy. Here, we experimentally demonstrate non-destructive detection of the quantum state of a single trapped molecular ion through its strong Coulomb coupling to a well controlled, co-trapped atomic ion. An algorithm based on a state-dependent optical dipole force changes the internal state of the atom according to the internal state of the molecule. We show that individual quantum states in the molecular ion can be distinguished by the strength of their coupling to the optical dipole force. We also observe quantum jumps (induced by black-body radiation) between rotational states of a single molecular ion. Using the detuning dependence of the state-detection signal, we implement a variant of quantum logic spectroscopy of a molecular resonance. Our state-detection technique is relevant to a wide range of molecular ions, and could be applied to state-controlled quantum chemistry and to spectroscopic investigations of molecules that serve as probes for interstellar clouds. PMID:26855427

  5. Non-destructive mobile monitoring of microbial contaminations on meat surfaces using porphyrin fluorescence intensities.

    PubMed

    Durek, J; Fröhling, A; Bolling, J; Thomasius, R; Durek, P; Schlüter, O K

    2016-05-01

    A non-destructive mobile system for meat quality monitoring was developed and investigated for the possible application along the whole production chain of fresh meat. Pork and lamb meat was stored at 5 °C for up to 20 days post mortem and measured with a fluorescence spectrometer. Additionally, the bacterial influence on the fluorescence signals was evaluated by different experimental procedures. Fluorescence of NADH and different porphyrins could be correlated to the growth of diverse bacteria and hence used for contamination monitoring. The increase of porphyrin fluorescence started after 9 days p.m. for pork and after 2 days p.m. for lamb meat. Based on the results, a mobile fluorescence system was built and compared with the laboratory system. The corrected function of the meat slices showed a root mean square error of 1156.97 r.u. and a mean absolute percentage error of 12.59%; for lamb the values were 470.81 r.u. and 15.55%, respectively. A mobile and non-invasive measurement system would improve the microbial security of fresh meat. PMID:26773794

  6. Non-destructive Assay Measurements Using the RPI Lead Slowing Down Spectrometer

    SciTech Connect

    Becker, Bjorn; Weltz, Adam; Kulisek, Jonathan A.; Thompson, J. T.; Thompson, N.; Danon, Yaron

    2013-10-01

    The use of a Lead Slowing-Down Spectrometer (LSDS) is consid- ered as a possible option for non-destructive assay of fissile material of used nuclear fuel. The primary objective is to quantify the 239Pu and 235U fissile content via a direct measurement, distinguishing them through their characteristic fission spectra in the LSDS. In this pa- per, we present several assay measurements performed at the Rensse- laer Polytechnic Institute (RPI) to demonstrate the feasibility of such a method and to provide benchmark experiments for Monte Carlo cal- culations of the assay system. A fresh UOX fuel rod from the RPI Criticality Research Facility, a 239PuBe source and several highly en- riched 235U discs were assayed in the LSDS. The characteristic fission spectra were measured with 238U and 232Th threshold fission cham- bers, which are only sensitive to fission neutron with energy above the threshold. Despite the constant neutron and gamma background from the PuBe source and the intense interrogation neutron flux, the LSDS system was able to measure the characteristic 235U and 239Pu responses. All measurements were compared to Monte Carlo simula- tions. It was shown that the available simulation tools and models are well suited to simulate the assay, and that it is possible to calculate the absolute count rate in all investigated cases.

  7. Non-destructive inspection using HTS SQUID on aluminum liner covered by CFRP

    NASA Astrophysics Data System (ADS)

    Hatsukade, Y.; Yotsugi, K.; Sakaguchi, Y.; Tanaka, S.

    2007-10-01

    An eddy-current-based SQUID non-destructive inspection (NDI) system to detect deep-lying cracks in multi-layer composite-Al vessels was developed taking advantage of the uncontested sensitivity of HTS-SQUID in low-frequency range. An HTS-SQUID gradiometer was mounted in a pulse tube cryocooler. A pair of differential coils with C-shaped ferrite cores was employed to induce an enhanced eddy current in an Al vessel wrapped in a carbon fiber reinforced plastic (CFRP) cover. Ellipsoidal dome-shaped Al liners containing through cracks, which were made by pressure cycle tests, in the CFRP covers with total thickness of 6 mm (CFPR 3 mm, and Al 3 mm) were inspected by the system. While inducing eddy currents in the vessels with excitation fields at 100 Hz or 7 kHz, the vessels were rotated under the HTS-SQUID. Above the cracks, anomalous signals due to the cracks were clearly detected at both frequencies. These results suggested the SQUID-NDI technique would be a possible candidate for inspection of high-pressure multi-layer composite-Al vessels.

  8. Non-destructive characterization of microdamage in cortical bone using low field pulsed NMR.

    PubMed

    Nicolella, Daniel P; Ni, Qingwen; Chan, Kwai S

    2011-04-01

    The microcracking and damage accumulation process in human cortical bone was characterized by performing cyclic loading under four-point bending at ambient temperature. A non-destructive nuclear magnetic resonance (NMR) spin-spin (T(2)) relaxation technique was applied to quantify the apparent changes in bone porosity as a function of cyclic loading and prior damage accumulation, first to unloaded cortical bone to quantify the initial porosity and then to fatigued cortical bone that was subjected to cyclic loading to various levels of modulus degradation and microdamage in the form of microcracks. The NMR T(2) relaxation time and amplitude data of the fatigued bone were compared against the undamaged state. The difference in the T(2) relaxation time data was taken as a measure of the increase in pore size, bone porosity or microcrack density due to microdamage induced by cyclic loading. A procedure was developed to deduce the number and size distributions of microcracks formed in cortical bone. Serial sectioning of the fatigued bone showed the formation of microcracks along the cement lines or within the interstitial tissue. The results on the evolution of microdamage derived from NMR measurements were verified by independent experimental measurements of microcrack density using histological characterization techniques. The size distribution and population of the microcracks were then utilized in conjunction with an analytical model to predict the degradation of the elastic modulus of cortical bone as a function of damage accumulation. PMID:21316626

  9. NON-DESTRUCTIVE RADIOCARBON DATING: NATURALLY MUMMIFIED INFANT BUNDLE FROM SW TEXAS

    SciTech Connect

    Steelman, K L; Rowe, M W; Turpin, S A; Guilderson, T P; Nightengale, L

    2004-09-07

    Plasma oxidation was used to obtain radiocarbon dates on six different materials from a naturally mummified baby bundle from the Lower Pecos River region of southwest Texas. This bundle was selected because it was thought to represent a single event and would illustrate the accuracy and precision of the plasma oxidation method. Five of the materials were clearly components of the original bundle with 13 dates combined to yield a weighted average of 2135 {+-} 11 B.P. Six dates from a wooden stick of Desert Ash averaged 939 {+-} 14 B.P., indicating that this artifact was not part of the original burial. Plasma oxidation is shown to be a virtually non-destructive alternative to combustion. Because only sub-milligram amounts of material are removed from an artifact over its exposed surface, no visible change in fragile materials has been observed, even under magnification. The method is best applied when natural organic contamination is unlikely and serious consideration of this issue is needed in all cases. If organic contamination is present, it will have to be removed before plasma oxidation to obtain accurate radiocarbon dates.

  10. Non-destructive assessment of mechanical properties of microcrystalline cellulose compacts.

    PubMed

    Palomäki, Emmi; Ehlers, Henrik; Antikainen, Osmo; Sandler, Niklas; Yliruusi, Jouko

    2015-11-30

    In the present study the mechanical properties of microcrystalline cellulose compacts compressed were studied. The resistance to crushing was tested using diametral compression testing and apparent Young's modulus was determined using consecutive uniaxial compression of the full cross-sectional area of single tablets. As non-elastic deformation during the first compression cycle and reverse plasticity were discovered, the loading phase of the second compression cycle was used to determine Young's modulus. The relative standard deviation of 10 consecutive measurements was 3.6%. The results indicate a direct correlation between crushing strength and Young's modulus, which found further support when comparing surface roughness data and radial recovery of the tablets to Young's modulus. The extrapolated elastic modulus at zero-porosity was found to be 1.80±0.08 GPa, which is slightly lower than previously reported values, confirming the complexity of measuring the elastic properties of microcrystalline cellulose compacts. The method can be used for non-destructive assessment of mechanical properties of powder compacts for example during storage studies. PMID:26410756

  11. Non-destructive determination of anisotropic mechanical properties of pharmaceutical solid dosage forms.

    PubMed

    Akseli, I; Hancock, B C; Cetinkaya, C

    2009-07-30

    The mechanical property anisotropy of compacts made from four commercially available pharmaceutical excipient powders (microcrystalline cellulose, lactose monohydrate, ascorbic acid, and aspartame) was evaluated. The speed of pressure (longitudinal) waves in the uni-axially compressed cubic compacts of each excipient in the three principle directions was determined using a contact ultrasonic method. Average Young's moduli of each compact in the axial (x) and radial (y and z) directions were characterized. The contact ultrasonic measurements revealed that average Young's modulus values vary with different testing orientations which indicate Young's modulus anisotropy in the compacts. The extent of Young's modulus anisotropy was quantified by using a dimensionless ratio and was found to be significantly different for each material (microcrystalline cellulose>lactose>aspartame>ascorbic acid). It is also observed that using the presented contact method, compacts at high solid fraction (0.857-0.859) could be differentiated than those at the solid fraction of 0.85 in their groups. The presented contact ultrasonic method is an attractive tool since it has the advantages of being sensitive to solid fraction ratio, non-destructive, requiring small amount of material and rapid. It is noteworthy that, since the approach provides insight into the performance of common pharmaceutical materials and fosters increased process knowledge, it can be applied to broaden the understanding of the effect of the mechanical properties on the performance (e.g., disintegration profiles) of solid oral dosage forms. PMID:19426791

  12. Non-destructive provenance differentiation of prehistoric pigments by external PIXE

    NASA Astrophysics Data System (ADS)

    Beck, L.; Salomon, H.; Lahlil, S.; Lebon, M.; Odin, G. P.; Coquinot, Y.; Pichon, L.

    2012-02-01

    The elemental analysis of minerals/rocks has been often used for the determination of their geological origin. When these natural rocks were exploited by prehistoric civilizations as objects, weapons, or pigments, the composition of the minerals can provide information on the mobility, the exchanges and the interaction between groups of population. In this paper, we will present results obtained from archaeological samples of prehistoric pigments, mainly iron and manganese oxides. PIXE analysis has been applied to samples of the prehistoric cave "La grotte du Renne" in Arcy-sur-Cure, France (Chatelperronian, 38,000-34,000 BP). Because most of the archaeological objects are decorated or display some use marks, it is not possible to take samples. Consequently, we have used a non-destructive technique thanks to the external beam of AGLAE (C2RMF, Paris). In order to improve the limits of detection (LOD less than 10 ppm from Cu to Sb), a metal absorber has been placed on the X-ray detector to preferentially filter the Fe-K or Mn-K lines. Based on the quantitative analysis of major and trace elements, we have obtained groups of compositions corresponding to different geological sources. We demonstrate in this study that it is possible to extend PIXE analysis to the characterization of prehistoric pigments such as iron and manganese oxides for differentiating potential sources of pigments in archaeological contexts.

  13. Non-destructive analysis of DU content in the NIF hohlraums

    SciTech Connect

    Gharibyan, Narek; Moody, Ken J.; Shaughnessy, Dawn A.

    2015-12-16

    The advantage of using depleted uranium (DU) hohlraums in high-yield deuterium-tritium (DT) shots at the National Ignition Facility (NIF) is addressed by Döppner, et al., in great detail [1]. This DU based hohlraum incorporates a thin layer of DU, ~7 μm thick, on the inner surface along with a thin layer of a gold coating, ~0.7 μm thick, while the outer layer is ~22 μm thick gold. A thickness measurement of the DU layer can be performed using an optical microscope where the total DU weight can be computed provided a uniform DU layer. However, the uniformity of the thickness is not constant throughout the hohlraum since CAD drawing calculations of the DU weight do not agree with the computed values from optical measurements [2]. Therefore, a non-destructive method for quantifying the DU content in hohlraums has been established by utilizing gamma-ray spectroscopy. The details of this method, along with results from several hohlraums, are presented in this report.

  14. Feasibility for non-destructive discrimination of natural and beryllium-diffused sapphires using Raman spectroscopy.

    PubMed

    Chang, Kyeol; Lee, Sanguk; Park, Jimin; Chung, Hoeil

    2016-03-01

    Raman spectroscopy based non-destructive discrimination between natural and beryllium-diffused (Be-diffused) sapphires has been attempted. The initial examination of Raman image acquired on a sapphire revealed that microscopic structural and compositional heterogeneity was apparent in the sample, so acquisition of spectra able to represent a whole body of sapphire rather than a localized area was necessary for a reliable discrimination. For this purpose, a wide area illumination (WAI) scheme (illumination area: 28.3mm(2)) providing a large sampling volume was employed to collect representative Raman spectra of sapphires. Upon the diffusion of Be into a sapphire, the band shift originated from varied lattice structure by substitution of Be at cation sites was observed and utilized as a valuable spectral signature for the discrimination. In the domain of principal component (PC) scores, the groups of natural and Be-diffused sapphires were identifiable with minor overlapping and the cross-validated discrimination error was 7.3% when k-Nearest Neighbor (k-NN) was used as a classifier. PMID:26717849

  15. X-ray based methods for non-destructive testing and material characterization

    NASA Astrophysics Data System (ADS)

    Hanke, Randolf; Fuchs, Theobald; Uhlmann, Norman

    2008-06-01

    The increasing complexity and miniaturization in the field of new materials as well as in micro-production requires in the same way improvements and technical advances in the field of micro-NDT to provide better quality data and more detailed knowledge about the internal structures of micro-components. Therefore, non-destructive methods like radioscopy, ultrasound, optical or thermal imaging increasingly gain in importance with respect to ongoing product and material development in the different phases like material characterization, production control or module reliability testing. Because of the manifold different application fields, i.e., certain physical NDT methods applied to material inspection, characterization or reliability testing, this contribution will focus on the radioscopic-based methods related to their most important applications. Today, in modern industrial quality control, X-ray transmission is used in two different ways: Two-dimensional radioscopic transmission imaging (projection technique), usually applied to inline inspection tasks in application fields like lightweight material production, electronic component soldering or food production. Computed tomography (CT) for generation of three-dimensional data, representing spatial information and density distribution of objects. CT application fields are on the one hand the understanding of production process failure or component and module inspection (completeness) and on the other hand the dimensional measuring of hidden geometrical outlines (metrology). This paper demonstrates the methods including technical set-ups (X-ray source and detector), imaging and reconstruction results and the methods for high speed and high-resolution volume data generation and evaluation.

  16. Passive Neutron Non-Destructive Assay for Remediation of Radiological Waste at Hanford Burial Grounds- 13189

    SciTech Connect

    Simpson, A.; Pitts, M.; Ludowise, J.D.; Valentinelli, P.; Grando, C.J.; Haggard, D.L.

    2013-07-01

    The Hanford burial grounds contains a broad spectrum of low activity radioactive wastes, transuranic (TRU) wastes, and hazardous wastes including fission products, byproduct material (thorium and uranium), plutonium and laboratory chemicals. A passive neutron non-destructive assay technique has been developed for characterization of shielded concreted drums exhumed from the burial grounds. This method facilitates the separation of low activity radiological waste containers from TRU waste containers exhumed from the burial grounds. Two identical total neutron counting systems have been deployed, each consisting of He-3 detectors surrounded by a polyethylene moderator. The counts are processed through a statistical filter that removes outliers in order to suppress cosmic spallation events and electronic noise. Upon completion of processing, a 'GO / NO GO' signal is provided to the operator based on a threshold level equivalent to 0.5 grams of weapons grade plutonium in the container being evaluated. This approach allows instantaneous decisions to be made on how to proceed with the waste. The counting systems have been set up using initial on-site measurements (neutron emitting standards loaded into surrogate waste containers) combined with Monte Carlo modeling techniques. The benefit of this approach is to allow the systems to extend their measurement ranges, in terms of applicable matrix types and container sizes, with minimal interruption to the operations at the burial grounds. (authors)

  17. Non-destructive testing of composite materials by means of active thermography-based tools

    NASA Astrophysics Data System (ADS)

    Lizaranzu, Miguel; Lario, Alberto; Chiminelli, Agustín; Amenabar, Ibán

    2015-07-01

    Infrared analysis tools are nowadays widely used for the non-destructive testing of components made up in composite materials, belonging to many different industrial sectors. Being a non-contact method, its capability for the inspection of large areas in short periods of time justifies the great number of works and technical studies that can be found in this field. The growing interest in the technique is also supported by the development, during recent years, of increasingly powerful equipment and data analysis tools. In order to establish a base of knowledge to assist defect identification in real components inspections, the design and manufacturing of inspection samples including controlled defects, is a frequently used strategy. This paper deals with the analysis, by means of transient active thermography, of a set of inspection patterns made out of different composite materials and configurations that can be found in the wind turbine blade manufacturing industry. The design and manufacturing of these patterns are described, including different types of representative defects, stack configurations and composite manufacturing techniques. Reference samples are then inspected by means of active thermography analysis tools and the results obtained are discussed.

  18. Combined non-destructive XRF and SR-XAS study of archaeological artefacts.

    PubMed

    Bardelli, Fabrizio; Barone, Germana; Crupi, Vincenza; Longo, Francesca; Majolino, Domenico; Mazzoleni, Paolo; Venuti, Valentina

    2011-03-01

    We report on a non-destructive study of Sicilian ceramic fragments of cultural heritage interest, classified as "proto-majolica" pottery and dating back to the twelfth to thirteen centuries AD. The analytical approach used is based on the employment of two totally non-invasive spectroscopic techniques: X-ray fluorescence (XRF), using a portable energy-dispersive XRF analyser, and X-ray absorption spectroscopy, using synchrotron radiation as a probe (SR-XAS). XRF measurements allowed us to collect elemental and spatially resolved information on major and minor constituents of the decorated coating of archaeological pottery fragments, so providing preliminary results on the main components characterizing the surface. In particular, we assigned to Fe and Mn the role of key elements of the colouring agent. With the aim of obtaining more detailed information, we performed SR-XAS measurements at the Fe and Mn K-edges at the Italian BM08 beamline at the European Synchrotron Radiation Facility (Grenoble, France). The experimental data were analysed by applying principal component analysis and least-squares fitting to the near-edge part of the spectra (X-ray absorption near-edge structure) to determine the samples' speciation. From the overall results, umber, a class of brownish pigments characterized by a mixture of hydrated iron and manganese oxides, has been ascribed as a pigmenting agent. PMID:21311873

  19. From local to global analysis of defect detectability in infrared non-destructive testing

    NASA Astrophysics Data System (ADS)

    Florez-Ospina, J. F.; Benitez, H. D.

    2014-03-01

    Several image processing techniques are employed in Infrared Non-Destructive Testing (IRNDT) to enhance defect detectability. To date, there is no adequate global measurement that objectively assesses defect visibility in processed frames. In this work, a Global Signal to Noise Ratio (GSNR) that comprehensively evaluates defect detectability in processed infrared (IR) images is proposed, as well as a defect visibility measure named Infrared Image Quality Index (IRIQI) that compares the structural information of defective and sound areas. In addition, GSNR and IRIQI are validated by using the area under ROC curve (AUC). AUC quantitatively assesses defect visibility by comparing the outcomes of processing techniques to human judgements. The remarkable benefit of this global approach is that it allows one to determine the frame at which processing techniques reveals the majority of the defects by evaluating the times at which AUC curves reach their maxima. The test pieces were a Carbon-Fiber Reinforced Plastic (CFRP) sample containing delaminations and a honeycomb specimen with delaminations, skin unbonds, excessive adhesive, and crushed core.

  20. Quantitative impact characterization of aeronautical CFRP materials with non-destructive testing methods

    NASA Astrophysics Data System (ADS)

    Kiefel, Denis; Stoessel, Rainer; Grosse, Christian

    2015-03-01

    In recent years, an increasing number of safety-relevant structures are designed and manufactured from carbon fiber reinforced polymers (CFRP) in order to reduce weight of airplanes by taking the advantage of their specific strength into account. Non-destructive testing (NDT) methods for quantitative defect analysis of damages are liquid- or air-coupled ultrasonic testing (UT), phased array ultrasonic techniques, and active thermography (IR). The advantage of these testing methods is the applicability on large areas. However, their quantitative information is often limited on impact localization and size. In addition to these techniques, Airbus Group Innovations operates a micro x-ray computed tomography (μ-XCT) system, which was developed for CFRP characterization. It is an open system which allows different kinds of acquisition, reconstruction, and data evaluation. One main advantage of this μ-XCT system is its high resolution with 3-dimensional analysis and visualization opportunities, which enables to gain important quantitative information for composite part design and stress analysis. Within this study, different NDT methods will be compared at CFRP samples with specified artificial impact damages. The results can be used to select the most suitable NDT-method for specific application cases. Furthermore, novel evaluation and visualization methods for impact analyzes are developed and will be presented.