NMR investigations of surfaces and interfaces using spin-polarized xenon

International Nuclear Information System (INIS)

Gaede, H.C.; Lawrence Berkeley Lab., CA

1995-07-01

129 Xe NMR is potentially useful for the investigation of material surfaces, but has been limited to high surface area samples in which sufficient xenon can be loaded to achieve acceptable signal to noise ratios. In Chapter 2 conventional 129 Xe NMR is used to study a high surface area polymer, a catalyst, and a confined liquid crystal to determine the topology of these systems. Further information about the spatial proximity of different sites of the catalyst and liquid crystal systems is determined through two dimensional exchange NMR in Chapter 3. Lower surface area systems may be investigated with spin-polarized xenon, which may be achieved through optical pumping and spin exchange. Optically polarized xenon can be up to 10 5 times more sensitive than thermally polarized xenon. In Chapter 4 highly polarized xenon is used to examine the surface of poly(acrylonitrile) and the formation of xenon clathrate hydrates. An attractive use of polarized xenon is as a magnetization source in cross polarization experiments. Cross polarization from adsorbed polarized xenon may allow detection of surface nuclei with drastic enhancements. A non-selective low field thermal mixing technique is used to enhance the 13 C signal of CO 2 of xenon occluded in solid CO 2 by a factor of 200. High-field cross polarization from xenon to proton on the surface of high surface area polymers has enabled signal enhancements of ∼1,000. These studies, together with investigations of the efficiency of the cross polarization process from polarized xenon, are discussed in Chapter 5. Another use of polarized xenon is as an imaging contrast agent in systems that are not compatible with traditional contrast agents. The resolution attainable with this method is determined through images of structured phantoms in Chapter 6

Impact of opal nanoconfinement on electronic properties of sodium particles: NMR studies

Energy Technology Data Exchange (ETDEWEB)

Charnaya, E.V., E-mail: charnaya@live.com [Department of Physics, National Cheng Kung University, Tainan, 70101 Taiwan (China); Institute of Physics, St. Petersburg State University, St. Petersburg, 198504 (Russian Federation); Lee, M.K. [Department of Physics, National Cheng Kung University, Tainan, 70101 Taiwan (China); MoST Instrument Center at NCKU, Tainan, 70101 Taiwan (China); Chang, L.J. [Department of Physics, National Cheng Kung University, Tainan, 70101 Taiwan (China); Kumzerov, Yu.A.; Fokin, A.V. [A.F. Ioffe Physico-Technical Institute RAS, St. Petersburg, 194021 (Russian Federation); Samoylovich, M.I. [Moscow Institute of Physics and Technology, Moscow, 141700 (Russian Federation); Bugaev, A.S. [CSR Institute of Technology “Technomash”, Moscow, 121108 (Russian Federation)

2015-03-20

The {sup 23}Na Knight shift of NMR line which is highly correlated with the electron spin susceptibility and density of states at the Fermi level was studied for the sodium loaded opal. The measurements were carried out within a temperature range from 100 to 400 K for solid and melted confined sodium nanoparticles. The NMR line below 305 K was a singlet with the Knight shift reduced compared to that in bulk. Above this temperature the NMR line split reproducibly into two components with opposite trends in the Knight shift temperature dependences which evidenced a nanoconfinement-induced transformation and heterogeneity in the electron system. The findings were suggested to be related to changes in the topology of the Fermi surface.

New insight into hydration and aging mechanisms of paper by the line shape analysis of proton NMR spectra

International Nuclear Information System (INIS)

Mallamace, D.; Vasi, S.; Missori, M.; Corsaro, C.

2016-01-01

The action of water within biological systems is strictly linked either with their physical chemical properties and with their functions. Cellulose is one of the most studied biopolymers due to its biological importance and its wide use in manufactured products. Among them, paper is mainly constituted by an almost equimolar ratio of cellulose and water. Therefore the study of the behavior of water within pristine and aged paper samples can help to shed light on the degradation mechanisms that irremediably act over time and spoil paper. In this work we present Nuclear Magnetic Resonance (NMR) experiments on modern paper samples made of pure cellulose not aged and artificially aged as well as on ancient paper samples made in 1413 in Perpignan (France). The line shape parameters of the proton NMR spectra were studied as a function of the hydration content. Results indicate that water in aged samples is progressively involved in the hydration of the byproducts of cellulose degradation. This enhances the degradation process itself through the progressive consumption of the cellulose amorphous regions.

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-08-01

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

NMR detects molecular interactions of graphene with aromatic and aliphatic hydrocarbons in water

Science.gov (United States)

Bichenkova, Elena V.; Raju, Arun P. A.; Burusco, Kepa K.; Kinloch, Ian A.; Novoselov, Kostya S.; Clarke, David J.

2018-03-01

Polyaromatic carbon is widely held to be strongly diamagnetic and hydrophobic, with textbook van der Waals and ‘π-stacked’ binding of hydrocarbons, which disrupt their self-assembled supramolecular structures. The NMR of organic molecules sequestered by polyaromatic carbon is expected to be dominated by shielding from the orbital diamagnetism of π electrons. We report the first evidence of very different polar and magnetic behavior in water, wherein graphene remained well-dispersed after extensive dialysis and behaved as a 1H-NMR-silent ghost. Magnetic effects dominated the NMR of organic structures which interacted with graphene, with changes in spin-spin coupling, vast increase in relaxation, line broadening and decrease in NMR peak heights when bound to graphene. However, the interactions were weak, reversible and did not disrupt organic self-assemblies reliant on hydrophobic ‘π-stacking’, even when substantially sequestered on the surface of graphene by the high surface area available. Interacting assemblies of aromatic molecules retained their strongly-shielded NMR signals and remained within self-assembled structures, with slower rates of diffusion from association with graphene, but with no further shielding from graphene. Binding to graphene was selective for positively-charged organic assemblies, weaker for non-aromatic and negligible for strongly-negatively-charged molecules, presumably repelled by a negative zeta potential of graphene in water. Stronger binders, or considerable excess of weaker binders readily reversed physisorption, with no evidence of structural changes from chemisorption. The fundamental nature of these different electronic interactions between organic and polyaromatic carbon is considered with relevance to electronics, charge storage, sensor, medical, pharmaceutical and environmental research.

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

Directory of Open Access Journals (Sweden)

Michael D. Pinter

2014-03-01

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

Nitrogen Use Efficiency and Carbon Isotope Discrimination Study on NMR151 and NMR152 Mutant Lines Rice at Field Under Different Nitrogen Rates and Water Potentials

International Nuclear Information System (INIS)

Ahmad Nazrul Abdul Wahid; Shyful Azizi Abdul Rahman; Abdul Rahim Harun; Latiffah Nordin; Abdul Razak Ruslan; Hazlina Abdullah; Khairuddin Abdul Rahim

2016-01-01

This study was conducted to evaluate the nitrogen use efficiency and "1"3C isotope discrimination of rice mutant lines viz. NMR151 and NMR152. Both cultivars are developed under rice radiation mutagenesis programme for adaptability to aerobic conditions. In the present study, NMR151 and NMR152 were grown under conditions of varying water potentials and nitrogen levels in a field. Two water potentials and three nitrogen rates in a completely randomized design with three replications were carried out. The rice mutants were grown for 110 days under two water potentials, (i) Field capacity from 0 to 110 DAS [FC], and (ii) Field capacity from 0 to 40 DAS and 30 % dry of field capacity from 41 to 110 DAS [SS] and three nitrogen rates, (i) 0 kg N/ ha (0N), (ii) 60 kg N/ ha (60N), and (iii) 120 kg N/ ha (120N). "1"5N isotopic tracer technique was used in this study, whereby the "1"5N labeled urea fertilizer 5.20 % atom excess (a.e) was utilized as a tracer for nitrogen use efficiency (NUE) study. "1"5N isotope presence in the samples was determined using emission spectrometry and percentage of total nitrogen was determined by the Kjeldahl method. "1"5N a.e values of the samples were used in the determination of the NUE. The value of "1"3C isotope discrimination (Δ"1"3C) in the sample was determined using isotope ratio mass spectrometry (IRMS). The "1"3C isotope discrimination technique was used as a tool to identify drought resistance rice cultivars with improves water use efficiency. The growth and agronomy data, viz. plant height, number of tillers, grain yield, straw yield, and 1000 grain weight also were recorded. Results from this study showed nitrogen rates imparted significant effects on yield (grain and straw) plant height, number of tillers and 1000 grain weight. Water potentials had significant effects only on 1000 grain weight and Δ"1"3C. The NUE for both mutant lines rice showed no significant different between treatments. Both Rice mutant lines rice NMR151

Hyperpolarized Xenon Nuclear Magnetic Resonance (NMR of Building Stone Materials

Directory of Open Access Journals (Sweden)

Michele Mauri

2012-09-01

Full Text Available We have investigated several building stone materials, including minerals and rocks, using continuous flow hyperpolarized xenon (CF-HP NMR spectroscopy to probe the surface composition and porosity. Chemical shift and line width values are consistent with petrographic information. Rare upfield shifts were measured and attributed to the presence of transition metal cations on the surface. The evolution of freshly cleaved rocks exposed to the atmosphere was also characterized. The CF-HP 129Xe NMR technique is non-destructive and it could complement currently used techniques, like porosimetry and microscopy, providing additional information on the chemical nature of the rock surface and its evolution.

High-performance liquid chromatography on-line coupled to high-field NMR and mass spectrometry for structure elucidation of constituents of Hypericum perforatum L

DEFF Research Database (Denmark)

Hansen, S. H.; Jensen, A. G.; Cornett, Claus

1999-01-01

The on-line separation and structure elucidation of naphthodianthrones, flavonoids, and other constituents of an extract from Hypericum perforatum L, using high performance liquid chromatography (HPLC) coupled on-line with ultraviolet-visible, nuclear magnetic resonance (NMR), and mass spectrometry...... (MS) is described. A conventional reversed-phase HPLC system using ammonium acetate as the buffer substance in the eluent tvas used, and proton NMR spectra were obtained on a 500 MHz NMR instrument. The MS and MS/MS analyses were performed using negative electrospray ionization, In the present study...

Statistical removal of background signals from high-throughput 1H NMR line-broadening ligand-affinity screens

International Nuclear Information System (INIS)

Worley, Bradley; Sisco, Nicholas J.; Powers, Robert

2015-01-01

NMR ligand-affinity screens are vital to drug discovery, are routinely used to screen fragment-based libraries, and used to verify chemical leads from high-throughput assays and virtual screens. NMR ligand-affinity screens are also a highly informative first step towards identifying functional epitopes of unknown proteins, as well as elucidating the biochemical functions of protein–ligand interaction at their binding interfaces. While simple one-dimensional 1 H NMR experiments are capable of indicating binding through a change in ligand line shape, they are plagued by broad, ill-defined background signals from protein 1 H resonances. We present an uncomplicated method for subtraction of protein background in high-throughput ligand-based affinity screens, and show that its performance is maximized when phase-scatter correction is applied prior to subtraction

Structure of the charge density wave in cuprate superconductors: Lessons from NMR

Science.gov (United States)

Atkinson, W. A.; Ufkes, S.; Kampf, A. P.

2018-03-01

Using a mix of numerical and analytic methods, we show that recent NMR 17O measurements provide detailed information about the structure of the charge-density wave (CDW) phase in underdoped YBa2Cu3O6 +x . We perform Bogoliubov-de Gennes (BdG) calculations of both the local density of states and the orbitally resolved charge density, which are closely related to the magnetic and electric quadrupole contributions to the NMR spectrum, using a microscopic model that was shown previously to agree closely with x-ray experiments. The BdG results reproduce qualitative features of the experimental spectrum extremely well. These results are interpreted in terms of a generic "hot-spot" model that allows one to trace the origins of the NMR line shapes. We find that four quantities—the orbital character of the Fermi surface at the hot spots, the Fermi surface curvature at the hot spots, the CDW correlation length, and the magnitude of the subdominant CDW component—are key in determining the line shapes.

Surface Properties of Squalene/Meibum Films and NMR Confirmation of Squalene in Tears

Directory of Open Access Journals (Sweden)

Slavyana Ivanova

2015-09-01

Full Text Available Squalene (SQ possesses a wide range of pharmacological activities (antioxidant, drug carrier, detoxifier, hydrating, emollient that can be of benefit to the ocular surface. It can come in contact with human meibum (hMGS; the most abundant component of the tear film lipid layer as an endogenous tear lipid or from exogenous sources as eyelid sebum or pharmaceuticals. The aims of this study were to determine (i if SQ is in tear lipids and (ii its influence on the surface properties of hMGS films. Heteronuclear single quantum correlation NMR confirmed 7 mol % SQ in Schirmer’s strips extracts. The properties of SQ/hMGS pseudo-binary films at the air/water interface were studied with Langmuir surface balance, stress-relaxation dilatational rheology and Brewster angle microscopy. SQ does not possess surfactant properties. When mixed with hMGS squalene (i localized over the layers’ thinner regions and (ii did not affect the film pressure at high compression. Therefore, tear SQ is unlikely to instigate dry eye, and SQ can be used as a safe and “inert” ingredient in formulations to protect against dry eye. The layering of SQ over the thinner film regions in addition to its pharmacological properties could contribute to the protection of the ocular surface.

31P NMR spectroscopy studies of phospholipid metabolism in human melanoma xenograft lines differing in rate of tumour cell proliferation.

Science.gov (United States)

Lyng, H; Olsen, D R; Petersen, S B; Rofstad, E K

1995-04-01

The concentration of phospholipid metabolites in tumours has been hypothesized to be related to rate of cell membrane turnover and may reflect rate of cell proliferation. The purpose of the study reported here was to investigate whether 31P NMR resonance ratios involving the phosphomonoester (PME) or phosphodiester (PDE) resonance are correlated to fraction of cells in S-phase or volume-doubling time in experimental tumours. Four human melanoma xenograft lines (BEX-t, HUX-t, SAX-t, WIX-t) were included in the study. The tumours were grown subcutaneously in male BALB/c-nu/nu mice. 31P NMR spectroscopy was performed at a magnetic field strength of 4.7 T. Fraction of cells in S-phase was measured by flow cytometry. Tumour volume-doubling time was determined by Gompertzian analysis of volumetric growth data. BEX-t and SAX-t tumours differed in fraction of cells in S-phase and volume-doubling time, but showed similar 31P NMR resonance ratios. BEX-t and WIX-t tumours showed significantly different 31P NMR resonance ratios but similar fractions of cells in S-phase. The 31P NMR resonance ratios were significantly different for small and large HUX-t tumours even though fraction of cells in S-phase and volume-doubling time did not differ with tumour volume. None of the 31P NMR resonance ratios showed significant increase with increasing fraction of cells in S-phase or significant decrease with increasing tumour volume-doubling time across the four xenograft lines.(ABSTRACT TRUNCATED AT 250 WORDS)

Proton NMR studies of functionalized nanoparticles in aqueous environments

Science.gov (United States)

Tataurova, Yulia Nikolaevna

Nanoscience is an emerging field that can provide potential routes towards addressing critical issues such as clean and sustainable energy, environmental remediation and human health. Specifically, porous nanomaterials, such as zeolites and mesoporous silica, are found in a wide range of applications including catalysis, drug delivery, imaging, environmental protection, and sensing. The characterization of the physical and chemical properties of nanocrystalline materials is essential to the realization of these innovative applications. The great advantage of porous nanocrystals is their increased external surface area that can control their biological, chemical and catalytic activities. Specific functional groups synthesized on the surface of nanoparticles are able to absorb heavy metals from the solution or target disease cells, such as cancer cells. In these studies, three main issues related to functionalized nanomaterials will be addressed through the application of nuclear magnetic resonance (NMR) techniques including: 1) surface composition and structure of functionalized nanocrystalline particles; 2) chemical properties of the guest molecules on the surface of nanomaterials, and 3) adsorption and reactivity of surface bound functional groups. Nuclear magnetic resonance (NMR) is one of the major spectroscopic techniques available for the characterization of molecular structure and conformational dynamics with atomic level detail. This thesis deals with the application of 1H solution state NMR to porous nanomaterial in an aqueous environment. Understanding the aqueous phase behavior of functionalized nanomaterials is a key factor in the design and development of safe nanomaterials because their interactions with living systems are always mediated through the aqueous phase. This is often due to a lack of fundamental knowledge in interfacial chemical and physical phenomena that occur on the surface of nanoparticles. The use of solution NMR spectroscopy results

Nonclassical dynamics of the methyl group in 1,1,1-triphenylethane. Evidence from powder 1H NMR spectra

KAUST Repository

Osior, Agnieszka

2017-03-14

According to the damped quantum rotation (DQR) theory, hindered rotation of methyl groups, evidenced in nuclear magnetic resonance (NMR) line shapes, is a nonclassical process. It comprises a number of quantum-rate processes measured by two different quantum-rate constants. The classical jump model employing only one rate constant is reproduced if these quantum constants happen to be equal. The values of their ratio, or the nonclassicallity coefficient, determined hitherto from NMR spectra of single crystals and solutions range from about 1.20 to 1.30 in the latter case to above 5.0 in the former, with the value of 1 corresponding to the jump model. Presently, first systematic investigations of the DQR effects in wide-line NMR spectra of a powder sample are reported. For 1,1,1-triphenylethane deuterated in the aromatic positions, the relevant line-shape effects were monitored in the range 99–121 K. The values of the nonclassicality coefficient dropping from 2.7 to 1.7 were evaluated in line shape fits to the experimental powder spectra from the range 99–108 K. At these temperatures, the fits with the conventional line-shape model are visibly inferior to the DQR fits. Using a theoretical model reported earlier, a semiquantitative interpretation of the DQR parameters evaluated from the spectra is given. It is shown that the DQR effects as such can be detected in wide-line NMR spectra of powdered samples, which are relatively facile to measure. However, a fully quantitative picture of these effects can only be obtained from the much more demanding experiments on single crystals.

NMR

International Nuclear Information System (INIS)

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

1984-01-01

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

Surface-NMR measurements of the longitudinal relaxation time T1 in a homogeneous sandy aquifer in Skive, Denmark

Science.gov (United States)

Walbrecker, J.; Behroozmand, A.

2011-12-01

Efficient groundwater management requires reliable means of characterizing shallow groundwater aquifers. One key parameter in this respect is hydraulic conductivity. Surface nuclear magnetic resonance (NMR) is a geophysical exploration technique that can potentially provide this type of information in a noninvasive, cost-effective way. The technique is based on measuring the precession of nuclear spins of protons in groundwater molecules. It involves large loop antennas deployed on Earth's surface to generate electromagnetic pulses tuned to specifically excite and detect groundwater proton spins. Naturally, the excited state of spins is transitory - once excited, spins relax back to their equilibrium state. This relaxation process is strongly influenced by the spin environment, which, in the case of groundwater, is defined by the aquifer. By employing empirical relations, changes in relaxation behavior can be used to identify changes in aquifer hydraulic conductivity, making the NMR relaxation signal a very important piece of information. Particularly, efforts are made to record the longitudinal relaxation parameter T1, because it is known from laboratory studies that it often reliably correlates with hydraulic conductivity, even in the presence of magnetic species. In surface NMR, T1 data are collected by recording the NMR signal amplitude following two sequential excitation pulses as a function of the delay time τ between the two pulses. In conventional acquisition, the two pulses have a mutual phase shift of π. Based on theoretical arguments it was recently shown that T1 times acquired according to this conventional surface-NMR scheme are systematically biased. It was proposed that the bias can be minimized by cycling the phase of the two pulses between π and zero in subsequent double-pulse experiments, and subtracting the resulting signal amplitudes (phase-cycled pseudosaturation recovery scheme, pcPSR). We present the first surface-NMR T1 data set recorded

Quantification of C=C and C=O Surface Carbons in Detonation Nanodiamond by NMR

Energy Technology Data Exchange (ETDEWEB)

Cui, J -F; Fang, X -W; Schmidt-Rohr, K

2014-05-08

The ability of solid-state 13C NMR to detect and quantify small amounts of sp2-hybridized carbon on the surface of ~5 nm diameter nanodiamond particles is demonstrated. The C=C carbon fraction is only 1.1 ± 0.4% in pristine purified detonation nanodiamond, while a full single-layer graphitic or “bucky diamond” shell would contain ca. 25% of all C in a 5 nm diameter particle. Instead of large aromatic patches repeatedly proposed in the recent literature, sp3-hybridized CH and COH carbons cover most of the nanodiamond particle surface, accounting for ~5% each. C=O and COO groups also seen in X-ray absorption near-edge structure spectroscopy (XANES) but not detected in previous NMR studies make up ca. 1.5% of all C. They are removed by heat treatment at 800 °C, which increases the aromatic fraction. 13C{1H} NMR demonstrates that the various sp2-hybridized carbons are mostly not protonated, but cross-polarization shows that they are separated from 1H by only a few bond lengths, which proves that they are near the protonated surface. Together, the observed C–H, C–OH, C=O, and C=C groups account for 12–14% of all C, which matches the surface fraction expected for bulk-terminated 5 nm diameter diamond particles.

NMR reaction monitoring in flow synthesis.

Science.gov (United States)

Gomez, M Victoria; de la Hoz, Antonio

2017-01-01

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

Line printing solution-processable small molecules with uniform surface profile via ink-jet printer.

Science.gov (United States)

Liu, Huimin; Xu, Wei; Tan, Wanyi; Zhu, Xuhui; Wang, Jian; Peng, Junbiao; Cao, Yong

2016-03-01

Line printing offers a feasible approach to remove the pixel well structure which is widely used to confine the ink-jet printed solution. In the study, a uniform line is printed by an ink-jet printer. To achieve a uniform surface profile of the printed line, 10vol% low-volatile solvent DMA (3,4-Dimethylanisole) is mixed with high-volatile solvent Pxy (p-xylene) as the solvent. After a solution-processable small molecule is dissolved, the surface tension of DMA solution becomes lower than that of Pxy solution, which creates an inward Marangoni flow during the solvent evaporation. The inward Marangoni flow balances out the outward capillary flow, thereby forming a flat film surface. The line width of the printed line depends on the contact angle of the solution on the hole injection layer. Copyright © 2015 Elsevier Inc. All rights reserved.

Shape of the nuclear magnetic resonance line in anisotropic superconductors with an irregular vortex lattice

International Nuclear Information System (INIS)

Minkin, A.V.; Tsarevskij, S.L.

2006-01-01

For high-temperature superconductors the shape of a NMR spectrum line is built regarding for variation of inhomogeneity of irregular vortex lattice magnetic field near superconductor surface. It is shown that the shape of a NMR line is not simply widened but noticeably varies depending on the degree of irregularity of a superconductor vortex lattice. This variation is associated with a local symmetry decrease in an irregular vortex lattice of the superconductor. Taking into account these circumstances may considerably change conclusions about the type of a vortex lattice and superconductor parameters which are commonly gained from NMR line shape analysis [ru

NMR reaction monitoring in flow synthesis

Directory of Open Access Journals (Sweden)

M. Victoria Gomez

2017-02-01

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

Analysis of the quadrupolar coupling effect on the line intensities using single-crystal nutation NMR in α-Al2O3 crystals

International Nuclear Information System (INIS)

Woo, Ae Ja; Cho, So Hyun; Han, Duk Young

2000-01-01

With 1D-nutation NMR for a spin I = 5/2 system, the relative line intensities of central and the inner- and outer-satellite transitions are calculated as functions of quadrupolar coupling ω Q and rf pulse strength ω rf . Experimentally measured line intensities including both central and satellites are used to extract the values of ω Q and ω rf from nonlinear least-squares fits. The method is illustrated in α-Al 2 O 3 crystals (ruby and corundum) with the single-crystal 27 Al nutation NMR spectra. As a result, the new feature that the rf pulse strength shows reduced effect on the satellite transition lines according to the quadrupolar coupling is discussed by using fictitious spin-1/2 operator

NMRFx Processor: a cross-platform NMR data processing program

International Nuclear Information System (INIS)

Norris, Michael; Fetler, Bayard; Marchant, Jan; Johnson, Bruce A.

2016-01-01

NMRFx Processor is a new program for the processing of NMR data. Written in the Java programming language, NMRFx Processor is a cross-platform application and runs on Linux, Mac OS X and Windows operating systems. The application can be run in both a graphical user interface (GUI) mode and from the command line. Processing scripts are written in the Python programming language and executed so that the low-level Java commands are automatically run in parallel on computers with multiple cores or CPUs. Processing scripts can be generated automatically from the parameters of NMR experiments or interactively constructed in the GUI. A wide variety of processing operations are provided, including methods for processing of non-uniformly sampled datasets using iterative soft thresholding. The interactive GUI also enables the use of the program as an educational tool for teaching basic and advanced techniques in NMR data analysis.

NMRFx Processor: a cross-platform NMR data processing program

Energy Technology Data Exchange (ETDEWEB)

Norris, Michael; Fetler, Bayard [One Moon Scientific, Inc. (United States); Marchant, Jan [University of Maryland Baltimore County, Howard Hughes Medical Institute (United States); Johnson, Bruce A., E-mail: bruce.johnson@asrc.cuny.edu [One Moon Scientific, Inc. (United States)

2016-08-15

NMRFx Processor is a new program for the processing of NMR data. Written in the Java programming language, NMRFx Processor is a cross-platform application and runs on Linux, Mac OS X and Windows operating systems. The application can be run in both a graphical user interface (GUI) mode and from the command line. Processing scripts are written in the Python programming language and executed so that the low-level Java commands are automatically run in parallel on computers with multiple cores or CPUs. Processing scripts can be generated automatically from the parameters of NMR experiments or interactively constructed in the GUI. A wide variety of processing operations are provided, including methods for processing of non-uniformly sampled datasets using iterative soft thresholding. The interactive GUI also enables the use of the program as an educational tool for teaching basic and advanced techniques in NMR data analysis.

Lining seam elimination algorithm and surface crack detection in concrete tunnel lining

Science.gov (United States)

Qu, Zhong; Bai, Ling; An, Shi-Quan; Ju, Fang-Rong; Liu, Ling

2016-11-01

Due to the particularity of the surface of concrete tunnel lining and the diversity of detection environments such as uneven illumination, smudges, localized rock falls, water leakage, and the inherent seams of the lining structure, existing crack detection algorithms cannot detect real cracks accurately. This paper proposed an algorithm that combines lining seam elimination with the improved percolation detection algorithm based on grid cell analysis for surface crack detection in concrete tunnel lining. First, check the characteristics of pixels within the overlapping grid to remove the background noise and generate the percolation seed map (PSM). Second, cracks are detected based on the PSM by the accelerated percolation algorithm so that the fracture unit areas can be scanned and connected. Finally, the real surface cracks in concrete tunnel lining can be obtained by removing the lining seam and performing percolation denoising. Experimental results show that the proposed algorithm can accurately, quickly, and effectively detect the real surface cracks. Furthermore, it can fill the gap in the existing concrete tunnel lining surface crack detection by removing the lining seam.

On-line plant-wide monitoring using neural networks

International Nuclear Information System (INIS)

Turkcan, E.; Ciftcioglu, O.; Eryurek, E.; Upadhyaya, B.R.

1992-06-01

The on-line signal analysis system designed for a multi-level mode operation using neural networks is described. The system is capable of monitoring the plant states by tracking different number of signals up to 32 simultaneously. The data used for this study were acquired from the Borssele Nuclear Power Plant (PWR type), and using the on-line monitoring system. An on-line plant-wide monitoring study using a multilayer neural network model is discussed in this paper. The back-propagation neural network algorithm is used for training the network. The technique assumes that each physical state of the power plant can be represented by a unique pattern of instrument readings which can be related to the condition of the plant. When disturbance occurs, the sensor readings undergo a transient, and form a different set of patterns which represent the new operational status. Diagnosing these patterns can be helpful in identifying this new state of the power plant. To this end, plant-wide monitoring with neutral networks is one of the new techniques in real-time applications. (author). 9 refs.; 5 figs

Remote tuning of NMR probe circuits.

Science.gov (United States)

Kodibagkar, V D; Conradi, M S

2000-05-01

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

Development of Elite BPH-Resistant Wide-Spectrum Restorer Lines for Three and Two Line Hybrid Rice.

Science.gov (United States)

Fan, Fengfeng; Li, Nengwu; Chen, Yunping; Liu, Xingdan; Sun, Heng; Wang, Jie; He, Guangcun; Zhu, Yingguo; Li, Shaoqing

2017-01-01

Hybrid rice has contributed significantly to the world food security. Breeding of elite high-yield, strong-resistant broad-spectrum restorer line is an important strategy for hybrid rice in commercial breeding programs. Here, we developed three elite brown planthopper (BPH)-resistant wide-spectrum restorer lines by pyramiding big-panicle gene Gn8.1 , BPH-resistant genes Bph6 and Bph9 , fertility restorer genes Rf3, Rf4, Rf5 , and Rf6 through molecular marker assisted selection. Resistance analysis revealed that the newly developed restorer lines showed stronger BPH-resistance than any of the single-gene donor parent Luoyang-6 and Luoyang-9. Moreover, the three new restorer lines had broad spectrum recovery capabilities for Honglian CMS, Wild abortive CMS and two-line GMS sterile lines, and higher grain yields than that of the recurrent parent 9,311 under nature field conditions. Importantly, the hybrid crosses also showed good performance for grain yield and BPH-resistance. Thus, the development of elite BPH-resistant wide-spectrum restorer lines has a promising future for breeding of broad spectrum BPH-resistant high-yield varieties.

Nonclassical dynamics of the methyl group in 1,1,1-triphenylethane. Evidence from powder 1H NMR spectra

KAUST Repository

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

2017-01-01

interpretation of the DQR parameters evaluated from the spectra is given. It is shown that the DQR effects as such can be detected in wide-line NMR spectra of powdered samples, which are relatively facile to measure. However, a fully quantitative picture

Real quartic surfaces containing 16 skew lines

Directory of Open Access Journals (Sweden)

Isidro Nieto

2004-01-01

Full Text Available It is well known that there is an open three-dimensional subvariety Ms of the Grassmannian of lines in ℙ3 which parametrizes smooth irreducible complex surfaces of degree 4 which are Heisenberg invariant, and each quartic contains 32 lines but only 16 skew lines, being determined by its configuration of lines, are called a double 16. We consider here the problem of visualizing in a computer the real Heisenberg invariant quartic surface and the real double 16. We construct a family of points l∈Ms parametrized by a two-dimensional semialgebraic variety such that under a change of coordinates of l into its Plüecker, coordinates transform into the real coordinates for a line L in ℙ3, which is then used to construct a program in Maple 7. The program allows us to draw the quartic surface and the set of transversal lines to L. Additionally, we include a table of a group of examples. For each test example we specify a parameter, the viewing angle of the image, compilation time, and other visual properties of the real surface and its real double 16. We include at the end of the paper an example showing the surface containing the double 16.

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

International Nuclear Information System (INIS)

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

1994-01-01

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

Structural properties of carbon nanotubes derived from 13C NMR

KAUST Repository

Abou-Hamad, E.

2011-10-10

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

Whole-core analysis by 13C NMR

International Nuclear Information System (INIS)

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

1991-01-01

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

Magic Angle Spinning NMR Metabolomics

Energy Technology Data Exchange (ETDEWEB)

Zhi Hu, Jian

2016-01-01

Nuclear Magnetic Resonance (NMR) spectroscopy is a non-destructive, quantitative, reproducible, untargeted and unbiased method that requires no or minimal sample preparation, and is one of the leading analytical tools for metabonomics research [1-3]. The easy quantification and the no need of prior knowledge about compounds present in a sample associated with NMR are advantageous over other techniques [1,4]. 1H NMR is especially attractive because protons are present in virtually all metabolites and its NMR sensitivity is high, enabling the simultaneous identification and monitoring of a wide range of low molecular weight metabolites.

Dynamic NMR under nonstationary conditions: Theoretical model, numerical calculation, and potential of application

Energy Technology Data Exchange (ETDEWEB)

Babailov, S. P., E-mail: babajlov@niic.nsc.ru [A. V. Nikolaevs Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences, Novosibirsk (Russian Federation); National Research Tomsk Polytechnic University, Lenin Avenue 30, Tomsk 634050 (Russian Federation); Purtov, P. A. [Voevodsky Institute of Chemical Kinetics and Combustion, Siberian Branch of the Russian Academy of Sciences, Insitutskaya 3, 630090 Novosibirsk (Russian Federation); Fomin, E. S. [Institute of Cytology and Genetics of the Siberian Branch of the Russian Academy of Sciences, Av. Lavrentyev 10, 630090 Novosibirsk (Russian Federation)

2016-08-07

An expression has been derived for the time dependence of the NMR line shape for systems with multi-site chemical exchange in the absence of spin-spin coupling, in a zero saturation limit. The dynamics of variation of the NMR line shape with time is considered in detail for the case of two-site chemical exchange. Mathematical programs have been designed for numerical simulation of the NMR spectra of chemical exchange systems. The analytical expressions obtained are useful for NMR line shape simulations for systems with photoinduced chemical exchange.

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-10-05

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

29-Silicon NMR evidence for the improved chromatographic siloxane bond stability of bulky alkylsilane ligands on a silica surface

NARCIS (Netherlands)

Scholten, A.B.; Haan, de J.W.; Claessens, H.A.; Ven, van de L.J.M.; Cramers, C.A.

1994-01-01

A stable bond stationary phase for reversed-phase HPLC, with a diisobutyl-n-octadecylsilane derivatized surface, was studied using 29Si CPMAS NMR. Fumed silica surfaces (Aerosil), trimethylsilylated to different extents, were used to illustrate the effect of ligand surface loading on the hydrogen

Dynamic pulsed-field-gradient NMR

CERN Document Server

Sørland, Geir Humborstad

2014-01-01

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

27Al NMR studies of NpPd5Al2

International Nuclear Information System (INIS)

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

2009-01-01

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

Determination of Monomers Reactivity Ratios in Ethyl Acrylate-Methacrylic Acid Copolymerization by Off-Line 1H NMR

Directory of Open Access Journals (Sweden)

Samaneh Ashenagar

2017-03-01

Full Text Available The physical, chemical and mechanical properties of polymer systems depend on the micro-structural characteristics of their macromolecular chains. Along with the most characteristic kinetic parameters in copolymerization reactions are the reactivity ratios, which give a clear idea of the average composition and the monomer sequence distribution in copolymer systems. This research studies the solution radical copolymerization of methacrylic acid (MAA-ethyl acrylate (EA system at low conversion with 2,2'-azobisisobutyronitrile (AIBN as thermal initiator at 60°C in deuterated dimethyl sulfoxide (DMSO-d6 as a reaction solvent. In this case, the monomer reactivity ratios were determined using linear off-line 1H nuclear magnetic resonance spectroscopy (1H NMR methods such as Mayo-Louis, Finemann-Ross, Inverted Finemann-Ross , Ezrielev-Brokhina-Roskin, Joshi-Joshi, Kelen-Tudos, extended Kelen- Tudos, Mao-Huglin at low and high conversions. The next estimation process in off-line 1H NMR methods were performed by applying techniques based on ordinary least square (OLS and generalized least square (GLS. The results showed that the GLS approach compared to the OLS increased regression coefficients (R2 and the order of magnitude of parameter variances obtained from GLS was many times lower than that obtained from OLS. In addition, the monomer reactivity ratios obtained by the Mao-Huglin method and the GLS approach showed the best linear estimation.

NMR imaging of solids with multiple-pulse line narrowing and radiofrequency gradients

International Nuclear Information System (INIS)

Werner, M.H.

1993-01-01

The usual methods of magnetic resonance imaging fail in rigid solids due to the line-shape contributions of dipolar coupling, chemical shift dispersion and anisotropy, and bulk magnetic susceptibility. This dissertation presents a new method of solid-stage imaging by nuclear magnetic resonance which averages away these contributions with multiple-pulse line-narrowing and encodes spatial information with pulsed radiofrequency field gradients. This method is closely related to simultaneously developed methods utilizing pulsed DC gradients, and offers similar improvements in sensitivity and resolution. The advantage of rf gradients is that they can be rapidly switched without inducing eddy currents in the probe or the magnet. In addition, the phases and amplitudes of the rf gradients can be switched by equipment which is already part of an NMR spectrometer capable of solid-state spectroscopy. The line-narrowing and gradient pulses originate in separate rf circuits tuned to the same frequency. Interactions between the circuits have been minimized by a method of active Q-switching which employs PIN diodes in the matching networks of these circuits. Both one- and two-dimensional images are presented. The latter are obtained by a novel method in which the two dimensions of imaging transverse to the static magnetic field are encoded by two orthogonal components of a single rf gradient. A π/2 phase shift of the rf phase relative to that of the line-narrowing pulses selects one component or the other. This arrangement allows the solid-state analogs of versatile imaging sequences based on Fourier imaging and eliminates the need for sample rotation and back-projection methods. Coherent averaging theory is used to analyze this imaging technique and exact numerical simulations on several coupled spins are discussed. These lend insight to the residual linewidth and its dependence on pixel position as well as to the range of applicability of this technique

Solid state NMR of spin-1/2 nuclei

International Nuclear Information System (INIS)

Wind, R.A.

1991-01-01

The detection of nuclear magnetic resonance by Bloch et al. and Purcell and co-workers in 1946 has led to the development of one of the most powerful spectroscopic techniques known today. The reason is that, besides the applied external magnetic field, a nuclear spin also experiences extra local magnetic fields, which are due to surrounding electron clouds (the chemical shift) and other spins. These local fields differ for nuclei located at chemically different positions in a molecule. The result is that an NMR spectrum often consists of several lines, which can be considered to be a fingerprint of the material under investigation an can assist the clarifying its molecular structure. NMR has been especially successful in liquids and liquid like materials, where fast molecular tumblings average out the anisotropies in the local fields, resulting in well-resolved NMR spectra. This paper reports that initially the development of solid-state NMR was less dramatic. Originally, for reasons of sensitivity, attention was focused mainly on 1 H NMR. The result is that the NMR spectrum usually consists of single, broad, featureless line, which, except for special cases such as more or less isolated spin pairs or methyl groups, does not provide much information

NMR study of LaPb2

International Nuclear Information System (INIS)

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

1995-01-01

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

Nuclear magnetic resonance (NMR): principles and applications

International Nuclear Information System (INIS)

Quibilan, E.I.

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

Genetic Analysis of Health-Related Secondary Metabolites in a Brassica rapa Recombinant Inbred Line Population

NARCIS (Netherlands)

Bagheri, H.; Soda, El M.; Kim, H.K.; Fritsche, S.; Jung, C.; Aarts, M.G.M.

2013-01-01

The genetic basis of the wide variation for nutritional traits in Brassica rapa is largely unknown. A new Recombinant Inbred Line (RIL) population was profiled using High Performance Liquid Chromatography (HPLC) and Nuclear Magnetic Resonance (NMR) analysis to detect quantitative trait loci (QTLs)

Solid-state NMR of inorganic semiconductors.

Science.gov (United States)

Yesinowski, James P

2012-01-01

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

nmrML: A Community Supported Open Data Standard for the Description, Storage, and Exchange of NMR Data.

Science.gov (United States)

Schober, Daniel; Jacob, Daniel; Wilson, Michael; Cruz, Joseph A; Marcu, Ana; Grant, Jason R; Moing, Annick; Deborde, Catherine; de Figueiredo, Luis F; Haug, Kenneth; Rocca-Serra, Philippe; Easton, John; Ebbels, Timothy M D; Hao, Jie; Ludwig, Christian; Günther, Ulrich L; Rosato, Antonio; Klein, Matthias S; Lewis, Ian A; Luchinat, Claudio; Jones, Andrew R; Grauslys, Arturas; Larralde, Martin; Yokochi, Masashi; Kobayashi, Naohiro; Porzel, Andrea; Griffin, Julian L; Viant, Mark R; Wishart, David S; Steinbeck, Christoph; Salek, Reza M; Neumann, Steffen

2018-01-02

NMR is a widely used analytical technique with a growing number of repositories available. As a result, demands for a vendor-agnostic, open data format for long-term archiving of NMR data have emerged with the aim to ease and encourage sharing, comparison, and reuse of NMR data. Here we present nmrML, an open XML-based exchange and storage format for NMR spectral data. The nmrML format is intended to be fully compatible with existing NMR data for chemical, biochemical, and metabolomics experiments. nmrML can capture raw NMR data, spectral data acquisition parameters, and where available spectral metadata, such as chemical structures associated with spectral assignments. The nmrML format is compatible with pure-compound NMR data for reference spectral libraries as well as NMR data from complex biomixtures, i.e., metabolomics experiments. To facilitate format conversions, we provide nmrML converters for Bruker, JEOL and Agilent/Varian vendor formats. In addition, easy-to-use Web-based spectral viewing, processing, and spectral assignment tools that read and write nmrML have been developed. Software libraries and Web services for data validation are available for tool developers and end-users. The nmrML format has already been adopted for capturing and disseminating NMR data for small molecules by several open source data processing tools and metabolomics reference spectral libraries, e.g., serving as storage format for the MetaboLights data repository. The nmrML open access data standard has been endorsed by the Metabolomics Standards Initiative (MSI), and we here encourage user participation and feedback to increase usability and make it a successful standard.

Metabolite profiling of leek (Allium porrum L) cultivars by (1) H NMR and HPLC-MS.

Science.gov (United States)

Soininen, Tuula H; Jukarainen, Niko; Soininen, Pasi; Auriola, Seppo O K; Julkunen-Tiitto, Riitta; Oleszek, Wieslaw; Stochmal, Anna; Karjalainen, Reijo O; Vepsäläinen, Jouko J

2014-01-01

Leek (Allium ampeloprasum var. porrum) is consumed as a vegetable throughout the world. However, little is known about the metabolites of leek cultivars, especially those with potentially important beneficial properties for human health. We provide new information for the overall metabolite composition of several leek cultivars grown in Europe by using HPLC-MS and (1) H NMR. The use of a novel CTLS/NMR (constrained total-line-shape nuclear magnetic resonance) approach was found to be capable of reliable quantification, even with overlapping metabolite signals in the (1) H NMR of plant metabolites. Additionally, a new application for leek flavonoids was optimised for HPLC-MS. The total concentration of carbohydrates (glucose, fructose, kestose/nystose and sucrose) and nine amino acids varied by fourfold in leek juice from different cultivars, while the total concentrations of four organic acids were similar in all cultivars. All the quantified flavonols were kaempferol derivatives or quercetin derivatives and threefold differences in flavonol concentrations were detected between cultivars. In this study, various phytochemical profiles were determined for several leek cultivars by (1) H NMR spectroscopy with CTLS combined with HPLC-MS. The wide variation in bioactive compounds among commercial leek cultivars offers promising opportunities for breeders to raise the levels of important biochemical compounds in leek breeding lines, and also provides some objective measure for quality assurance for the leek industry. Copyright © 2014 John Wiley & Sons, Ltd.

The NMR Probe of High-T$_{c}$ Materials

CERN Document Server

Walstedt, Russell E

2008-01-01

The NMR probe has yielded a vast array of data for the high-Tc materials, corresponding to different compounds, ionic sites, and nuclear species, as well as to a wide variety of experimental conditions. Over the twenty years, since the discovery of superconducting cuprates, ongoing analysis and discussion of cuprate NMR data have resulted in a wealth of important insights into the physics of these exotic systems. The aims of this monograph are threefold. First, it reviews NMR methodology as it has been applied to the cuprate studies. This is addressed to NMR practitioners and to physics laypersons alike. Next, it presents a review of cuprate NMR measurements and the wide variety of phenomena which they represent. The third phase is to recount the theoretical model calculations and other proposals which have been put forward to account for these data. Parts two and three are presented in parallel, as there are many aspects to both topics, each with its own interesting history. There is, even twenty years on, a...

Principles of high resolution NMR in solids

CERN Document Server

Mehring, Michael

1983-01-01

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

Two-dimensional NMR spectroscopy. Applications for chemists and biochemists

International Nuclear Information System (INIS)

Croasmun, W.R.; Carlson, R.M.K.

1987-01-01

Two-dimensional nuclear magnetic resonance spectroscopy (2-D NMR) has become a very powerful class of experiments (in the hands of an adept scientist) with broad adaptability to new situations. It is the product of a happy marriage between modern pulse FT-NMR technology, with its large memory and high-speed computers, and the physicists and chemists who love to manipulate spin systems. Basic 2-D experiments are now a standard capability of modern NMR spectrometers, and this timely book intends to make 2-D NMR users of those who are familiar with normal 1-D NMR. The 2-D NMR goal is correlation of the lines of the observed NMR spectrum with other properties of the system. This book deals with applications to high-resolution spectrum analysis, utilizing either coupling between the NMR-active nuclei or chemical exchange to perform the correlation. The coupling can be scalar (through bonds) or direct through space (within 5 A). The coupling may be homonuclear (between like nuclei) or heteronuclear

Advanced NMR technology for bioscience and biotechnology

Energy Technology Data Exchange (ETDEWEB)

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

1998-11-01

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

Proton NMR study of α-MnH 0.06

Science.gov (United States)

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

2004-07-01

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

The characterisation of polymers using pulsed NMR

International Nuclear Information System (INIS)

Charlesby, A.

1983-01-01

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

Petrophysical properties of greensand as predicted from NMR measurements

DEFF Research Database (Denmark)

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

2011-01-01

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

NMR-based approach to the analysis of radiopharmaceuticals: radiochemical purity, specific activity, and radioactive concentration values by proton and tritium NMR spectroscopy.

Science.gov (United States)

Schenk, David J; Dormer, Peter G; Hesk, David; Pollack, Scott R; Lavey, Carolee Flader

2015-06-15

Compounds containing tritium are widely used across the drug discovery and development landscape. These materials are widely utilized because they can be efficiently synthesized and produced at high specific activity. Results from internally calibrated (3)H and (1)H nuclear magnetic resonance (NMR) spectroscopy suggests that at least in some cases, this calibrated approach could supplement or potentially replace radio-high-performance liquid chromatography for radiochemical purity, dilution and scintillation counting for the measurement of radioactivity per volume, and liquid chromatography/mass spectrometry analysis for the determination of specific activity. In summary, the NMR-derived values agreed with those from the standard approaches to within 1% to 9% for solution count and specific activity. Additionally, the NMR-derived values for radiochemical purity deviated by less than 5%. A benefit of this method is that these values may be calculated at the same time that (3)H NMR analysis provides the location and distribution of tritium atoms within the molecule. Presented and discussed here is the application of this method, advantages and disadvantages of the approach, and a rationale for utilizing internally calibrated (1)H and (3)H NMR spectroscopy for specific activity, radioactive concentration, and radiochemical purity whenever acquiring (3)H NMR for tritium location. Copyright © 2015 John Wiley & Sons, Ltd.

Investigation of the dynamic NMR frequency shift for Fe57 in FeBO3

International Nuclear Information System (INIS)

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

1978-01-01

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

Meandered-line antenna with integrated high-impedance surface.

Energy Technology Data Exchange (ETDEWEB)

Forman, Michael A.

2010-09-01

A reduced-volume antenna composed of a meandered-line dipole antenna over a finite-width, high-impedance surface is presented. The structure is novel in that the high-impedance surface is implemented with four Sievenpiper via-mushroom unit cells, whose area is optimized to match the meandered-line dipole antenna. The result is an antenna similar in performance to patch antenna but one fourth the area that can be deployed directly on the surface of a conductor. Simulations demonstrate a 3.5 cm ({lambda}/4) square antenna with a bandwidth of 4% and a gain of 4.8 dBi at 2.5 GHz.

Accessible surface area from NMR chemical shifts

Energy Technology Data Exchange (ETDEWEB)

Hafsa, Noor E.; Arndt, David; Wishart, David S., E-mail: david.wishart@ualberta.ca [University of Alberta, Department of Computing Science (Canada)

2015-07-15

Accessible surface area (ASA) is the surface area of an atom, amino acid or biomolecule that is exposed to solvent. The calculation of a molecule’s ASA requires three-dimensional coordinate data and the use of a “rolling ball” algorithm to both define and calculate the ASA. For polymers such as proteins, the ASA for individual amino acids is closely related to the hydrophobicity of the amino acid as well as its local secondary and tertiary structure. For proteins, ASA is a structural descriptor that can often be as informative as secondary structure. Consequently there has been considerable effort over the past two decades to try to predict ASA from protein sequence data and to use ASA information (derived from chemical modification studies) as a structure constraint. Recently it has become evident that protein chemical shifts are also sensitive to ASA. Given the potential utility of ASA estimates as structural constraints for NMR we decided to explore this relationship further. Using machine learning techniques (specifically a boosted tree regression model) we developed an algorithm called “ShiftASA” that combines chemical-shift and sequence derived features to accurately estimate per-residue fractional ASA values of water-soluble proteins. This method showed a correlation coefficient between predicted and experimental values of 0.79 when evaluated on a set of 65 independent test proteins, which was an 8.2 % improvement over the next best performing (sequence-only) method. On a separate test set of 92 proteins, ShiftASA reported a mean correlation coefficient of 0.82, which was 12.3 % better than the next best performing method. ShiftASA is available as a web server ( http://shiftasa.wishartlab.com http://shiftasa.wishartlab.com ) for submitting input queries for fractional ASA calculation.

Determination of free fatty acids in pharmaceutical lipids by ¹H NMR and comparison with the classical acid value.

Science.gov (United States)

Skiera, Christina; Steliopoulos, Panagiotis; Kuballa, Thomas; Diehl, Bernd; Holzgrabe, Ulrike

2014-05-01

Indices like acid value, peroxide value, and saponification value play an important role in quality control and identification of lipids. Requirements on these parameters are given by the monographs of the European pharmacopeia. (1)H NMR spectroscopy provides a fast and simple alternative to these classical approaches. In the present work a new (1)H NMR approach to determine the acid value is described. The method was validated using a statistical approach based on a variance components model. The performance under repeatability and in-house reproducibility conditions was assessed. We applied this (1)H NMR assay to a wide range of different fatty oils. A total of 305 oil and fat samples were examined by both the classical and the NMR method. Except for hard fat, the data obtained by the two methods were in good agreement. The (1)H NMR method was adapted to analyse waxes and oleyloleat. Furthermore, the effect of solvent and in the case of castor oil the effect of the oil matrix on line broadening and chemical shift of the carboxyl group signal are discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

Investigations of CuFeS{sub 2} semiconductor mineral from ocean rift hydrothermal vent fields by Cu NMR in a local field

Energy Technology Data Exchange (ETDEWEB)

Matukhin, V. L.; Pogoreltsev, A. I.; Gavrilenko, A. N., E-mail: ang-2000@mail.ru; Garkavyi, S. O.; Shmidt, E. V. [Kazan State Power University (Russian Federation); Babaeva, S. F. [All-Russia Research Institute of Geology and Mineral Resources of the World Ocean “VNIIOkeangeologiya” (Russian Federation); Sukhanova, A. A. [Saint-Petersburg Mining University (Russian Federation); Terukov, E. I. [Russian Academy of Sciences, Ioffe Physical-Technical Institute (Russian Federation)

2017-01-15

The results of investigating natural samples of chalcopyrite mineral CuFeS{sub 2} from massive oceanic sulfide ores of the Mid-Atlantic ridge by the {sup 63}Cu nuclear magnetic resonance (NMR {sup 63}Cu) in a local field at room temperature are presented. The significant width of the resonance lines found in the {sup 63}Cu NMR spectrum directly testifies to a wide distribution of local magnetic and electric fields in the investigated chalcopyrite samples. This distribution can be the consequence of an appreciable deviation of the structure of the investigated chalcopyrite samples from the stoichiometric one. The obtained results show that the pulsed {sup 63}Cu NMR can be an efficient method for studying the physical properties of deep-water polymetallic sulfides of the World Ocean.

NMR imaging of soft tissue tumors

International Nuclear Information System (INIS)

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

1986-01-01

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

Nuclear Magnetic Resonance (NMR) Spectroscopic Characterization of Nanomaterials and Biopolymers

Science.gov (United States)

Guo, Chengchen

Nanomaterials have attracted considerable attention in recent research due to their wide applications in various fields such as material science, physical science, electrical engineering, and biomedical engineering. Researchers have developed many methods for synthesizing different types of nanostructures and have further applied them in various applications. However, in many cases, a molecular level understanding of nanoparticles and their associated surface chemistry is lacking investigation. Understanding the surface chemistry of nanomaterials is of great significance for obtaining a better understanding of the properties and functions of the nanomaterials. Nuclear magnetic resonance (NMR) spectroscopy can provide a familiar means of looking at the molecular structure of molecules bound to surfaces of nanomaterials as well as a method to determine the size of nanoparticles in solution. Here, a combination of NMR spectroscopic techniques including one- and two-dimensional NMR spectroscopies was used to investigate the surface chemistry and physical properties of some common nanomaterials, including for example, thiol-protected gold nanostructures and biomolecule-capped silica nanoparticles. Silk is a natural protein fiber that features unique properties such as excellent mechanical properties, biocompatibility, and non-linear optical properties. These appealing physical properties originate from the silk structure, and therefore, the structural analysis of silk is of great importance for revealing the mystery of these impressive properties and developing novel silk-based biomaterials as well. Here, solid-state NMR spectroscopy was used to elucidate the secondary structure of silk proteins in N. clavipes spider dragline silk and B. mori silkworm silk. It is found that the Gly-Gly-X (X=Leu, Tyr, Gln) motif in spider dragline silk is not in a beta-sheet or alpha-helix structure and is very likely to be present in a disordered structure with evidence for 31-helix

Gaining insight into the T _2^*-T2 relationship in surface NMR free-induction decay measurements

Science.gov (United States)

Grombacher, Denys; Auken, Esben

2018-05-01

One of the primary shortcomings of the surface nuclear magnetic resonance (NMR) free-induction decay (FID) measurement is the uncertainty surrounding which mechanism controls the signal's time dependence. Ideally, the FID-estimated relaxation time T_2^* that describes the signal's decay carries an intimate link to the geometry of the pore space. In this limit the parameter T_2^* is closely linked to a related parameter T2, which is more closely linked to pore-geometry. If T_2^* ˜eq {T_2} the FID can provide valuable insight into relative pore-size and can be used to make quantitative permeability estimates. However, given only FID measurements it is difficult to determine whether T_2^* is linked to pore geometry or whether it has been strongly influenced by background magnetic field inhomogeneity. If the link between an observed T_2^* and the underlying T2 could be further constrained the utility of the standard surface NMR FID measurement would be greatly improved. We hypothesize that an approach employing an updated surface NMR forward model that solves the full Bloch equations with appropriately weighted relaxation terms can be used to help constrain the T_2^*-T2 relationship. Weighting the relaxation terms requires estimating the poorly constrained parameters T2 and T1; to deal with this uncertainty we propose to conduct a parameter search involving multiple inversions that employ a suite of forward models each describing a distinct but plausible T_2^*-T2 relationship. We hypothesize that forward models given poor T2 estimates will produce poor data fits when using the complex-inversion, while forward models given reliable T2 estimates will produce satisfactory data fits. By examining the data fits produced by the suite of plausible forward models, the likely T_2^*-T2 can be constrained by identifying the range of T2 estimates that produce reliable data fits. Synthetic and field results are presented to investigate the feasibility of the proposed technique.

30 CFR 75.705-2 - Repairs to energized surface high-voltage lines.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Repairs to energized surface high-voltage lines... Repairs to energized surface high-voltage lines. An energized high-voltage surface line may be repaired... on power circuits with a phase-to-phase nominal voltage no greater than 15,000 volts; (3) Such...

An introduction to biological NMR spectroscopy

International Nuclear Information System (INIS)

Marion, Dominique

2013-01-01

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

Heteronuclear 2D NMR studies on an engineered insulin monomer: Assignments and characterization of the receptor-binding surface by selective 2H and 13C labeling with application to protein design

International Nuclear Information System (INIS)

Weiss, M.A.; Hua, Qingxin; Lynch, C.S.; Shoelson, S.E.; Frank, B.H.

1991-01-01

Insulin provides an important model for the application of genetic engineering to rational protein design and has been well characterized in the crystal state. However, self-association of insulin in solution has precluded complementary 2D NMR study under physiological conditions. The authors demonstrate here that such limitations may be circumvented by the use of a monomeric analogue that contains three amino acid substitutions on the protein surface (HisB10 → Asp, ProB28 → Lys, and LysB29 → Pro); this analogue (designated DKP-insulin) retains native receptor-binding potency. Comparative 1 H NMR studies of native human insulin and a series of three related analogues-(i) the singly substituted analogue [HisB10→Asp], (ii) the doubly substituted analogue [ProB28→Lys; LysB29→Pro], and (iii) DKP-insulin-demonstrate progressive reduction in concentration-dependent line-broadening in accord with the results of analytical ultracentrifugation. Extensive nonlocal interactions are observed in the NOESY spectrum of DKP-insulin, indicating that this analogue adopts a compact and stably folded structure as a monomer in overall accord with crystal models. Site-specific 2 H and 13 C isotopic labels are introduced by semisynthesis as probes for the structure and dynamics of the receptor-binding surface. These studies confirm and extend under physiological conditions the results of a previous 2D NMR analysis of native insulin in 20% acetic acid. Implications for the role of protein flexibility in receptor recognition are discussed with application to the design of novel insulin analogues

Effect of resonance line shape on precision measurements of nuclear magnetic resonance shifts

International Nuclear Information System (INIS)

Kachurin, A.M.; Smelyanskij, A.Ya.

1986-01-01

Effect of resonance line shape on the systematic error of precision measurements of nuclear magnetic resonance (NMR) shifts of high resolution (on the center of NMR dispersion line) is analysed. Effect of the device resonance line form-function asymmetry is evaluated; the form-function is determined by configuration of the spectrometer magnetic field and enters the convolution, which describes the resonance line form. It is shown that with the increase of the relaxation line width the form-function effect on the measurement error yields to zero. The form-function effect on measurements and correction of a phase angle of NMR detection is evaluated. The method of semiquantitative evaluation of resonance line and NMR spectrometer parameters, guaranteeing the systematic error of the given infinitesimal, is presented

Solid-state (49/47)Ti NMR of titanium-based MCM-41 hybrid materials.

Science.gov (United States)

Ballesteros, Ruth; Fajardo, Mariano; Sierra, Isabel; Force, Carmen; del Hierro, Isabel

2009-11-03

Titanium solid-state NMR spectroscopy data for a series of organic-inorganic titanium MCM-41 based materials have been collected. These materials have been synthesized by first modifying the mesoporous silica MCM-41 in one step with a mixture of silanes: a triazine propyl triethoxysilane acting as functional linker and methyltrimethoxysilane or hexamethyldisilizane as capped agents to mask the remaining silanol groups. Second, the appropiate titanium precursor Ti(OPr(i))(4), [{Ti(OPr(i))(3)(OMent)}(2)] (OMent = 1R,2S,5R-(-)-menthoxo), Ti(OPr(i))(4), or [Ti(eta(5)-C(5)HMe(4))Cl(3)], has been immobilized by reaction with the modified MCM-41. Finally, after Ti(OPr(i))(4) immobilization onto the organomodified support the reaction with the chiral (+)-diethyl-l-tartrate was accomplished. The materials without functional linker have been also prepared by reaction in one step of the capped agent and the titanium precursor with the mesoporous silica. Relevant correlations of titanium NMR resonance chemical shifts and line widths can be inferred depending on different factors. The immobilization procedure used to prepare titanium-based MCM-41 hybrid materials and the choice of the silylating reagents employed to mask the silanol groups present on the silica surfaces produce significant differences in the Ti NMR spectra. Furthermore, depending on the electronic and sterical influence of the substituents directly attached to the titanium center, chemical shifts and line widths are modified providing novel information about titanium structure.

Carbon-13 NMR of flavinoids

International Nuclear Information System (INIS)

Agrawal, P.K.

1989-01-01

The present book has been written with the objective of introducing the organic chemists with the conceptual and experimental basis required for interpretation of 13 C NMR spectra of a flavonoid and to a discussion of general usefulness of the technique in solving flavonoid structural problem. After a brief general introduction to the essential aspects of flavonoids and 13 C NMR spectroscopy, considerable emphasis has been placed in chapter 2 on the various experimental methods and the interpretation of spectral details which enable individual resonance lines to be associated with the appropriate carbons in a molecule. The whole bulk of the literature, published on 13 C NMR of flavonoids in the major journals upto 1986 alongwith some recent references of 1987 has been classified in several categories such as: flavonoids, isflavonoids, other flavonoids, flavonoid glycosides, chalconoids and flavanoids. Each category constitutes a chapter. Finally the last chapter is devoted largely to a discussion for the differentiation of various categories and subcategories of flavonoids and for the establishment of aromatic substitution pattern in these compounds. It should be emphasized that the book is a data book and only concerned with the actual analysis of 13 C NMR spectra, thus a reasonable familiarity with basic instrumentation of 13 C NMR and general pattern of nuclear chemical shifts has been assumed. (author). refs.; figs.; tabs

Optimization and practical implementation of ultrafast 2D NMR experiments

Energy Technology Data Exchange (ETDEWEB)

Queiroz Junior, Luiz H. K., E-mail: professorkeng@gmail.com [Universidade Federal de Sao Carlos (UFSC), SP (Brazil). Departamento de Quimica; Universidade Federal de Goias (UFGO), Goiania, GO (Brazil). Inst. de Quimica; Ferreira, Antonio G. [Universidade Federal de Sao Carlos (UFSC), SP (Brazil). Departamento de Quimica; Giraudeau, Patrick [Universite de Nantes (France). CNRS, Chimie et Interdisciplinarite: Synthese, Analyse, Modelisation

2013-09-01

Ultrafast 2D NMR is a powerful methodology that allows recording of a 2D NMR spectrum in a fraction of second. However, due to the numerous non-conventional parameters involved in this methodology its implementation is no trivial task. Here, an optimized experimental protocol is carefully described to ensure efficient implementation of ultrafast NMR. The ultrafast spectra resulting from this implementation are presented based on the example of two widely used 2D NMR experiments, COSY and HSQC, obtained in 0.2 s and 41 s, respectively. (author)

NMR imaging of the brain: initial impressions

International Nuclear Information System (INIS)

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

1983-01-01

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

2D COSY sup 1 H NMR; A new tool for studying in sity brain metabolism in the living animal

Energy Technology Data Exchange (ETDEWEB)

Barrere, B.; Peres, M.; Seulaz, J. (Universite Paris 7 (France). Laboratoire de Physiologie et Physiopathologie Cerebrovasculaire INSERM U 182 CNRS UA 641, Paris (France)); Gillet, B.; Mergui, S.; Beloeil, J.-C. (Centre National de la Recherche Scientifique, 91 - Gif-sur-Yvette (France). Inst. de Chimie des Substances Naturelles)

1990-05-21

2D COSY {sup 1}H NMR with surface coil has been used to resolve and assign cerebral metabolites which had previously been detected but could not be resolved or assigned in situ in the living animal by conventional 1D {sup 1}H NMR. A wide range of cerebral metabolites, including alanine, N-acetyl asparate, asparate, choline derivatives, creatine/phosphocreatine pool, GABA, glucose, glutamate/glutamine pool, inositol, lactate and taurine were simultaneously resolved and assigned in situ in the whole animal using the 2D COSY correlation graphs. Global irreversible ischemia caused the appearance and the disappearance of cross-peaks in the 2D COSY {sup 1}H NMR map, corresponding to increases in alanine, GABA and lactate and glucose depletion. (author). 21 refs.; 3 figs.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-03-22

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

NMR imaging of the cardiovascular system

International Nuclear Information System (INIS)

Canby, R.C.; Evanochko, W.T.; Pohost, G.M.

1986-01-01

Proton nuclear magnetic resonance (NMR) imaging permits high-resolution tomographic and three-dimensional images of the human body to be obtained without exposure to ionizing radiation. Such imaging not only yields anatomic resolution comparable to X-ray examinations but also provides a potential means to discriminate between healthy tissue and diseased tissue. This potential is based on certain NMR properties known as relaxation times, which determine, in part, the signal intensity in an image. These properties are related to such factors as the sizes and concentrations of proteins and mobile lipids and the compartmentalization of the protons of water. Although NMR imaging (also called magnetic resonance imaging, MRI) is becoming widely available for clinical use, application to the cardiovascular system, though promising, remains primarily a research tool. Gated proton NMR imaging can generate cardiac images with excellent morphologic detail and contrast; however, its ultimate importance as a cardiovascular diagnostic modality will depend on the development of several unique applications. These applications are discussed in this paper

Chemical profiling of anti-hepatocellular carcinoma constituents from Caragana tangutica Maxim. by off-line semi-preparative HPLC-NMR.

Science.gov (United States)

Yang, Xinzhou; Huang, Mi; Cai, Jinyan; Lv, Dan; Lv, Jingnan; Zheng, Sijian; Ma, Xinhua; Zhao, Ping; Wang, Qiang

2017-05-01

An EtOAc fraction from the roots of Caragana tangutica Maxim. (CTEA) displayed promising anti-hepatocellular carcinoma (HCC) activity during screening of a traditional Chinese ethnic herb library against HepG2 and Hep3B cell lines. HPLC-based activity profiling of CTEA by combination of MS-guided large-scale semi-preparative HPLC and NMR methods led to the identification of a new pterocarpan glycoside, (-)-maackiain 3-O-6'-O-methyl malonyl-β-d-glucopyranoside (1), together with three known pterocarpan glycosides, (-)-maackiain 3-O-β-d-glucopyranoside (2), 3-O-6'-O-acrylyl-β-d-galactopyranoside (3), and (-)-maackiain 3-O-6'-O-acetyl-β-d-glucopyranoside (4). Compound 1 was isolated during a drug discovery programme aimed at identifying new anti-HCC leads from a natural product library. Anti-HCC study showed that all four compounds exhibited cytotoxic activity with IC 50 values range of 29.1-53.5 μg/mL against HepG2 and Hep3B cell lines.

Mapping the surface of Escherichia coli peptide deformylase by NMR with organic solvents.

Science.gov (United States)

Byerly, Douglas W; McElroy, Craig A; Foster, Mark P

2002-07-01

Identifying potential ligand binding sites on a protein surface is an important first step for targeted structure-based drug discovery. While performing control experiments with Escherichia coli peptide deformylase (PDF), we noted that the organic solvents used to solubilize some ligands perturbed many of the same resonances in PDF as the small molecule inhibitors. To further explore this observation, we recorded (15)N HSQC spectra of E. coli peptide deformylase (PDF) in the presence of trace quantities of several simple organic solvents (acetone, DMSO, ethanol, isopropanol) and identified their sites of interaction from local perturbation of amide chemical shifts. Analysis of the protein surface structure revealed that the ligand-induced shift perturbations map to the active site and one additional surface pocket. The correlation between sites of solvent and inhibitor binding highlights the utility of organic solvents to rapidly and effectively validate and characterize binding sites on proteins prior to designing a drug discovery screen. Further, the solvent-induced perturbations have implications for the use of organic solvents to dissolve candidate ligands in NMR-based screens.

Improving Visualization and Interpretation of Metabolome-Wide Association Studies: An Application in a Population-Based Cohort Using Untargeted 1H NMR Metabolic Profiling.

Science.gov (United States)

Castagné, Raphaële; Boulangé, Claire Laurence; Karaman, Ibrahim; Campanella, Gianluca; Santos Ferreira, Diana L; Kaluarachchi, Manuja R; Lehne, Benjamin; Moayyeri, Alireza; Lewis, Matthew R; Spagou, Konstantina; Dona, Anthony C; Evangelos, Vangelis; Tracy, Russell; Greenland, Philip; Lindon, John C; Herrington, David; Ebbels, Timothy M D; Elliott, Paul; Tzoulaki, Ioanna; Chadeau-Hyam, Marc

2017-10-06

1 H NMR spectroscopy of biofluids generates reproducible data allowing detection and quantification of small molecules in large population cohorts. Statistical models to analyze such data are now well-established, and the use of univariate metabolome wide association studies (MWAS) investigating the spectral features separately has emerged as a computationally efficient and interpretable alternative to multivariate models. The MWAS rely on the accurate estimation of a metabolome wide significance level (MWSL) to be applied to control the family wise error rate. Subsequent interpretation requires efficient visualization and formal feature annotation, which, in-turn, call for efficient prioritization of spectral variables of interest. Using human serum 1 H NMR spectroscopic profiles from 3948 participants from the Multi-Ethnic Study of Atherosclerosis (MESA), we have performed a series of MWAS for serum levels of glucose. We first propose an extension of the conventional MWSL that yields stable estimates of the MWSL across the different model parameterizations and distributional features of the outcome. We propose both efficient visualization methods and a strategy based on subsampling and internal validation to prioritize the associations. Our work proposes and illustrates practical and scalable solutions to facilitate the implementation of the MWAS approach and improve interpretation in large cohort studies.

Knowns and unknowns in metabolomics identified by multidimensional NMR and hybrid MS/NMR methods

Energy Technology Data Exchange (ETDEWEB)

Bingol, Kerem; Brüschweiler, Rafael

2017-02-01

Metabolomics continues to make rapid progress through the development of new and better methods and their applications to gain insight into the metabolism of a wide range of different biological systems from a systems biology perspective. Customization of NMR databases and search tools allows the faster and more accurate identification of known metabolites, whereas the identification of unknowns, without a need for extensive purification, requires new strategies to integrate NMR with mass spectrometry, cheminformatics, and computational methods. For some applications, the use of covalent and non-covalent attachments in the form of labeled tags or nanoparticles can significantly reduce the complexity of these tasks.

Effects of diffusion and surface interactions on the line shape of electron paramagnetic resonances in the presence of a magnetic field gradient

International Nuclear Information System (INIS)

Schaden, M.; Zhao, K. F.; Wu, Z.

2007-01-01

In an evanescent wave magnetometer the Zeeman polarization is probed at micrometer to submicrometer distances from the cell surface. The electron paramagnetic resonance lines of an evanescent wave magnetometer in the presence of a magnetic field gradient exhibit edge enhancement seen previously in nuclear magnetic resonance lines. We present a theoretical model that describes quantitatively the shape of the magnetic resonance lines of an evanescent wave magnetometer under a wide range of experimental conditions. It accounts for diffusion broadening in the presence of a magnetic field gradient as well as interactions of spin polarized Rb atoms with the coated Pyrex glass surfaces. Depending on the field gradient, cell thickness, and buffer gas pressure, the resonance line may have the form of a single asymmetric peak or two peaks localized near the front and back surfaces in frequency space. The double-peaked response depends on average characteristics of the surface interactions. Its shape is sensitive to the dwell time, relaxation probability, and average phase shift of adsorbed spin polarized Rb atoms

A Solid-State Deuterium NMR and SFG Study of the Side Chain Dynamics of Peptides Adsorbed onto Surfaces

Science.gov (United States)

Breen, Nicholas F.; Weidner, Tobias; Li, Kun; Castner, David G.; Drobny, Gary P.

2011-01-01

The artificial amphiphilic peptide LKα14 adopts a helical structure at interfaces, with opposite orientation of its leucine (L, hydrophobic) and lysine (K, hydrophilic) side chains. When adsorbed onto surfaces, different residue side chains necessarily have different proximities to the surface, depending on both their position in the helix and the composition of the surface itself. Deuterating the individual leucine residues (isopropyl-d7) permits the use of solid-state deuterium NMR as a site-specific probe of side chain dynamics. In conjunction with SFG as a probe of the peptide binding face, we demonstrate that the mobility of specific leucine side chains at the interface is quantifiable in terms of their surface proximity. PMID:19764755

129 Xe-NMR of carbon black filled elastomers

International Nuclear Information System (INIS)

Sperling-Ischinsky, K.; Veeman, W.S.

1999-01-01

It is shown that 129 Xe-NMR is a powerful tool to investigate carbon black and carbon black filled elastomers. For the carbon black material itself the 129 Xe chemical shift of xenon adsorbed at the surface of carbon black aggregates yields information about the relative average pore size of the carbon black aggregates. The experimental 129 Xe-NMR results of carbon black filled ethylene-propylene-diene (EPDM) can be explained when it is assumed that the xenon atoms in the bound EPDM fraction exchange rapidly on the NMR time scale between a state where they are adsorbed on the carbon black surface and a state in which they are absorbed in the EPDM layer. This would imply that the carbon black aggregates are not completely covered with EPDM chains. (author)

Crystallographically-based analysis of the NMR spectra of maghemite

International Nuclear Information System (INIS)

Spiers, K.M.; Cashion, J.D.

2012-01-01

All possible iron environments with respect to nearest neighbour vacancies in vacancy-ordered and vacancy-disordered maghemite have been evaluated and used as the foundation for a crystallographically-based analysis of the published NMR spectra of maghemite. The spectral components have been assigned to particular configurations and excellent agreement obtained in comparing predicted spectra with published spectra taken in applied magnetic fields. The broadness of the published NMR lines has been explained by calculations of the magnetic dipole fields at the various iron sites and consideration of the supertransferred hyperfine fields. - Highlights: ► Analysis of 57 Fe NMR of maghemite based on vacancy ordering and nearest neighbour vacancies. ► Assignment of NMR spectral components based on crystallographic analysis of unique iron sites. ► Strong agreement between predicted spectra and published spectra taken in applied magnetic fields. ► Maghemite NMR spectral broadening due to various iron sites and supertransferred hyperfine field.

NMR studies of metallic tin confined within porous matrices

International Nuclear Information System (INIS)

Charnaya, E. V.; Tien, Cheng; Lee, M. K.; Kumzerov, Yu. A.

2007-01-01

119 Sn NMR studies were carried out for metallic tin confined within synthetic opal and porous glass. Tin was embedded into nanoporous matrices in the melted state under pressure. The Knight shift for liquid confined tin was found to decrease with decreasing pore size. Correlations between NMR line shapes, Knight shift, and pore filling were observed. The melting and freezing phase transitions of tin under confinement were studied through temperature dependences of NMR signals upon warming and cooling. Melting of tin within the opal matrix agreed well with the liquid skin model suggested for small isolated particles. The influence of the pore filling on the melting process was shown

Mixture analysis by long-range J-resolved 2D NMR

International Nuclear Information System (INIS)

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

1987-01-01

In most spectroscopic qualitative analyses chromatographic separations are done before identification. Unfortunately, this general approach has suffered from a number of shortcomings. Off-line chromatographic separation followed by spectroscopic analysis is time consuming and inefficient and on-line analysis suffers from mismatch of the material flow requirements between chromatographic columns and spectroscopic instruments. An alternative mixture identification procedure solely based upon use of edited 13 C NMR spectra and a 13 C NMR chemical shift data base is reported. This approach has been demonstrated in the analyses of several mixtures, including a mixture of amino acids and some isomers. In all cases, identifications of components of these mixtures are successful

Development and applications of quantitative NMR spectroscopy

International Nuclear Information System (INIS)

Yamazaki, Taichi

2016-01-01

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

On low-dimensional models at NMR line shape analysis in nanomaterial systems

Science.gov (United States)

Kucherov, M. M.; Falaleev, O. V.

2018-03-01

We present a model of localized spin dynamics at room temperature for the low-dimensional solid-state spin system, which contains small ensembles of magnetic nuclei (N ~ 40). The standard spin Hamiltonian (XXZ model) is the sum of the Zeeman term in a strong external magnetic field and the magnetic dipole interaction secular term. The 19F spins in a single crystal of fluorapatite [Ca5(PO4)3F] have often been used to approximate a one-dimensional spin system. If the constant external field is parallel to the c axis, the 3D 19F system may be treated as a collection of many identical spin chains. When considering the longitudinal part of the secular term, we suggest that transverse component of a spin in a certain site rotates in a constant local magnetic field. This field changes if the spin jumps to another site. On return, this spin continues to rotate in the former field. Then we expand the density matrix in a set of eigenoperators of the Zeeman Hamiltonian. A system of coupled differential equations for the expansion coefficients then solved by straightforward numerical methods, and the fluorine NMR line shapes of fluorapatite for different chain lengths are calculated.

Natural abundant (17) O NMR in a 1.5-T Halbach magnet.

Science.gov (United States)

Sørensen, Morten K; Bakharev, Oleg N; Jensen, Ole; Nielsen, Niels Chr

2016-06-01

We present mobile, low-field (17) O NMR as a means for monitoring oxygen in liquids. Whereas oxygen is one of the most important elements, oxygen NMR is limited by a poor sensitivity related to low natural abundance and gyro-magnetic ratio of the NMR active (17) O isotope. Here, we demonstrate (17) O NMR detection at a Larmor frequency of 8.74 MHz in a 1.5-T Halbach neodymium magnet with a home-built digital NMR instrument suitable for large-scale production and in-line monitoring applications. The proposed (17) O NMR sensor may be applied for direct, noninvasive measurements of water content in, for example, oil, manure, or food in automated quality or process control. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

AEM and NMR: Tools for the Future of Groundwater Management

Science.gov (United States)

Abraham, J. D.; Cannia, J. C.; Lawrie, K.

2012-12-01

nuclear magnetization of the hydrogen (protons) in the water. These measurements are the basis of the familiar MRI (magnetic resonance imaging) in medical applications. NMR is also widely used in logging applications within the petroleum industry. Effective porosity values were derived directly from the borehole and surface NMR data, and hydraulic conductivity values were calculated using empirical relationships calibrated and verified with few laboratory permeameter and aquifer tests. NMR provides measurements of the effective porosity and hydraulic conductivity at a resolution not possible using traditional methods. Unlike aquifer tests, NMR logs are not unique in design and are applied in similar fashion from borehole to borehole providing a standard way of measuring hydraulic properties. When the hydraulic properties from the NMR are integrated with hydrogeological framework interpretations of AEM data large areas can be characterized. This allows a much more robust method for conceptualizing groundwater models then simply using previously published data for assigning effective porosity and hydraulic conductivity. Examples from the North Platte River Basin in Nebraska and the Murray Darling Basin of Australia illustrate that borehole and surface NMR allows superior, rapid measurements of the complexities of aquifers within when integrated with AEM.

Improvement of Surface Layer Characteristics by Shot Lining

Science.gov (United States)

Harada, Yasunori

In the present study, lining of the metal with foils using shot peening was investigated to improve the surface layer characteristics. In the shot peening experiment, the foils set on the metal are pelted with hard particles traveling at a high velocity. The foils are bonded to the metal surface due to plastic deformation induced by the collision of the particles. The foils and the metal are heated to heighten the bondability because of the reduction of flow stress. Lining the metal with the hard powder sandwiched between two aluminum foil sheets was also attempted. In this experiment, a centrifugal shot peening machine wite an electrical heater was employed. The metals are commercially aluminium alloys and magnesium alloys, and the foils are commercially aluminum, titanium and nickel. The effects of shot speed and the heating temperature on the bondability were examined. Wear resistance was also evaluated by grinding. The foils were successfully bonded to the metal surface. It was found that the present method is effective in improving of surface layer characteristics.

Realization of seven-qubit Deutsch-Jozsa algorithm on NMR quantum computer

International Nuclear Information System (INIS)

Wei Daxiu; Yang Xiaodong; Luo Jun; Sun Xianping; Zeng Xizhi; Liu Maili; Ding Shangwu

2002-01-01

Recent years, remarkable progresses in experimental realization of quantum information have been made, especially based on nuclear magnetic resonance (NMR) theory. In all quantum algorithms, Deutsch-Jozsa algorithm has been widely studied. It can be realized on NMR quantum computer and also can be simplified by using the Cirac's scheme. At first the principle of Deutsch-Jozsa quantum algorithm is analyzed, then the authors implement the seven-qubit Deutsch-Jozsa algorithm on NMR quantum computer

NMR shielding calculations across the periodic table: diamagnetic uranium compounds. 2. Ligand and metal NMR.

Science.gov (United States)

Schreckenbach, Georg

2002-12-16

In this and a previous article (J. Phys. Chem. A 2000, 104, 8244), the range of application for relativistic density functional theory (DFT) is extended to the calculation of nuclear magnetic resonance (NMR) shieldings and chemical shifts in diamagnetic actinide compounds. Two relativistic DFT methods are used, ZORA ("zeroth-order regular approximation") and the quasirelativistic (QR) method. In the given second paper, NMR shieldings and chemical shifts are calculated and discussed for a wide range of compounds. The molecules studied comprise uranyl complexes, [UO(2)L(n)](+/-)(q); UF(6); inorganic UF(6) derivatives, UF(6-n)Cl(n), n = 0-6; and organometallic UF(6) derivatives, UF(6-n)(OCH(3))(n), n = 0-5. Uranyl complexes include [UO(2)F(4)](2-), [UO(2)Cl(4)](2-), [UO(2)(OH)(4)](2-), [UO(2)(CO(3))(3)](4-), and [UO(2)(H(2)O)(5)](2+). For the ligand NMR, moderate (e.g., (19)F NMR chemical shifts in UF(6-n)Cl(n)) to excellent agreement [e.g., (19)F chemical shift tensor in UF(6) or (1)H NMR in UF(6-n)(OCH(3))(n)] has been found between theory and experiment. The methods have been used to calculate the experimentally unknown (235)U NMR chemical shifts. A large chemical shift range of at least 21,000 ppm has been predicted for the (235)U nucleus. ZORA spin-orbit appears to be the most accurate method for predicting actinide metal chemical shifts. Trends in the (235)U NMR chemical shifts of UF(6-n)L(n) molecules are analyzed and explained in terms of the calculated electronic structure. It is argued that the energy separation and interaction between occupied and virtual orbitals with f-character are the determining factors.

Nature and structure of aluminum surface sites grafted on silica from a combination of high-field aluminum-27 solid-state NMR spectroscopy and first-principles calculations

KAUST Repository

Kerber, Rachel Nathaniel; Kermagoret, Anthony; Callens, Emmanuel; Florian, Pierre A.; Massiot, Dominique; Lesage, Anne; Copé ret, Christophe; Delbecq, Franç oise; Rozanska, Xavier; Sautet, Philippe

2012-01-01

The determination of the nature and structure of surface sites after chemical modification of large surface area oxides such as silica is a key point for many applications and challenging from a spectroscopic point of view. This has been, for instance, a long-standing problem for silica reacted with alkylaluminum compounds, a system typically studied as a model for a supported methylaluminoxane and aluminum cocatalyst. While 27Al solid-state NMR spectroscopy would be a method of choice, it has been difficult to apply this technique because of large quadrupolar broadenings. Here, from a combined use of the highest stable field NMR instruments (17.6, 20.0, and 23.5 T) and ultrafast magic angle spinning (>60 kHz), high-quality spectra were obtained, allowing isotropic chemical shifts, quadrupolar couplings, and asymmetric parameters to be extracted. Combined with first-principles calculations, these NMR signatures were then assigned to actual structures of surface aluminum sites. For silica (here SBA-15) reacted with triethylaluminum, the surface sites are in fact mainly dinuclear Al species, grafted on the silica surface via either two terminal or two bridging siloxy ligands. Tetrahedral sites, resulting from the incorporation of Al inside the silica matrix, are also seen as minor species. No evidence for putative tri-coordinated Al atoms has been found. © 2012 American Chemical Society.

Nature and structure of aluminum surface sites grafted on silica from a combination of high-field aluminum-27 solid-state NMR spectroscopy and first-principles calculations

KAUST Repository

Kerber, Rachel Nathaniel

2012-04-18

The determination of the nature and structure of surface sites after chemical modification of large surface area oxides such as silica is a key point for many applications and challenging from a spectroscopic point of view. This has been, for instance, a long-standing problem for silica reacted with alkylaluminum compounds, a system typically studied as a model for a supported methylaluminoxane and aluminum cocatalyst. While 27Al solid-state NMR spectroscopy would be a method of choice, it has been difficult to apply this technique because of large quadrupolar broadenings. Here, from a combined use of the highest stable field NMR instruments (17.6, 20.0, and 23.5 T) and ultrafast magic angle spinning (>60 kHz), high-quality spectra were obtained, allowing isotropic chemical shifts, quadrupolar couplings, and asymmetric parameters to be extracted. Combined with first-principles calculations, these NMR signatures were then assigned to actual structures of surface aluminum sites. For silica (here SBA-15) reacted with triethylaluminum, the surface sites are in fact mainly dinuclear Al species, grafted on the silica surface via either two terminal or two bridging siloxy ligands. Tetrahedral sites, resulting from the incorporation of Al inside the silica matrix, are also seen as minor species. No evidence for putative tri-coordinated Al atoms has been found. © 2012 American Chemical Society.

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

International Nuclear Information System (INIS)

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

1985-01-01

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

Mechanism of formation of humus coatings on mineral surfaces 3. Composition of adsorbed organic acids from compost leachate on alumina by solid-state 13C NMR

Science.gov (United States)

Wershaw, R. L.; Llaguno, E.C.; Leenheer, J.A.

1996-01-01

The adsorption of compost leachate DOC on alumina is used as a model for elucidation of the mechanism of formation of natural organic coatings on hydrous metal oxide surfaces in soils and sediments. Compost leachate DOC is composed mainly of organic acid molecules. The solid-state 13C NMR spectra of these organic acids indicate that they are very similar in composition to aquatic humic substances. Changes in the solid-state 13C NMR spectra of compost leachate DOC fractions adsorbed on alumina indicate that the DOC molecules are most likely adsorbed on metal oxide surfaces through a combination of polar and hydrophobic interaction mechanisms. This combination of polar and hydrophobic mechanism leads to the formation of bilayer coatings of the leachate molecules on the oxide surfaces.

DISCRETIZATION APPROACH USING RAY-TESTING MODEL IN PARTING LINE AND PARTING SURFACE GENERATION

Institute of Scientific and Technical Information of China (English)

HAN Jianwen; JIAN Bin; YAN Guangrong; LEI Yi

2007-01-01

Surface classification, 3D parting line, parting surface generation and demoldability analysis which is helpful to select optimal parting direction and optimal parting line are involved in automatic cavity design based on the ray-testing model. A new ray-testing approach is presented to classify the part surfaces to core/cavity surfaces and undercut surfaces by automatic identifying the visibility of surfaces. A simple, direct and efficient algorithm to identify surface visibility is developed. The algorithm is robust and adapted to rather complicated geometry, so it is valuable in computer-aided mold design systems. To validate the efficiency of the approach, an experimental program is implemented. Case studies show that the approach is practical and valuable in automatic parting line and parting surface generation.

Amorphous surface layer versus transient amorphous precursor phase in bone - A case study investigated by solid-state NMR spectroscopy.

Science.gov (United States)

Von Euw, Stanislas; Ajili, Widad; Chan-Chang, Tsou-Hsi-Camille; Delices, Annette; Laurent, Guillaume; Babonneau, Florence; Nassif, Nadine; Azaïs, Thierry

2017-09-01

The presence of an amorphous surface layer that coats a crystalline core has been proposed for many biominerals, including bone mineral. In parallel, transient amorphous precursor phases have been proposed in various biomineralization processes, including bone biomineralization. Here we propose a methodology to investigate the origin of these amorphous environments taking the bone tissue as a key example. This study relies on the investigation of a bone tissue sample and its comparison with synthetic calcium phosphate samples, including a stoichiometric apatite, an amorphous calcium phosphate sample, and two different biomimetic apatites. To reveal if the amorphous environments in bone originate from an amorphous surface layer or a transient amorphous precursor phase, a combined solid-state nuclear magnetic resonance (NMR) experiment has been used. The latter consists of a double cross polarization 1 H→ 31 P→ 1 H pulse sequence followed by a 1 H magnetization exchange pulse sequence. The presence of an amorphous surface layer has been investigated through the study of the biomimetic apatites; while the presence of a transient amorphous precursor phase in the form of amorphous calcium phosphate particles has been mimicked with the help of a physical mixture of stoichiometric apatite and amorphous calcium phosphate. The NMR results show that the amorphous and the crystalline environments detected in our bone tissue sample belong to the same particle. The presence of an amorphous surface layer that coats the apatitic core of bone apatite particles has been unambiguously confirmed, and it is certain that this amorphous surface layer has strong implication on bone tissue biogenesis and regeneration. Questions still persist on the structural organization of bone and biomimetic apatites. The existing model proposes a core/shell structure, with an amorphous surface layer coating a crystalline bulk. The accuracy of this model is still debated because amorphous calcium

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

International Nuclear Information System (INIS)

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

1991-01-01

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

Adiabatic sweep pulses for earth's field NMR with a surface coil

Science.gov (United States)

Conradi, Mark S.; Altobelli, Stephen A.; Sowko, Nicholas J.; Conradi, Susan H.; Fukushima, Eiichi

2018-03-01

Adiabatic NMR sweep pulses are described for inversion and excitation in very low magnetic fields B0 and with broad distribution of excitation field amplitude B1. Two aspects distinguish the low field case: (1) when B1 is comparable to or greater than B0, the rotating field approximation fails and (2) inversion sweeps cannot extend to values well below the Larmor frequency because they would approach or pass through zero frequency. Three approaches to inversion are described. The first is a conventional tangent frequency sweep down to the Larmor frequency, a 180° phase shift, and a sweep back up to the starting frequency. The other two are combined frequency and amplitude sweeps covering a narrower frequency range; one is a symmetric sweep from above to below the Larmor frequency and the other uses a smooth decrease of B1 immediately before and after the 180° phase shift. These two AM/FM sweeps show excellent inversion efficiencies over a wide range of B1, a factor of 30 or more. We also demonstrate an excitation sweep that works well in the presence of the same wide range of B1. We show that the primary effect of the counter-rotating field (i.e., at low B0) is that the magnetization suffers large, periodic deviations from where it would be at large B0. Thus, successful sweep pulses must avoid any sharp features in the amplitude, phase, or frequency.

WaVPeak: Picking NMR peaks through wavelet-based smoothing and volume-based filtering

KAUST Repository

Liu, Zhi; Abbas, Ahmed; Jing, Bing-Yi; Gao, Xin

2012-01-01

Motivation: Nuclear magnetic resonance (NMR) has been widely used as a powerful tool to determine the 3D structures of proteins in vivo. However, the post-spectra processing stage of NMR structure determination usually involves a tremendous amount

Arrays of Molecular Rotors with Triptycene Stoppers: Surface Inclusion in Hexagonal Tris(o-phenylenedioxy)cyclotriphosphazene.

Science.gov (United States)

Kaleta, Jiří; Dron, Paul I; Zhao, Ke; Shen, Yongqiang; Císařová, Ivana; Rogers, Charles T; Michl, Josef

2015-06-19

A new generation of rod-shaped dipolar molecular rotors designed for controlled insertion into channel arrays in the surface of hexagonal tris(o-phenylenedioxy)cyclotriphosphazene (TPP) has been designed and synthesized. Triptycene is used as a stopper intended to prevent complete insertion, forcing the formation of a surface inclusion. Two widely separated (13)C NMR markers are present in the shaft for monitoring the degree of insertion. The structure of the two-dimensional rotor arrays contained in these surface inclusions was examined by solid-state NMR and X-ray powder diffraction. The NMR markers and the triptycene stopper functioned as designed, but half of the guest molecules were not inserted as deeply into the TPP channels as the other half. As a result, the dipolar rotators were distributed equally in two planes parallel to the crystal surface instead of being located in a single plane as would be required for ferroelectricity. Dielectric spectroscopy revealed rotational barriers of ∼4 kcal/mol but no ferroelectric behavior.

Application Of The SPV-based Surface Lifetime Technique To In-Line Monitoring Of Surface Cu Contamination

Science.gov (United States)

D'Amico, John; Savtchouk, Alexandre; Wilson, Matthew; Kim, Chul Hong; Yoo, Hyung Won; Lee, Chang Hwan; Kim, Tae Kyoung; Son, Sang Hoon

2009-09-01

Implementation of Cu interconnects into Silicon Integrated Circuits (IC's) has been instrumental in the continuing improvement of IC device performance. Copper as a well known Gate Oxide Integrity (GOI) killer [1, 2] requires extensive protocols to minimize the possibility of cross contamination. Despite such protocols the risk for cross contamination exists, and consequently there is the need for in-line Cu cross-contamination detection metrology. Preferably the metrology will be non-destructive, fast, and capable of mapping on product wafers. Up to now the most common approaches for monitoring Cu contamination in IC fabrication lines either measure Cu in the bulk Si, which is not applicable to Cu cross-contamination monitoring because Back-End-of-the-Line thermal budgets restrict the ability to diffuse the surface Cu into the bulk Si; or the techniques are not optimal for in-line monitoring due to their destructive, time-consuming, or costly nature. In this work we demonstrate for the first time the application of the ac-Surface Photo Voltage (ac-SPV) surface lifetime approach [3] to in-line, full wafer coverage mapping of low level (metrology system. Furthermore, because the metrology is non-contact (utilizing edge-grip handling) and non-destructive, it is directly applicable to measurement of production wafers. In-line fab data acquired using this metrology is presented and compared to data from Inductively Coupled Plasma Mass Spectroscopy (ICP-MS).

NMR studies of interfaces, strain and anisotropy in Co/Cu multilayers

International Nuclear Information System (INIS)

Thomson, T.; Riedi, P.C.

1999-01-01

59 Co NMR studies of multilayers are able to give three direct pieces of information: (i) the crystal phase of Co, fcc (217.4 MHz), hcp (220-228 MHz) and in exotic cases bcc (198 MHz) for films measured at T= 4.2 K, (ii) the nature of the interfaces from low frequency satellite lines, and (iii) the strain state deduced from small changes in the line positions. Extensive studies of Co/Cu multilayer interfacial structures as a function of deposition technique, layer thickness, substrate/buffer layer structure and annealing temperature have been undertaken. This work has shed new light on the relationship between interfacial structure and magnetoresistance and in particular has demonstrated that flat, atomic scale, interfaces lead to greater magnetoresistance. The difference between the Co and Cu lattice constant results in an extensive, tensile in-plane strain developing in Co layers provided that some epitaxial registry is present. Information on strain effects can be obtained from the position and width of the NMR lines. The magnetic anisotropy field can be determined by measuring the field dependence of the enhancement effect due to electronic magnetisation. This provides unique insight into the distribution of magnetic anisotropy within the Co layers, as the enhancement can be investigated independently for each NMR line and, hence, provides environment specific information on magnetic anisotropy at the interfaces and in the interior of the layers

Extracting protein dynamics information from overlapped NMR signals using relaxation dispersion difference NMR spectroscopy.

Science.gov (United States)

Konuma, Tsuyoshi; Harada, Erisa; Sugase, Kenji

2015-12-01

Protein dynamics plays important roles in many biological events, such as ligand binding and enzyme reactions. NMR is mostly used for investigating such protein dynamics in a site-specific manner. Recently, NMR has been actively applied to large proteins and intrinsically disordered proteins, which are attractive research targets. However, signal overlap, which is often observed for such proteins, hampers accurate analysis of NMR data. In this study, we have developed a new methodology called relaxation dispersion difference that can extract conformational exchange parameters from overlapped NMR signals measured using relaxation dispersion spectroscopy. In relaxation dispersion measurements, the signal intensities of fluctuating residues vary according to the Carr-Purcell-Meiboon-Gill pulsing interval, whereas those of non-fluctuating residues are constant. Therefore, subtraction of each relaxation dispersion spectrum from that with the highest signal intensities, measured at the shortest pulsing interval, leaves only the signals of the fluctuating residues. This is the principle of the relaxation dispersion difference method. This new method enabled us to extract exchange parameters from overlapped signals of heme oxygenase-1, which is a relatively large protein. The results indicate that the structural flexibility of a kink in the heme-binding site is important for efficient heme binding. Relaxation dispersion difference requires neither selectively labeled samples nor modification of pulse programs; thus it will have wide applications in protein dynamics analysis.

Extracting protein dynamics information from overlapped NMR signals using relaxation dispersion difference NMR spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Konuma, Tsuyoshi [Icahn School of Medicine at Mount Sinai, Department of Structural and Chemical Biology (United States); Harada, Erisa [Suntory Foundation for Life Sciences, Bioorganic Research Institute (Japan); Sugase, Kenji, E-mail: sugase@sunbor.or.jp, E-mail: sugase@moleng.kyoto-u.ac.jp [Kyoto University, Department of Molecular Engineering, Graduate School of Engineering (Japan)

2015-12-15

Protein dynamics plays important roles in many biological events, such as ligand binding and enzyme reactions. NMR is mostly used for investigating such protein dynamics in a site-specific manner. Recently, NMR has been actively applied to large proteins and intrinsically disordered proteins, which are attractive research targets. However, signal overlap, which is often observed for such proteins, hampers accurate analysis of NMR data. In this study, we have developed a new methodology called relaxation dispersion difference that can extract conformational exchange parameters from overlapped NMR signals measured using relaxation dispersion spectroscopy. In relaxation dispersion measurements, the signal intensities of fluctuating residues vary according to the Carr-Purcell-Meiboon-Gill pulsing interval, whereas those of non-fluctuating residues are constant. Therefore, subtraction of each relaxation dispersion spectrum from that with the highest signal intensities, measured at the shortest pulsing interval, leaves only the signals of the fluctuating residues. This is the principle of the relaxation dispersion difference method. This new method enabled us to extract exchange parameters from overlapped signals of heme oxygenase-1, which is a relatively large protein. The results indicate that the structural flexibility of a kink in the heme-binding site is important for efficient heme binding. Relaxation dispersion difference requires neither selectively labeled samples nor modification of pulse programs; thus it will have wide applications in protein dynamics analysis.

NMR measurements in milled GdCo2 and GdFe2 intermetallic compounds

International Nuclear Information System (INIS)

Tribuzy, C.V.B.; Guimaraes, A.P.; Biondo, A.; Larica, C.; Alves, K.M.B.

1998-12-01

We have used the nuclear magnetic resonance technique to study the magnetic and structural properties of the Gd-Co and Gd-Fe metallic systems, starting with the C15 laves phase intermetallic compounds, and submitting them to a high energy milling process. This leads to the amorphization of the samples, as determined by the X-ray diffraction spectra. For the Gd-Co system the NMR study used the 59 Co nucleus; in the Gd-Fe system, 155,157 Gd and 57 Fe were used. Both systems showed segregation of the pure elements, after a few hours of milling. In the Gd-Co system, a single line, of increasing width, was observed in the 59 Co spectrum. In the Gd-Fe system, the 155 Gd and 157 Gd resonances show three lines, arising from electrical quadrupole interaction. With increasing milling time, the lines broaden, and extra lines appear attributed to a cubic phase of Gd; this interpretation is supported by the X-ray analysis of the samples. The 57 Fe NMR spectrum of this system also informs on the direction of magnetization of the samples in the early stages of milling. From 1 h to 7 h of milling, a spectrum of α-Fe was observed. The study of the NMR line intensity as a function of radio frequency (r.f.) power in Gd Co 2 suggests the existence of regions of the samples with different degrees of disorder. We have observed the persistence of NMR signals from the original intermetallic compounds in the samples with up to 10 h and 7 h of milling, respectively, for Gd Co 2 and Gd Fe 2 . (author)

Reassessment of MxiH subunit orientation and fold within native Shigella T3SS needles using surface labelling and solid-state NMR.

Science.gov (United States)

Verasdonck, Joeri; Shen, Da-Kang; Treadgold, Alexander; Arthur, Christopher; Böckmann, Anja; Meier, Beat H; Blocker, Ariel J

2015-12-01

T3SSs are essential virulence determinants of many Gram-negative bacteria, used to inject bacterial effectors of virulence into eukaryotic host cells. Their major extracellular portion, a ∼50 nm hollow, needle-like structure, is essential to host cell sensing and the conduit for effector secretion. It is formed of a small, conserved subunit arranged as a helical polymer. The structure of the subunit has been studied by electron cryomicroscopy within native polymers and by solid-state NMR in recombinant polymers, yielding two incompatible atomic models. To resolve this controversy, we re-examined the native polymer used for electron cryomicroscopy via surface labelling and solid-state NMR. Our data show the orientation and overall fold of the subunit within this polymer is as established by solid-state NMR for recombinant polymers. Copyright © 2015 The Authors. Published by Elsevier Inc. All rights reserved.

A 55Mn NMR Study of the La0.75Sr0.25MnO3 Nanoparticles

International Nuclear Information System (INIS)

Kapusta, Cz.; Rybicki, D.; Sikora, M.

2005-01-01

We report on a 55 Mn NMR study of the La 0.75 Sr 0.25 MnO 3 nanoparticles with the average grain size of 33 nm and 114 nm at 4.2 K and at the applied field 0, 0.2 and 0.5 T. A dominant signal from the double exchange (DE) controlled metallic ferromagnetic interior of the grains as well as a small signal from insulating ferromagnetic surface regions of the grains are observed. The DE resonant line shows a frequency shift in the applied field according to a full gyromagnetic ratio and a value of the demagnetizing field much smaller than 0.2 T is obtained. In both samples studied a two-exponential nuclear spin-spin (T 2 ) relaxation is observed at zero field, whereas a single-exponential relaxation is observed at the applied field of 0.5 T. For the sample with larger grains a higher NMR enhancement is observed, which indicates a higher magnetic susceptibility of the sample at the NMR frequencies. A comparison to the NMR data obtained on a bulk material is made. The results are discussed in terms of the influence of the grain size and on the presence of domain walls or other magnetic inhomogeneities and on the magnetic anisotropy

Line operators from M-branes on compact Riemann surfaces

Energy Technology Data Exchange (ETDEWEB)

Amariti, Antonio [Physics Department, The City College of the CUNY, 160 Convent Avenue, New York, NY 10031 (United States); Orlando, Domenico [Albert Einstein Center for Fundamental Physics, Institute for Theoretical Physics, University of Bern, Sidlerstrasse 5, CH-3012 Bern (Switzerland); Reffert, Susanne, E-mail: sreffert@itp.unibe.ch [Albert Einstein Center for Fundamental Physics, Institute for Theoretical Physics, University of Bern, Sidlerstrasse 5, CH-3012 Bern (Switzerland)

2016-12-15

In this paper, we determine the charge lattice of mutually local Wilson and 't Hooft line operators for class S theories living on M5-branes wrapped on compact Riemann surfaces. The main ingredients of our analysis are the fundamental group of the N-cover of the Riemann surface, and a quantum constraint on the six-dimensional theory. The latter plays a central role in excluding some of the possible lattices and imposing consistency conditions on the charges. This construction gives a geometric explanation for the mutual locality among the lines, fixing their charge lattice and the structure of the four-dimensional gauge group.

Bioanalytical Applications of Fluorescence Line-Narrowing and Non-Line-Narrowing Spectroscopy Interfaced with Capillary Electrophoresis and High-Performance Liquid Chromatography

Energy Technology Data Exchange (ETDEWEB)

Roberts, Kenneth Paul [Iowa State Univ., Ames, IA (United States)

2001-01-01

Capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) are widely used analytical separation techniques with many applications in chemical, biochemical, and biomedical sciences. Conventional analyte identification in these techniques is based on retention/migration times of standards; requiring a high degree of reproducibility, availability of reliable standards, and absence of coelution. From this, several new information-rich detection methods (also known as hyphenated techniques) are being explored that would be capable of providing unambiguous on-line identification of separating analytes in CE and HPLC. As further discussed, a number of such on-line detection methods have shown considerable success, including Raman, nuclear magnetic resonance (NMR), mass spectrometry (MS), and fluorescence line-narrowing spectroscopy (FLNS). In this thesis, the feasibility and potential of combining the highly sensitive and selective laser-based detection method of FLNS with analytical separation techniques are discussed and presented. A summary of previously demonstrated FLNS detection interfaced with chromatography and electrophoresis is given, and recent results from on-line FLNS detection in CE (CE-FLNS), and the new combination of HPLC-FLNS, are shown.

NMR signal analysis in the large COMPASS $^{14}$NH$_{3}$ target

CERN Document Server

Koivuniemi, J; Hess, C; Kisselev, Y U; Meyer, W; Radtke, E; Reicherz, G; Doshita, N; Iwata, T; Kondo, K; Michigami, T

2009-01-01

In the large COMPASS polarized proton target the 1508 cm$^{3}$ of irradiated granular ammonia is polarized with dynamic nuclear polarization method using 4 mm microwaves in 2.5 T eld. The nuclear polarization up to 90 - 93 % is determined with cw NMR. The properties of the observed ammonia proton signals are described and spin thermodynamics in high elds is presented. Also the second moment of the NMR line is estimated.

Spectroscopic study on variations in illite surface properties after acid-base titration.

Science.gov (United States)

Liu, Wen-xin; Coveney, R M; Tang, Hong-xiao

2003-07-01

FT-IR, Raman microscopy, XRD, 29Si and 27Al MAS NMR, were used to investigate changes in surface properties of a natural illite sample after acid-base potentiometric titration. The characteristic XRD lines indicated the presence of surface Al-Si complexes, preferable to Al(OH)3 precipitates. In the microscopic Raman spectra, the vibration peaks of Si-O and Al-O bonds diminished as a result of treatment with acid, then increased after hydroxide back titration. The varied ratio of signal intensity between (IV)Al and (VI)Al species in 27Al MAS NMR spectra, together with the stable BET surface area after acidimetric titration, suggested that edge faces and basal planes in the layer structure of illite participated in dissolution of structural components. The combined spectroscopic evidence demonstrated that the reactions between illite surfaces and acid-leaching silicic acid and aluminum ions should be considered in the model description of surface acid-base properties of the aqueous illite.

Fluid-Rock Characterization and Interactions in NMR Well Logging

Energy Technology Data Exchange (ETDEWEB)

Hirasaki, George J.; Mohanty, Kishore K.

2003-02-10

The objective of this project was to characterize the fluid properties and fluid-rock interactions which are needed for formation evaluation by NMR well logging. NMR well logging is finding wide use in formation evaluation. The formation parameters commonly estimated were porosity, permeability, and capillary bound water. Special cases include estimation of oil viscosity, residual oil saturation, location of oil/water contact, and interpretation on whether the hydrocarbon is oil or gas.

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

Science.gov (United States)

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

2017-07-01

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

Chirp echo Fourier transform EPR-detected NMR.

Science.gov (United States)

Wili, Nino; Jeschke, Gunnar

2018-04-01

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

Chirp echo Fourier transform EPR-detected NMR

Science.gov (United States)

Wili, Nino; Jeschke, Gunnar

2018-04-01

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

Carbon-13 NMR characterization of actinyl(VI) carbonate complexes in aqueous solution

International Nuclear Information System (INIS)

Clark, D.L.; Hobart, D.E.; Palmer, P.D.; Sullivan, J.C.; Stout, B.E.

1992-01-01

The uranyl(VI) carbonate system has been re-examined using 13 C NMR of 99.9% 13 C-enriched U VI O 2 ( 13 CO 3 ) 3 4- in millimolar concentrations. By careful control of carbonate ion concentration, we have confirmed the existence of the trimer, and observed dynamic equilibrium between the monomer and the timer. In addition, the ligand exchange reaction between free and coordinated carbonate on Pu VI O 2 ( 13 CO 3 ) 3 4- and Am VI O 2 ( 13 CO 3 ) 3 4- systems has been examined by variable temperature 13 C NMR line-broadening techniques 13 C NMR line-broadening techniques. A modified Carr-Purcell-Meiboom-Gill NMR pulse sequence was written to allow for experimental determination of ligand exchange parameters for paramagnetic actinide complexes. Preliminary Eyring analysis has provided activation parameters of ΔG double-dagger 295 = 56 kJ/M, ΔH double-dagger = 38 kJ/M, and ΔS double-dagger = -60 J/M-K for the plutonyl triscarbonate system, suggesting an associative transition state for the plutonyl (VI) carbonate complex self-exchange reaction. Experiments for determination of the activation parameters for the americium (VI) carbonate system are in progress

Identification of Radical Scavenging Compounds in Rhaponticum carthamoides by Means of LC-DAD-SPE-NMR

NARCIS (Netherlands)

Miliauskas, G.; Beek, van T.A.; Waard, de P.; Venskutonis, R.P.; Sudhölter, E.J.R.

2005-01-01

A hyphenated LC-DAD-SPE-NMR setup in combination with on-line radical scavenging detection has been applied for the identification of radical scavenging compounds in extracts of Rhaponticum carthamoides. After NMR measurements, the pure compounds were infused into a mass spectrometer. The technique

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

NARCIS (Netherlands)

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

1993-01-01

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

{sup 103}Rh-NMR studies in the superconductor Rh{sub 17}S{sub 15}

Energy Technology Data Exchange (ETDEWEB)

Koyama, T; Kanda, K; Ueda, K; Mito, T; Kohara, T [Graduate School of Material Science, University of Hyogo, Kamigori, Hyogo 678-1297 (Japan); Nakamura, H, E-mail: t-koyama@sci.u-hyogo.ac.j [Department of Materials Science and Engineering, Kyoto University, Kyoto 606-8501 (Japan)

2010-01-15

{sup 103}Rh nuclear magnetic resonance (NMR) measurements have been performed in the superconductor Rh{sub 17}S{sub 15} with the transition temperature T{sub C}=5.4 K. The observed {sup 103}Rh-NMR spectrum shows an asymmetric shape with several peaks, reflecting the local symmetry around each Rh site. We have identified the observed NMR lines corresponding to four different Rh sites and obtained the temperature (T) dependence of the Knight shift of 24m site. The isotropic part of the Knight shift K{sub iso} decreases with decreasing T, indicating the existence of the electron correlation in Rh{sub 17}S{sub 15}. In the superconducting state, the resonance lines shift to higher frequencies owing to a decrease of the spin part of the Knight shift with negative hyperfine coupling.

NMR experiments on ion permeation in irradiated model membranes

International Nuclear Information System (INIS)

Sprinz, H.; Winkler, E.; Schaefer, H.

1981-01-01

In aqueous solutions of egg-lecithin vesicles treated with ultrasonics the 1 H NMR parameters line width, area, and chemical shift of the signal of the (CH 3 ) 3 N + group were determined as a function of the gamma dose (0 ... 12 kGy). Using europium and the line shape analysis, it has been possible to calculate these parameters for the inside as well as for the outside lipid layer. Increasing 60 Co radiation dose leads to linear increases of the line widths, which are significantly more rapid for the outer than for the inner layer. From that it can be concluded that the outside lipid layer has been more damaged by irradiation. The asymmetry may be the consequence of a radiation effect induced by the radicals of water radiolysis. From the temporal changes of the NMR parameters information can be obtained about the radiation effect on transport processes in the vesicles. Beginning at a threshold (approx. 5 kGy) the permeation of Eu +++ ions to the (CH 3 ) 3 N + head groups, previously not accessible, increases significantly. (author)

NMR study of hyper-polarized 129Xe and applications to liquid-phase NMR experiments

International Nuclear Information System (INIS)

Marion, D.

2008-07-01

In liquid samples where both nuclear polarization and spin density are strong, the magnetization dynamics, which can be analysed by NMR (nuclear magnetic resonance) methods, is deeply influenced by the internal couplings induced by local dipolar fields. The present thesis describes some of the many consequences associated to the presence in the sample of concentrated xenon hyper-polarized by an optical pumping process. First, we deal with the induced modifications in frequency and line width of the proton and xenon spectra, then we present the results of SPIDER, a coherent polarization transfer experiment designed to enhance the polarization of protons, in order to increase their NMR signal level. A third part is dedicated to the description of the apparition of repeated chaotic maser emissions by un unstable xenon magnetization coupled to the detection coil tuned at the xenon Larmor frequency (here 138 MHz). In the last part, we present a new method allowing a better tuning of any NMR detection probe and resulting in sensible gains in terms of sensitivity and signal shaping. Finally, we conclude with a partial questioning of the classical relaxation theory in the specific field of highly polarized and concentrated spin systems in a liquid phase. (author)

NMRbox: A Resource for Biomolecular NMR Computation.

Science.gov (United States)

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

2017-04-25

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

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

DEFF Research Database (Denmark)

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

2005-01-01

High-resolution 2H MAS NMR spectra can be obtained for nanocrystalline particles of goethite (alpha-FeOOH, particle size approximately 4-10 nm) at room temperature, facilitating NMR studies of sorption under environmentally relevant conditions. Li sorption was investigated as a function of pH, th...... on the goethite surface. Even larger Li hyperfine shifts (289 ppm) were observed for Li+-exchanged goethite, which contains lithium ions in the tunnels of the goethite structure, confirming the Li assignment of the 145 ppm Li resonance to the surface sites. Udgivelsesdato: 2005-Oct-6...

Dynamic NMR Study of Model CMP Slurry Containing Silica Particles as Abrasives

Science.gov (United States)

Odeh, F.; Al-Bawab, A.; Li, Y.

2018-02-01

Chemical mechanical planarization (CMP) should provide a good surface planarity with minimal surface defectivity. Since CMP slurries are multi-component systems, it is very important to understand the various processes and interactions taking place in such slurries. Several techniques have been employed for such task, however, most of them lack the molecular recognition to investigate molecular interactions without adding probes which in turn increase complexity and might alter the microenvironment of the slurry. Nuclear magnetic resonance (NMR) is a powerful technique that can be employed in such study. The longitudinal relaxation times (T1) of the different components of CMP slurries were measured using Spin Echo-NMR (SE-NMR) at a constant temperature. The fact that NMR is non-invasive and gives information on the molecular level gives more advantage to the technique. The model CMP slurry was prepared in D2O to enable monitoring of T1 for the various components' protons. SE-NMR provide a very powerful tool to study the various interactions and adsorption processes that take place in a model CMP silica based slurry which contains BTA and/or glycine and/or Cu+2 ions. It was found that BTA is very competitive towards complexation with Cu+2 ions and BTA-Cu complex adsorbs on silica surface.

Method of detecting cancer by measuring lipid-peroxidation using NMR

International Nuclear Information System (INIS)

Fossel, E.T.

1992-01-01

A technique and an apparatus are disclosed for the detection of cancer using nuclear magnetic resonance (NMR). Specifically, NMR parameters for protons of lipid methyl and/or methylene groups are determined and compared against a corresponding value for healthy patients. Suppression of the water proton signal is employed where necessary in order to obtain a suitable spectrum for the non-water component protons. In the event that a positive reading is obtained, the level of plasma triglycerides is determined and if it is high, the patient's bodily fluid sample is further subjected to second nuclear magnetic spectroscopy. The area or the intensity of the portion correlating to 2.0 and 2.8 ppm of the resonance line generated in the second NMR is measured which discriminates between true and false positive results from the proton NMR reading and determines the presence or absence of cancer in the patient

Fluid-Rock Characterization and Interactions in NMR Well Logging

Energy Technology Data Exchange (ETDEWEB)

George J. Hirasaki; Kishore K. Mohanty

2005-09-05

The objective of this report is to characterize the fluid properties and fluid-rock interactions that are needed for formation evaluation by NMR well logging. The advances made in the understanding of NMR fluid properties are summarized in a chapter written for an AAPG book on NMR well logging. This includes live oils, viscous oils, natural gas mixtures, and the relation between relaxation time and diffusivity. Oil based drilling fluids can have an adverse effect on NMR well logging if it alters the wettability of the formation. The effect of various surfactants on wettability and surface relaxivity are evaluated for silica sand. The relation between the relaxation time and diffusivity distinguishes the response of brine, oil, and gas in a NMR well log. A new NMR pulse sequence in the presence of a field gradient and a new inversion technique enables the T{sub 2} and diffusivity distributions to be displayed as a two-dimensional map. The objectives of pore morphology and rock characterization are to identify vug connectivity by using X-ray CT scan, and to improve NMR permeability correlation. Improved estimation of permeability from NMR response is possible by using estimated tortuosity as a parameter to interpolate between two existing permeability models.

Beam line 4: A dedicated surface science facility at Daresbury Laboratory

International Nuclear Information System (INIS)

Dhanak, V.R.; Robinson, A.W.; van der Laan, G.; Thornton, G.

1992-01-01

We describe a beam line currently under construction at the Daresbury Laboratory which forms part of a surface science research facility for the Interdisciplinary Research Centre in Surface Science. The beam line has three branches, two of which are described here. The first branch covers the high-energy range 640 eV≤hν≤10 keV, being equipped with a double-crystal monochromator and a novel multicoated premirror system. The second branch line is optimized for the energy range 15≤hν≤250 eV, using cylindrical focusing mirrors, a spherical diffraction grating and an ellipsoidal refocusing mirror to achieve high resolution with a small spot size

Time domain NMR evaluation of poly(vinyl alcohol) xerogels

Energy Technology Data Exchange (ETDEWEB)

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

2016-05-15

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

[Non-invasive analysis of proteins in living cells using NMR spectroscopy].

Science.gov (United States)

Tochio, Hidehito; Murayama, Shuhei; Inomata, Kohsuke; Morimoto, Daichi; Ohno, Ayako; Shirakawa, Masahiro

2015-01-01

NMR spectroscopy enables structural analyses of proteins and has been widely used in the structural biology field in recent decades. NMR spectroscopy can be applied to proteins inside living cells, allowing characterization of their structures and dynamics in intracellular environments. The simplest "in-cell NMR" approach employs bacterial cells; in this approach, live Escherichia coli cells overexpressing a specific protein are subjected to NMR. The cells are grown in an NMR active isotope-enriched medium to ensure that the overexpressed proteins are labeled with the stable isotopes. Thus the obtained NMR spectra, which are derived from labeled proteins, contain atomic-level information about the structure and dynamics of the proteins. Recent progress enables us to work with higher eukaryotic cells such as HeLa and HEK293 cells, for which a number of techniques have been developed to achieve isotope labeling of the specific target protein. In this review, we describe successful use of electroporation for in-cell NMR. In addition, (19)F-NMR to characterize protein-ligand interactions in cells is presented. Because (19)F nuclei rarely exist in natural cells, when (19)F-labeled proteins are delivered into cells and (19)F-NMR signals are observed, one can safely ascertain that these signals originate from the delivered proteins and not other molecules.

On the Analytical Superiority of 1D NMR for Fingerprinting the Higher Order Structure of Protein Therapeutics Compared to Multidimensional NMR Methods.

Science.gov (United States)

Poppe, Leszek; Jordan, John B; Rogers, Gary; Schnier, Paul D

2015-06-02

An important aspect in the analytical characterization of protein therapeutics is the comprehensive characterization of higher order structure (HOS). Nuclear magnetic resonance (NMR) is arguably the most sensitive method for fingerprinting HOS of a protein in solution. Traditionally, (1)H-(15)N or (1)H-(13)C correlation spectra are used as a "structural fingerprint" of HOS. Here, we demonstrate that protein fingerprint by line shape enhancement (PROFILE), a 1D (1)H NMR spectroscopy fingerprinting approach, is superior to traditional two-dimensional methods using monoclonal antibody samples and a heavily glycosylated protein therapeutic (Epoetin Alfa). PROFILE generates a high resolution structural fingerprint of a therapeutic protein in a fraction of the time required for a 2D NMR experiment. The cross-correlation analysis of PROFILE spectra allows one to distinguish contributions from HOS vs protein heterogeneity, which is difficult to accomplish by 2D NMR. We demonstrate that the major analytical limitation of two-dimensional methods is poor selectivity, which renders these approaches problematic for the purpose of fingerprinting large biological macromolecules.

The NMR probe of high-Tc materials and correlated electron systems. 2. ed.

International Nuclear Information System (INIS)

Walstedt, Russell E.

2018-01-01

This new edition updates readers in three areas of NMR studies, namely, recent developments in high-T c materials, heavy fermion systems and actinide oxides are presented. The NMR probe has yielded a vast array of data for solid state materials, corresponding to different compounds, ionic sites, and nuclear species, as well as to a wide variety of experimental conditions. The last two parts of the book are completely new in this edition, while the first part has seen major updates. This edition features the latest developments for high-T c materials, especially the advances in the area of pseudogap studies are reviewed. An in depth overview of heavy fermion systems is presented in the second part, notably Kondo lattices, quantum critical points and unconventional superconductivity are areas of intense research recently and are covered extensively. Finally, valuable information from NMR studies with actinide oxides will be provided. Ongoing analysis and discussion of NMR data have resulted in a wealth of important insights into the physics of these exotic systems. The aims of this monograph are manifold. First, it reviews NMR methodology as it has been applied to the different studies. This is addressed to NMR practitioners and to physics laypersons alike. Next, it presents a review of NMR measurements and the wide variety of phenomena which they represent. The third phase is to recount the theoretical model calculations and other proposals which have been put forward to account for these data.

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-08-15

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

Solid State NMR Characterization of Complex Metal Hydrides systems for Hydrogen Storage Applications

Directory of Open Access Journals (Sweden)

Son-Jong Hwang

2011-12-01

Full Text Available Solid state NMR is widely applied in studies of solid state chemistries for hydrogen storage reactions. Use of 11B MAS NMR in studies of metal borohydrides (BH4 is mainly focused, revisiting the issue of dodecaborane formation and observation of 11B{1H} Nuclear Overhauser Effect.

Applications of NMR in biological metabolic research

International Nuclear Information System (INIS)

Nie Jiarui; Li Xiuqin; He Chunjian

1989-01-01

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

Unevenness of Sliding Surface of Overhead Rigid Conductor Lines and Method for Reducing Unevenness

Science.gov (United States)

Aboshi, Mitsuo; Shimizu, Masashi

Rigid conductor lines are used in many subways, because the use of such conductor lines reduces the risk of accidents and because less space is required for their installation. However, as the unevenness of the sliding surface of the rigid conductor lines significantly influences the fluctuations in the contact force between pantographs and contact lines, it is necessary to decrease the unevenness at the construction as well as the maintenance stages. In order to investigate the installation accuracy of overhead rigid conductor lines, we have developed a device that accurately and continuously measures the unevenness of the sliding surface. By using this measuring device, we have confirmed that the unevenness of the sliding surface depends on various factors such as the sag between the support points, the deformation of the aluminum base or the conductive rail in the case of a long wavelength, the slight sagging unevenness between the bolts of the long ear, the undulating wear etc. This paper describes the actual unevenness conditions and the technical methods for decreasing the unevenness of the sliding surface of overhead rigid conductor lines.

Genome-wide methylation analysis identifies genes silenced in non-seminoma cell lines.

Science.gov (United States)

Noor, Dzul Azri Mohamed; Jeyapalan, Jennie N; Alhazmi, Safiah; Carr, Matthew; Squibb, Benjamin; Wallace, Claire; Tan, Christopher; Cusack, Martin; Hughes, Jaime; Reader, Tom; Shipley, Janet; Sheer, Denise; Scotting, Paul J

2016-01-01

Silencing of genes by DNA methylation is a common phenomenon in many types of cancer. However, the genome-wide effect of DNA methylation on gene expression has been analysed in relatively few cancers. Germ cell tumours (GCTs) are a complex group of malignancies. They are unique in developing from a pluripotent progenitor cell. Previous analyses have suggested that non-seminomas exhibit much higher levels of DNA methylation than seminomas. The genomic targets that are methylated, the extent to which this results in gene silencing and the identity of the silenced genes most likely to play a role in the tumours' biology have not yet been established. In this study, genome-wide methylation and expression analysis of GCT cell lines was combined with gene expression data from primary tumours to address this question. Genome methylation was analysed using the Illumina infinium HumanMethylome450 bead chip system and gene expression was analysed using Affymetrix GeneChip Human Genome U133 Plus 2.0 arrays. Regulation by methylation was confirmed by demethylation using 5-aza-2-deoxycytidine and reverse transcription-quantitative PCR. Large differences in the level of methylation of the CpG islands of individual genes between tumour cell lines correlated well with differential gene expression. Treatment of non-seminoma cells with 5-aza-2-deoxycytidine verified that methylation of all genes tested played a role in their silencing in yolk sac tumour cells and many of these genes were also differentially expressed in primary tumours. Genes silenced by methylation in the various GCT cell lines were identified. Several pluripotency-associated genes were identified as a major functional group of silenced genes.

Variable-temperature NMR and conformational analysis of Oenothein B

International Nuclear Information System (INIS)

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

2014-01-01

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

Variable-temperature NMR and conformational analysis of Oenothein B

Energy Technology Data Exchange (ETDEWEB)

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

2014-02-15

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

Canopy Dynamics in Nanoscale Ionic Materials Probed by NMR

Science.gov (United States)

Mirau, Peter

2013-03-01

Nanoscale ionic materials (NIMs) are hybrids prepared from ionically functionalized nanoparticles (NP) neutralized by oligomeric polymer counter-ions. NIMs are designed to behave as liquids under ambient conditions in the absence of solvent and have no volatile organic content, making them useful for a number of applications. We have used NMR relaxation and pulse-field gradient NMR to probe local and collective canopy dynamics in NIMs based on silica nanoparticles (NP), fullerols and proteins in order to understand the relationship between the core and canopy structure and the bulk properties. The NMR studies show that the canopy dynamics depend on the degree of neutralization, the canopy radius of gyration and molecular crowding at the ionically modified NP surface. The viscosity in NIMs can be directly controlled with the addition of ions that enhance the exchange rate for polymers at the NP surface. These results show that NIMs for many applications can be prepared by controlling the dynamics of the NP interface.

Paramagnetic NMR investigation of dendrimer-based host-guest interactions.

Directory of Open Access Journals (Sweden)

Fei Wang

Full Text Available In this study, the host-guest behavior of poly(amidoamine (PAMAM dendrimers bearing amine, hydroxyl, or carboxylate surface functionalities were investigated by paramagnetic NMR studies. 2,2,6,6-Tetramethylpiperidinyloxy (TEMPO derivatives were used as paramagnetic guest molecules. The results showed that TEMPO-COOH significantly broaden the ¹H NMR peaks of amine- and hydroxyl-terminated PAMAM dendrimers. In comparison, no paramagnetic relaxation enhancement (PRE was observed between TEMPO-NH₂, TEMPO-OH and the three types of PAMAM dendrimers. The PRE phenomenon observed is correlated with the encapsulation of TEMPO-COOH within dendrimer pockets. Protonation of the tertiary amine groups within PAMAM dendrimers plays an important role during this process. Interestingly, the absence of TEMPO-COOH encapsulation within carboxylate-terminated PAMAM dendrimer is observed due to the repulsion of TEMPO-COO- anion and anionic dendrimer surface. The combination of paramagnetic probes and ¹H NMR linewidth analysis can be used as a powerful tool in the analysis of dendrimer-based host-guest systems.

Can NMR solve some significant challenges in metabolomics?

Science.gov (United States)

Gowda, G.A. Nagana; Raftery, Daniel

2015-01-01

The field of metabolomics continues to witness rapid growth driven by fundamental studies, methods development, and applications in a number of disciplines that include biomedical science, plant and nutrition sciences, drug development, energy and environmental sciences, toxicology, etc. NMR spectroscopy is one of the two most widely used analytical platforms in the metabolomics field, along with mass spectrometry (MS). NMR's excellent reproducibility and quantitative accuracy, its ability to identify structures of unknown metabolites, its capacity to generate metabolite profiles using intact biospecimens with no need for separation, and its capabilities for tracing metabolic pathways using isotope labeled substrates offer unique strengths for metabolomics applications. However, NMR's limited sensitivity and resolution continue to pose a major challenge and have restricted both the number and the quantitative accuracy of metabolites analyzed by NMR. Further, the analysis of highly complex biological samples has increased the demand for new methods with improved detection, better unknown identification, and more accurate quantitation of larger numbers of metabolites. Recent efforts have contributed significant improvements in these areas, and have thereby enhanced the pool of routinely quantifiable metabolites. Additionally, efforts focused on combining NMR and MS promise opportunities to exploit the combined strength of the two analytical platforms for direct comparison of the metabolite data, unknown identification and reliable biomarker discovery that continue to challenge the metabolomics field. This article presents our perspectives on the emerging trends in NMR-based metabolomics and NMR's continuing role in the field with an emphasis on recent and ongoing research from our laboratory. PMID:26476597

Can NMR solve some significant challenges in metabolomics?

Science.gov (United States)

Nagana Gowda, G A; Raftery, Daniel

2015-11-01

The field of metabolomics continues to witness rapid growth driven by fundamental studies, methods development, and applications in a number of disciplines that include biomedical science, plant and nutrition sciences, drug development, energy and environmental sciences, toxicology, etc. NMR spectroscopy is one of the two most widely used analytical platforms in the metabolomics field, along with mass spectrometry (MS). NMR's excellent reproducibility and quantitative accuracy, its ability to identify structures of unknown metabolites, its capacity to generate metabolite profiles using intact bio-specimens with no need for separation, and its capabilities for tracing metabolic pathways using isotope labeled substrates offer unique strengths for metabolomics applications. However, NMR's limited sensitivity and resolution continue to pose a major challenge and have restricted both the number and the quantitative accuracy of metabolites analyzed by NMR. Further, the analysis of highly complex biological samples has increased the demand for new methods with improved detection, better unknown identification, and more accurate quantitation of larger numbers of metabolites. Recent efforts have contributed significant improvements in these areas, and have thereby enhanced the pool of routinely quantifiable metabolites. Additionally, efforts focused on combining NMR and MS promise opportunities to exploit the combined strength of the two analytical platforms for direct comparison of the metabolite data, unknown identification and reliable biomarker discovery that continue to challenge the metabolomics field. This article presents our perspectives on the emerging trends in NMR-based metabolomics and NMR's continuing role in the field with an emphasis on recent and ongoing research from our laboratory. Copyright © 2015 Elsevier Inc. All rights reserved.

Can NMR solve some significant challenges in metabolomics?

Science.gov (United States)

Nagana Gowda, G. A.; Raftery, Daniel

2015-11-01

The field of metabolomics continues to witness rapid growth driven by fundamental studies, methods development, and applications in a number of disciplines that include biomedical science, plant and nutrition sciences, drug development, energy and environmental sciences, toxicology, etc. NMR spectroscopy is one of the two most widely used analytical platforms in the metabolomics field, along with mass spectrometry (MS). NMR's excellent reproducibility and quantitative accuracy, its ability to identify structures of unknown metabolites, its capacity to generate metabolite profiles using intact bio-specimens with no need for separation, and its capabilities for tracing metabolic pathways using isotope labeled substrates offer unique strengths for metabolomics applications. However, NMR's limited sensitivity and resolution continue to pose a major challenge and have restricted both the number and the quantitative accuracy of metabolites analyzed by NMR. Further, the analysis of highly complex biological samples has increased the demand for new methods with improved detection, better unknown identification, and more accurate quantitation of larger numbers of metabolites. Recent efforts have contributed significant improvements in these areas, and have thereby enhanced the pool of routinely quantifiable metabolites. Additionally, efforts focused on combining NMR and MS promise opportunities to exploit the combined strength of the two analytical platforms for direct comparison of the metabolite data, unknown identification and reliable biomarker discovery that continue to challenge the metabolomics field. This article presents our perspectives on the emerging trends in NMR-based metabolomics and NMR's continuing role in the field with an emphasis on recent and ongoing research from our laboratory.

Singular surfaces in the open field line region of a diverted tokamak

International Nuclear Information System (INIS)

Reiman, A.

1995-05-01

The structure of the open field lines of a slightly nonaxisymmetric, poloidally diverted tokamak is explored by numerical integration of the field line equations for a simple model field. In practice, the nonaxisymmetry could be produced self-consistently by the nonlinear evolution of a free-boundary MHD mode, or it could be produced by field errors, or it could be imposed externally by design. In the presence of a nonaxisymmetric perturbation, the tokamak is shown to develop open field line regions of differing topology separated by singular surfaces. It is argued that the singular surfaces can be expected to play a role analogous to that of rational toroidal flux surfaces, in terms of constraining ideal MHD perturbations and thus constraining the free-energy that can be tapped by ideal MHD instabilities. The possibility of active control of free-boundary instabilities by means of currents driven on the open singular surfaces, which are directly accessible from the divertor plates, is discussed. Also discussed is the possibility of early detection of imminent disruptions through localized measurement of the singular surface currents

Lactation Defect in a Widely Used MMTV-Cre Transgenic Line of Mice

Science.gov (United States)

Yuan, Taichang; Wang, Yongping; Pao, Lily; Anderson, Steve M.; Gu, Haihua

2011-01-01

Background MMTV-Cre mouse lines have played important roles in our understanding about the functions of numerous genes in mouse mammary epithelial cells during mammary gland development and tumorigenesis. However, numerous studies have not included MMTV-Cre mice as controls, and many investigators have not indicated which of the different MMTV-Cre founder lines were used in their studies. Here, we describe a lactation defect that severely limits the use of one of the most commonly used MMTV-Cre founder lines. Methodology/Principal Findings To explore the role of protein tyrosine phosphatase Shp1 in mammary gland development, mice bearing the floxed Shp1 gene were crossed with MMTV-Cre mice and mammary gland development was examined by histological and biochemical techniques, while lactation competency was assessed by monitoring pup growth. Surprisingly, both the Shp1fl/+;MMTV-Cre and MMTV-Cre female mice displayed a severe lactation defect when compared to the Shp1 fl/+ control mice. Histological and biochemical analyses reveal that female mice expressing the MMTV-Cre transgene, either alone or in combination with floxed genes, exhibit defects in lobuloalveolar expansion, presence of large cytoplasmic lipid droplets in luminal alveolar epithelial cells postpartum, and precocious induction of involution. Using a PCR-based genotyping method, the three different founder lines can be distinguished, and we determined that the MMTV-Cre line A, the most widely used MMTV-Cre founder line, exhibits a profound lactation defect that limits its use in studies on mammary gland development. Conclusions/Significance The identification of a lactation defect in the MMTV-Cre line A mice indicates that investigators must use MMTV-Cre alone mice as control in studies that utilize Cre recombinase to excise genes of interest from mammary epithelial cells. Our results also suggest that previous results obtained in studies using the MMTV-Cre line A line should be re-evaluated if the

Singular surfaces in the open field line region of a diverted tokamak

International Nuclear Information System (INIS)

Reiman, A.

1996-01-01

The structure of the open field lines of a slightly nonaxisymmetric, poloidally diverted tokamak is explored by numerical integration of the field line equations for a simple model field. In practice, the nonaxisymmetry could be produced self-consistently by the nonlinear evolution of a free-boundary magnetohydrodynamic (MHD) mode, or it could be produced by field errors, or it could be imposed externally by design. In the presence of a nonaxisymmetric perturbation, the tokamak is shown to develop open field line regions of differing topology separated by singular surfaces. It is argued that the singular surfaces can be expected to play a role analogous to that of rational toroidal flux surfaces, in terms of constraining ideal MHD perturbations and thus constraining the free-energy that can be tapped by ideal MHD instabilities. The possibility of active control of free-boundary instabilities by means of currents driven on the open singular surfaces, which are directly accessible from the divertor plates, is discussed. copyright 1996 American Institute of Physics

Targeted Molecular Imaging of Cancer Cells Using MS2-Based ¹²⁹ Xe NMR

Energy Technology Data Exchange (ETDEWEB)

Jeong, Keunhong [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Netirojjanakul, Chawita [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Munch, Henrik K. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Sun, Jinny [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Finbloom, Joel A. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Wemmer, David E. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Physical Biosciences Division; Pines, Alexander [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division; Francis, Matthew B. [Univ. of California, Berkeley, CA (United States). Dept. of Chemistry; Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Materials Sciences Division

2016-07-25

Targeted, selective, and highly sensitive ¹²⁹Xe NMR nanoscale biosensors have been synthesized using a spherical MS2 viral capsid, Cryptophane A molecules, and DNA aptamers. The biosensors showed strong binding specificity toward targeted lymphoma cells (Ramos line). Hyperpolarized ¹²⁹Xe NMR signal contrast and hyper-CEST ¹²⁹Xe MRI image contrast indicated its promise as highly sensitive hyperpolarized ¹²⁹Xe NMR nanoscale biosensor for future applications in cancer detection in vivo.

NMR of geophysical drill cores with a mobile Halbach scanner

International Nuclear Information System (INIS)

Talnishnikh, E.

2007-01-01

This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

NMR of geophysical drill cores with a mobile Halbach scanner

Energy Technology Data Exchange (ETDEWEB)

Talnishnikh, E.

2007-08-21

This thesis is devoted to a mobile NMR with an improved Halbach scanner. This is a lightweight tube-shaped magnet with sensitive volume larger and a homogeneity of the magnetic field higher than the previous prototype version. The improved Halbach scanner is used for analysis of water-saturated drill cores and plugs with diameters up to 60 mm. To provide the analysis, the standard 1D technique with the CPMG sequence as well as 2D correlation experiments were successfully applied and adapted to study properties of fluid-saturated sediments. Afterwards the Halbach scanner was calibrated to fast non-destructive measurements of porosity, relaxation time distributions, and estimation of permeability. These properties can be calculated directly from the NMR data using the developed methodology. Any independent measurements of these properties with other methods are not needed. One of the main results of this work is the development of a new NMR on-line core scanner for measurements of porosity in long cylindrical and semi cylindrical drill cores. Also dedicated software was written to operate the NMR on-line core scanner. The physical background of this work is the study of the diffusion influence on transverse relaxation. The diffusion effect in the presence of internal gradients in porous media was probed by 1D and 2D experiments. The transverse relaxation time distributions obtained from 1D and from 2D experiments are comparable but different in fine details. Two new methodologies were developed based on the results of this study. First is the methodology quantifying the influence of diffusion in the internal gradients of water-saturated sediments on transverse relaxation from 2D correlation experiments. The second one is the correction of the permeability estimation from the NMR data taking in account the influence of the diffusion. Furthermore, PFG NMR technique was used to study restricted diffusion in the same kind of samples. Preliminary results are reported

Condensed Matter NMR under Extreme Conditions: Challenges and Opportunities

Science.gov (United States)

Reyes, Arneil

2006-11-01

Advances in resistive magnet and power supply technology have made available extremely high magnetic fields suitable for condensed matter broadline NMR experiments. This capability expands the available phase space for investigating a wide variety of materials using magnetic resonance; utilizing the strength of the field to expose or induce new physical phenomena resulting in better understanding of the physics. Continuous fields up to 45T in NHMFL Hybrid magnet have brought new challenges in designing NMR instrumentation. Field strengths and sample space limitations put constraints on RF pulse power, tuning range, bandwidth, and temperature control. The inclusion of other capabilities, including high pressure, optics, and sample rotation requires intricate probe design and construction, while extremely low milliKelvin temperatures are desired in order to explore energy scales where thermal fluctuations are suppressed. Optimization of these devices has been of paramount consideration in NHMFL Condensed Matter NMR user program. Science achieved at high fields, the new initiatives to develop resistively-detected NMR in 2D electron gas and similar systems, and the current new generation Series-Connected Hybrid magnets for NMR work will be discussed. The NHMFL is supported by the National Science Foundation and the State of Florida.

Evidence for an anisotropic contact shift. Proton NMR study of line shapes in uranocene and (C5H5)3UCl powders

International Nuclear Information System (INIS)

McGarvey, B.R.; Nagy, S.

1987-01-01

The proton NMR spectra of solid powders of uranocene and (C 5 H 5 ) 3 UCl were measured from 90 to 298 K. The line shapes of both systems became increasingly anisotropic as the temperature was lowered. The cyclooctatetraene rings in uranocene were found to be rotating at a frequency greater than 100 kHz down to 90 K. The (C 5 H 5 ) 3 UCl molecules were found to be reorienting rapidly above 220 K, but below 140 K the NMR spectra were characteristic of a rigid lattice with no rotation of the cyclopentadienyl rings. The spectra of both compounds could be simulated by assuming an axial paramagnetic shift tensor and an orientation-dependent line width. Comparison of the experimental shift tensor with that calculated for a point dipolar interaction revealed a large and very anisotropic paramagnetic shift for uranocene due to unpaired spin transferred into the ligand orbitals. The shift was large when the magnetic field was along the 8-fold symmetry axis of the molecule and nearly zero perpendicular to the axis. It appears conclusive that the contact shift in uranocene is not isotropic at all. A similar anisotropy in the contact shift associated with the cyclopentadienyl rings is evident also in the results for (C 5 H 5 )UCl. The average solid-state shift of uranocene agreed with the solution shift, within experimental error, but the solid state shift of (C 5 H 5 ) 3 UCl was 42 ppm greater than the solution shift at 298 K, indicating a difference in molecular geometry between the crystalline state and solution. 32 references, 8 figures, 3 tables

Fragment based drug discovery: practical implementation based on ¹⁹F NMR spectroscopy.

Science.gov (United States)

Jordan, John B; Poppe, Leszek; Xia, Xiaoyang; Cheng, Alan C; Sun, Yax; Michelsen, Klaus; Eastwood, Heather; Schnier, Paul D; Nixey, Thomas; Zhong, Wenge

2012-01-26

Fragment based drug discovery (FBDD) is a widely used tool for discovering novel therapeutics. NMR is a powerful means for implementing FBDD, and several approaches have been proposed utilizing (1)H-(15)N heteronuclear single quantum coherence (HSQC) as well as one-dimensional (1)H and (19)F NMR to screen compound mixtures against a target of interest. While proton-based NMR methods of fragment screening (FBS) have been well documented and are widely used, the use of (19)F detection in FBS has been only recently introduced (Vulpetti et al. J. Am. Chem. Soc.2009, 131 (36), 12949-12959) with the aim of targeting "fluorophilic" sites in proteins. Here, we demonstrate a more general use of (19)F NMR-based fragment screening in several areas: as a key tool for rapid and sensitive detection of fragment hits, as a method for the rapid development of structure-activity relationship (SAR) on the hit-to-lead path using in-house libraries and/or commercially available compounds, and as a quick and efficient means of assessing target druggability.

Study of β-NMR for Liquid Biological Samples

CERN Document Server

Beattie, Caitlin

2017-01-01

β-NMR is an exotic form of NMR spectroscopy that allows for the characterization of matter based on the anisotropic β-decay of radioactive probe nuclei. This has been shown to be an effective spectroscopic technique for many different compounds, but its use for liquid biological samples is relatively unexplored. The work at the VITO line of ISOLDE seeks to employ this technique to study such samples. Currently, preparations are being made for an experiment to characterize DNA G-quadruplexes and their interactions with stabilizing cations. More specifically, the work in which I engaged as a summer student focused on the experiment’s liquid handling system and the stability of the relevant biological samples under vacuum.

ASIC-based design of NMR system health monitor for mission/safety?critical applications

OpenAIRE

Balasubramanian, P.

2016-01-01

N-modular redundancy (NMR) is a generic fault tolerance scheme that is widely used in safety?critical circuit/system designs to guarantee the correct operation with enhanced reliability. In passive NMR, at least a majority (N?+?1)/2 out of N function modules is expected to operate correctly at any time, where N is odd. Apart from a conventional realization of the NMR system, it would be useful to provide a concurrent indication of the system?s health so that an appropriate remedial action may...

NMR studies of 55Mn in amorphous CexMn100-x alloys

International Nuclear Information System (INIS)

Niki, H.; Okamura, K.; Yogi, M.; Amakai, Y.; Takano, H.; Murayama, S.; Obi, Y.

2008-01-01

In order to investigate the heavy-fermion like behavior of amorphous alloy Ce x Mn 100-x , the NMR measurements of 55 Mn (I=5/2 ) in Ce 65 Mn 35 have been carried out from 4.2 to 270 K using powdered sample. A broadened NMR spectrum containing five NQR lines split due to NQR interaction is observed. Quadrupole coupling constant 3e 2 Qq/2I(2I-1)h is gradually changed from about 1.8 MHz at 4.2 K to about 1.6 MHz at 270 K. Temperature dependence of the line width is expressed in the Curie-Weiss law with θ p =-10.5K. The value of Knight shift would be almost constant from 4.2 to 270 K

Protein folding on the ribosome studied using NMR spectroscopy

Science.gov (United States)

Waudby, Christopher A.; Launay, Hélène; Cabrita, Lisa D.; Christodoulou, John

2013-01-01

NMR spectroscopy is a powerful tool for the investigation of protein folding and misfolding, providing a characterization of molecular structure, dynamics and exchange processes, across a very wide range of timescales and with near atomic resolution. In recent years NMR methods have also been developed to study protein folding as it might occur within the cell, in a de novo manner, by observing the folding of nascent polypeptides in the process of emerging from the ribosome during synthesis. Despite the 2.3 MDa molecular weight of the bacterial 70S ribosome, many nascent polypeptides, and some ribosomal proteins, have sufficient local flexibility that sharp resonances may be observed in solution-state NMR spectra. In providing information on dynamic regions of the structure, NMR spectroscopy is therefore highly complementary to alternative methods such as X-ray crystallography and cryo-electron microscopy, which have successfully characterized the rigid core of the ribosome particle. However, the low working concentrations and limited sample stability associated with ribosome–nascent chain complexes means that such studies still present significant technical challenges to the NMR spectroscopist. This review will discuss the progress that has been made in this area, surveying all NMR studies that have been published to date, and with a particular focus on strategies for improving experimental sensitivity. PMID:24083462

Surface impedance of superconductors in wide frequency ranges for wake field calculations

International Nuclear Information System (INIS)

Davidovskii, V.G.

2006-01-01

The problem of the surface impedance of superconductors in wide frequency ranges for calculations of wake fields, generated by bunches of charged particles moving axially inside a metallic vacuum chambers, is solved. The case of specular electron reflection at the superconductor surface is considered. The expression for the surface impedance of superconductors suitable for numerical computation is derived [ru

Earthquake free design of pipe lines

International Nuclear Information System (INIS)

Kurihara, Chizuko; Sakurai, Akio

1974-01-01

Long structures such as cooling sea water pipe lines of nuclear power plants have a wide range of extent along the ground surface, and are incurred by not only the inertia forces but also forces due to ground deformations or the seismic wave propagation during earthquakes. Since previous reports indicated the earthquake free design of underground pipe lines, it is discussed in this report on behaviors of pipe lines on the ground during earthquakes and is proposed the aseismic design of pipe lines considering the effects of both inertia forces and ground deformations. (author)

Trans and surface membrane bound zervamicin IIB: 13C-MAOSS-NMR at high spinning speed

International Nuclear Information System (INIS)

Raap, J.; Hollander, J.; Ovchinnikova, T. V.; Swischeva, N. V.; Skladnev, D.; Kiihne, S.

2006-01-01

Interactions between 15 N-labelled peptides or proteins and lipids can be investigated using membranes aligned on a thin polymer film, which is rolled into a cylinder and inserted into the MAS-NMR rotor. This can be spun at high speed, which is often useful at high field strengths. Unfortunately, substrate films like commercially available polycarbonate or PEEK produce severe overlap with peptide and protein signals in 13 C-MAOSS NMR spectra. We show that a simple house hold foil support allows clear observation of the carbonyl, aromatic and C α signals of peptides and proteins as well as the ester carbonyl and choline signals of phosphocholine lipids. The utility of the new substrate is validated in applications to the membrane active peptide zervamicin IIB. The stability and macroscopic ordering of thin PC10 bilayers was compared with that of thicker POPC bilayers, both supported on the household foil. Sidebands in the 31 P-spectra showed a high degree of alignment of both the supported POPC and PC10 lipid molecules. Compared with POPC, the PC10 lipids are slightly more disordered, most likely due to the increased mobilities of the shorter lipid molecules. This mobility prevents PC10 from forming stable vesicles for MAS studies. The 13 C-peptide peaks were selectively detected in a 13 C-detected 1 H-spin diffusion experiment. Qualitative analysis of build-up curves obtained for different mixing times allowed the transmembrane peptide in PC10 to be distinguished from the surface bound topology in POPC. The 13 C-MAOSS results thus independently confirms previous findings from 15 N spectroscopy [Bechinger, B., Skladnev, D.A., Ogrel, A., Li, X., Rogozhkina, E.V., Ovchinnikova, T.V., O'Neil, J.D.J. and Raap, J. (2001) Biochemistry, 40, 9428-9437]. In summary, application of house hold foil opens the possibility of measuring high resolution 13 C-NMR spectra of peptides and proteins in well ordered membranes, which are required to determine the secondary and

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

Energy Technology Data Exchange (ETDEWEB)

Garibay, J.A.V.

2004-07-01

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

Non-destructive characterization of materials by single-sided NMR

International Nuclear Information System (INIS)

Goga, Nicolae-Octavian

2007-01-01

The experiments conducted in this work demonstrate the efficiency and sensitivity of single-sided NMR for investigating macromolecular materials on large time and length scales. Elastomers can readily be characterized by unilateral NMR of protons in terms of a variety of parameters, which correlate with the overall molecular mobility. In this way information about the cross-link density, state of cure and strain, the effects of aging and product heterogeneity can obtained. For these purposes, the NMR-MOUSE was used to optimize product development and to monitor product and production quality on-line. The sensor is also suitable for nondestructive probing of the mechanical deformation in cross-linked elastomers. A special magnet design that fits a stress-strain device has been used for complementary investigation of a series of different rubber stripes during mechanical testing. The profile NMR-MOUSE was found to be a unique tool for the characterization of changes induced by the UV irradiation in natural rubber. The aging profiles were interpreted for the first time based on a novel model in which the radiation absorption coefficient depends on the depth in the sample. (orig.)

Non-destructive characterization of materials by single-sided NMR

Energy Technology Data Exchange (ETDEWEB)

Goga, Nicolae-Octavian

2007-08-20

The experiments conducted in this work demonstrate the efficiency and sensitivity of single-sided NMR for investigating macromolecular materials on large time and length scales. Elastomers can readily be characterized by unilateral NMR of protons in terms of a variety of parameters, which correlate with the overall molecular mobility. In this way information about the cross-link density, state of cure and strain, the effects of aging and product heterogeneity can obtained. For these purposes, the NMR-MOUSE was used to optimize product development and to monitor product and production quality on-line. The sensor is also suitable for nondestructive probing of the mechanical deformation in cross-linked elastomers. A special magnet design that fits a stress-strain device has been used for complementary investigation of a series of different rubber stripes during mechanical testing. The profile NMR-MOUSE was found to be a unique tool for the characterization of changes induced by the UV irradiation in natural rubber. The aging profiles were interpreted for the first time based on a novel model in which the radiation absorption coefficient depends on the depth in the sample. (orig.)

Automatic NMR field-frequency lock-pulsed phase locked loop approach.

Science.gov (United States)

Kan, S; Gonord, P; Fan, M; Sauzade, M; Courtieu, J

1978-06-01

A self-contained deuterium frequency-field lock scheme for a high-resolution NMR spectrometer is described. It is based on phase locked loop techniques in which the free induction decay signal behaves as a voltage-controlled oscillator. By pulsing the spins at an offset frequency of a few hundred hertz and using a digital phase-frequency discriminator this method not only eliminates the usual phase, rf power, offset adjustments needed in conventional lock systems but also possesses the automatic pull-in characteristics that dispense with the use of field sweeps to locate the NMR line prior to closure of the lock loop.

Solutions on a high-speed wide-angle zoom lens with aspheric surfaces

Science.gov (United States)

Yamanashi, Takanori

2012-10-01

Recent development in CMOS and digital camera technology has accelerated the business and market share of digital cinematography. In terms of optical design, this technology has increased the need to carefully consider pixel pitch and characteristics of the imager. When the field angle at the wide end, zoom ratio, and F-number are specified, choosing an appropriate zoom lens type is crucial. In addition, appropriate power distributions and lens configurations are required. At points near the wide end of a zoom lens, it is known that an aspheric surface is an effective means to correct off-axis aberrations. On the other hand, optical designers have to focus on manufacturability of aspheric surfaces and perform required analysis with respect to the surface shape. Centration errors aside, it is also important to know the sensitivity to aspheric shape errors and their effect on image quality. In this paper, wide angle cine zoom lens design examples are introduced and their main characteristics are described. Moreover, technical challenges are pointed out and solutions are proposed.

Lining cells on normal human vertebral bone surfaces

International Nuclear Information System (INIS)

Henning, C.B.; Lloyd, E.L.

1982-01-01

Thoracic vertebrae from two individuals with no bone disease were studied with the electron microscope to determine cell morphology in relation to bone mineral. The work was undertaken to determine if cell morphology or spatial relationships between the bone lining cells and bone mineral could account for the relative infrequency of bone tumors which arise at this site following radium intake, when compared with other sites, such as the head of the femur. Cells lining the vertebral mineral were found to be generally rounded in appearance with varied numbers of cytoplasmic granules, and they appeared to have a high density per unit of surface area. These features contrasted with the single layer of flattened cells characteristic of the bone lining cells of the femur. A tentative discussion of the reasons for the relative infrequency of tumors in the vertebrae following radium acquisition is presented

Comparing pharmacophore models derived from crystallography and NMR ensembles

Science.gov (United States)

Ghanakota, Phani; Carlson, Heather A.

2017-11-01

NMR and X-ray crystallography are the two most widely used methods for determining protein structures. Our previous study examining NMR versus X-Ray sources of protein conformations showed improved performance with NMR structures when used in our Multiple Protein Structures (MPS) method for receptor-based pharmacophores (Damm, Carlson, J Am Chem Soc 129:8225-8235, 2007). However, that work was based on a single test case, HIV-1 protease, because of the rich data available for that system. New data for more systems are available now, which calls for further examination of the effect of different sources of protein conformations. The MPS technique was applied to Growth factor receptor bound protein 2 (Grb2), Src SH2 homology domain (Src-SH2), FK506-binding protein 1A (FKBP12), and Peroxisome proliferator-activated receptor-γ (PPAR-γ). Pharmacophore models from both crystal and NMR ensembles were able to discriminate between high-affinity, low-affinity, and decoy molecules. As we found in our original study, NMR models showed optimal performance when all elements were used. The crystal models had more pharmacophore elements compared to their NMR counterparts. The crystal-based models exhibited optimum performance only when pharmacophore elements were dropped. This supports our assertion that the higher flexibility in NMR ensembles helps focus the models on the most essential interactions with the protein. Our studies suggest that the "extra" pharmacophore elements seen at the periphery in X-ray models arise as a result of decreased protein flexibility and make very little contribution to model performance.

Genome-wide comparative transcriptome analysis of CMS-D2 and its maintainer and restorer lines in upland cotton.

Science.gov (United States)

Wu, Jianyong; Zhang, Meng; Zhang, Bingbing; Zhang, Xuexian; Guo, Liping; Qi, Tingxiang; Wang, Hailin; Zhang, Jinfa; Xing, Chaozhu

2017-06-08

Cytoplasmic male sterility (CMS) conferred by the cytoplasm from Gossypium harknessii (D2) is an important system for hybrid seed production in Upland cotton (G. hirsutum). The male sterility of CMS-D2 (i.e., A line) can be restored to fertility by a restorer (i.e., R line) carrying the restorer gene Rf1 transferred from the D2 nuclear genome. However, the molecular mechanisms of CMS-D2 and its restoration are poorly understood. In this study, a genome-wide comparative transcriptome analysis was performed to identify differentially expressed genes (DEGs) in flower buds among the isogenic fertile R line and sterile A line derived from a backcross population (BC 8 F 1 ) and the recurrent parent, i.e., the maintainer (B line). A total of 1464 DEGs were identified among the three isogenic lines, and the Rf1-carrying Chr_D05 and its homeologous Chr_A05 had more DEGs than other chromosomes. The results of GO and KEGG enrichment analysis showed differences in circadian rhythm between the fertile and sterile lines. Eleven DEGs were selected for validation using qRT-PCR, confirming the accuracy of the RNA-seq results. Through genome-wide comparative transcriptome analysis, the differential expression profiles of CMS-D2 and its maintainer and restorer lines in Upland cotton were identified. Our results provide an important foundation for further studies into the molecular mechanisms of the interactions between the restorer gene Rf1 and the CMS-D2 cytoplasm.

Deciphering ligands' interaction with Cu and Cu2O nanocrystal surfaces by NMR solution tools.

Science.gov (United States)

Glaria, Arnaud; Cure, Jérémy; Piettre, Kilian; Coppel, Yannick; Turrin, Cédric-Olivier; Chaudret, Bruno; Fau, Pierre

2015-01-12

The hydrogenolysis of [Cu2{(iPrN)2(CCH3)}2] in the presence of hexadecylamine (HDA) or tetradecylphosphonic acid (TDPA) in toluene leads to 6-9 nm copper nanocrystals. Solution NMR spectroscopy has been used to describe the nanoparticle surface chemistry during the dynamic phenomenon of air oxidation. The ligands are organized as multilayered shells around the nanoparticles. The shell of ligands is controlled by both their intermolecular interactions and their bonding strength on the nanocrystals. Under ambient atmosphere, the oxidation rate of colloidal copper nanocrystals closely relies on the chemical nature of the employed ligands (base or acid). Primary amine molecules behave as soft ligands for Cu atoms, but are even more strongly coordinated on surface Cu(I) sites, thus allowing a very efficient corrosion protection of the copper core. On the contrary, the TDPA ligands lead to a rapid oxidation rate of Cu nanoparticles and eventually to the re-dissolution of Cu(II) species at the expense of the nanocrystals. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The NMR probe of high-T{sub c} materials and correlated electron systems. 2. ed.

Energy Technology Data Exchange (ETDEWEB)

Walstedt, Russell E. [Michigan Univ., Ann Arbor, MI (United States). Dept. of Physics

2018-03-01

This new edition updates readers in three areas of NMR studies, namely, recent developments in high-T{sub c} materials, heavy fermion systems and actinide oxides are presented. The NMR probe has yielded a vast array of data for solid state materials, corresponding to different compounds, ionic sites, and nuclear species, as well as to a wide variety of experimental conditions. The last two parts of the book are completely new in this edition, while the first part has seen major updates. This edition features the latest developments for high-T{sub c} materials, especially the advances in the area of pseudogap studies are reviewed. An in depth overview of heavy fermion systems is presented in the second part, notably Kondo lattices, quantum critical points and unconventional superconductivity are areas of intense research recently and are covered extensively. Finally, valuable information from NMR studies with actinide oxides will be provided. Ongoing analysis and discussion of NMR data have resulted in a wealth of important insights into the physics of these exotic systems. The aims of this monograph are manifold. First, it reviews NMR methodology as it has been applied to the different studies. This is addressed to NMR practitioners and to physics laypersons alike. Next, it presents a review of NMR measurements and the wide variety of phenomena which they represent. The third phase is to recount the theoretical model calculations and other proposals which have been put forward to account for these data.

NMR study of Gd2(Co1-xFex)14B compounds

International Nuclear Information System (INIS)

Hayashi, M.; Myojin, T.; Kasamatsu, Y.; Imaeda, Y.; Ushida, T.; Tsujimura, A.; Hihara, T.

1992-01-01

59 Co NMR measurements in Gd 2 (Co 1-x Fe x ) 14 B have been carried out at 4.2 K. The resonance line corresponding to each site of the Co atoms shifts gradually to a higher frequency region as the value of x increases, and when the value exceeds 0.3 the resonance line seems to be disturbed. (orig.)

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

Science.gov (United States)

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

2014-07-01

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

Development of new probes for NMR based analysis of biomolecules' cellular functions

International Nuclear Information System (INIS)

Fernandes, Laetitia

2015-01-01

Most NMR studies are carried out in vitro, but the structure and dynamics of some biomolecules inside cells differ from those in vitro. It thus becomes interesting to analyze biomolecules such as proteins in their natural environment: the cell. Recent progress of in cell NMR allowed to better understand the behaviour of proteins: their dynamics and their interactions with other biomolecules in the cell. But the low concentration of proteins leads to low signal intensity. Moreover, the viscosity of the environment induces faster transverse relaxation, resulting in line broadening for proteins signals. The use of the Long-Lived States and Coherencies (LLS and LLC, respectively) as well as dissolution Dynamic Nuclear Polarization (dissolution-DNP) can improve NMR observations in cells. LLS were used to understand and characterize the structure of the N-terminal domain of c-Src, which is intrinsically disordered. To follow the phosphorylation of proteins, a first preliminary study of a 21-aa peptides derived from IKBa electroporated into HepG2 cell lines was carried out. (author)

NMR of water in biological systems. I.-theoretical considerations

International Nuclear Information System (INIS)

Villa, M.; Borghi, L.; De Ambrosis, A.; Aldrovandi, S.

1983-01-01

A simple relationship has been thought to exist between the dynamics of water in heterogeneous (liquid-solid) systems and NMR response. This relationship is usually expressed by the Bloembergen-Purcell-Puond (BPP) equations for relaxation and the phase model. However, a requirement for the use of the BPP theory is that motions take place in an isotropic, infinite and three-dimensional space. It is shown that the mere presence of solid surfaces causes the appearance of solid-like features in the NMR response of the liquid even if its dynamics is directly affected by the surfaces. Some of these ''topological'' or ''indirect'' surface effects are of the same kind as the low-dimensionality effects. Their order of magnitude is estimated for simple geometries and by treating the liquid motion in a hydrodynamic approximation. Comparison with the experiment is carried on in a companion paper

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

International Nuclear Information System (INIS)

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

1991-01-01

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

NMR measurements in milled RE-TM2 compounds (RE=Gd and TM=Co, Fe)

International Nuclear Information System (INIS)

Tribuzy, C.V.; Guimaraes, A.P.; Biondo, A.; Larica, C.; Alves, K.M.B.

1996-09-01

Milled samples of the Laves phase intermetallic compounds Gd Fe 2 and Gd CO 2 were measured by NMR at 4.2 K. The milling was made from the crystalline intermetallic compounds, inside a cylindrical tool made of hard steel, under argon atmosphere, for several different time intervals. The initial compounds were produced from high purity elements in an arc furnace, under inert atmosphere. Their X-ray diffraction patterns agreed with those of the literature. The milling of Gd Fe 2 and of Gd CO 2 , induces amorphization. Above 1 hour the milling of Gd Fe 2 leads to segregation of α-Fe and formation of a Gd-Fe phase. These results are shown in the X-ray analysis. The spin-echo pulse NMR technique was utilized to study some structural and magnetic as a function of milling time. The measurements were made in a broad band pulse NMR spectrometer. The NMR spectra of the 155 Gd 157 Gd isotopes in Gd Fe 2 show a broadening and displacement of the NMR lines, reflecting the introduction of defects, some kind of disorder and also the formation of a new Gd-rich phase after 1 hour. This result is in agreement with the X-ray spectra. In both systems, the spectra of the amorphous samples show broader lines, and the measured hyperfine fields do not change much with milling. (author). 9 refs., 4 figs

Getting Your Peaks in Line: A Review of Alignment Methods for NMR Spectral Data

Directory of Open Access Journals (Sweden)

Trung Nghia Vu

2013-04-01

Full Text Available One of the most significant challenges in the comparative analysis of Nuclear Magnetic Resonance (NMR metabolome profiles is the occurrence of shifts between peaks across different spectra, for example caused by fluctuations in pH, temperature, instrument factors and ion content. Proper alignment of spectral peaks is therefore often a crucial preprocessing step prior to downstream quantitative analysis. Various alignment methods have been developed specifically for this purpose. Other methods were originally developed to align other data types (GC, LC, SELDI-MS, etc., but can also be applied to NMR data. This review discusses the available methods, as well as related problems such as reference determination or the evaluation of alignment quality. We present a generic alignment framework that allows for comparison and classification of different alignment approaches according to their algorithmic principles, and we discuss their performance.

Target immobilization as a strategy for NMR-based fragment screening: comparison of TINS, STD, and SPR for fragment hit identification.

Science.gov (United States)

Kobayashi, Masakazu; Retra, Kim; Figaroa, Francis; Hollander, Johan G; Ab, Eiso; Heetebrij, Robert J; Irth, Hubertus; Siegal, Gregg

2010-09-01

Fragment-based drug discovery (FBDD) has become a widely accepted tool that is complementary to high-throughput screening (HTS) in developing small-molecule inhibitors of pharmaceutical targets. Because a fragment campaign can only be as successful as the hit matter found, it is critical that the first stage of the process be optimized. Here the authors compare the 3 most commonly used methods for hit discovery in FBDD: high concentration screening (HCS), solution ligand-observed nuclear magnetic resonance (NMR), and surface plasmon resonance (SPR). They selected the commonly used saturation transfer difference (STD) NMR spectroscopy and the proprietary target immobilized NMR screening (TINS) as representative of the array of possible NMR methods. Using a target typical of FBDD campaigns, the authors find that HCS and TINS are the most sensitive to weak interactions. They also find a good correlation between TINS and STD for tighter binding ligands, but the ability of STD to detect ligands with affinity weaker than 1 mM K(D) is limited. Similarly, they find that SPR detection is most suited to ligands that bind with K(D) better than 1 mM. However, the good correlation between SPR and potency in a bioassay makes this a good method for hit validation and characterization studies.

Two approaches to 3D reconstruction in NMR zeugmatography

International Nuclear Information System (INIS)

Marr, R.B.; Chen, C.N.; Lauterbur, P.C.

1980-01-01

In nuclear magnetic resonance (NMR) zeugmatography, the primary data pertain to integrals of the unknown nuclear spin density f(x,y,z) over planes instead of lines in R 3 . Two natural approaches to reconstructing f from such data are: (1) By numerical implementation of the inverse Radon transform in three dimensions (the direct approach), and (2) by application, in two successive stages, of existing well-known algorithms for inverting the two-dimensional Radon transform (the two-stage approach). These two approaches are discussed and compared, both from a theoretical standpoint and through computer results obtained with real NMR data. For the cases studied to date the two methods appear to produce qualitatively similar results

Structure and dynamics of alpha-tocopherol in model membranes and in solution: a broad-line and high-resolution NMR study

International Nuclear Information System (INIS)

Ekiel, I.H.; Hughes, L.; Burton, G.W.; Jovall, P.A.; Ingold, K.U.; Smith, I.C.

1988-01-01

Nuclear magnetic resonance has been applied to study the conformational dynamics of alpha-tocopherol (vitamin E) in solution and in model membranes. In nonviscous solution, 1 H nuclear magnetic resonance (NMR) showed that alpha-tocopherol is in rapid equilibrium between two or more puckered conformers of its heterocyclic ring. The most likely conformers to be so involved are the two half-chair forms. Deuterium NMR spectra of specifically deuteriated alpha-tocopherol in multilamellar dispersions of egg phosphatidylcholine, measured in the liquid-crystalline state, were characteristic of axially symmetric motional averaging. The orientation of the rotational axis within the molecular framework was determined. Studies on oriented multilamellar membranes revealed that this axis is perpendicular to the surface of the membrane. The profile of quadrupolar splittings along the hydrophobic tail does not have a plateau, in contrast to that of the fatty acyl chains of the membrane lipids. Longitudinal relaxation times (T1) were short. The presence of a minimum in their temperature dependence shows that molecular motion with an effective correlation time tau eff approximately equal to 3 X 10(-9)s is responsible for relaxation. However, the temperatures and absolute values of the minima depend on the position of the deuterium in the molecule, demonstrating that tau eff represents a complex blend of motions

Temperature dependence of broadline NMR spectra of water-soaked, epoxy-graphite composites

Science.gov (United States)

Lawing, David; Fornes, R. E.; Gilbert, R. D.; Memory, J. D.

1981-10-01

Water-soaked, epoxy resin-graphite fiber composites show a waterline in their broadline proton NMR spectrum which indicates a state of intermediate mobility between the solid and free water liquid states. The line is still present at -42 °C, but shows a reversible decrease in amplitude with decreasing temperature. The line is isotropic upon rotation of the fiber axis with respect to the external magnetic field.

NMR imaging

International Nuclear Information System (INIS)

Andrew, E.R.

1983-01-01

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

Straight-Line Target Tracking for Unmanned Surface Vehicles

Directory of Open Access Journals (Sweden)

Morten Breivik

2008-10-01

Full Text Available This paper considers the subject of straight-line target tracking for unmanned surface vehicles (USVs. Target-tracking represents motion control scenarios where no information about the target behavior is known in advance, i.e., the path that the target traverses is not defined apriori. Specifically, this work presents the design of a motion control system which enables an underactuated USV to track a target that moves in a straight line at high speed. The motion control system employs a guidance principle originally developed for interceptor missiles, as well as a novel velocity controller inspired by maneuverability and agility concepts found in fighter aircraft literature. The performance of the suggested design is illustrated through full-scale USV experiments in the Trondheimsfjord.

NMR detection and characterization of sialylated glycoproteins and cell surface polysaccharides

International Nuclear Information System (INIS)

Barb, Adam W.; Freedberg, Darón I.; Battistel, Marcos D.; Prestegard, James H.

2011-01-01

Few solution NMR pulse sequences exist that are explicitly designed to characterize carbohydrates (glycans). This is despite the essential role carbohydrate motifs play in cell–cell communication, microbial pathogenesis, autoimmune disease progression and cancer metastasis, and despite that fact that glycans, often shed to extra-cellular fluids, can be diagnostic of disease. Here we present a suite of two dimensional coherence experiments to measure three different correlations (H3–C2, H3–C1, and C1–C2) on sialic acids, a group of nine-carbon carbohydrates found on eukaryotic cell surfaces that often play a key role in disease processes. The chemical shifts of the H3, C2, and C1 nuclei of sialic acids are sensitive to carbohydrate linkage, linkage conformation, and ionization state of the C1 carboxylate. The experiments reported include rigorous filter elements to enable detection and characterization of isotopically labeled sialic acids with high sensitivity in living cells and crude isolates with minimal interference from unwanted signals arising from the ∼1% 13 C-natural abundance of cellular metabolites. Application is illustrated with detection of sialic acids on living cells, in unpurified mixtures, and at the terminus of the N-glycan on the 55 kDa immunoglobulin G Fc.

NMR-CT scanner

International Nuclear Information System (INIS)

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

1983-01-01

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

The NMR probe of high-Tc materials and correlated electron systems

CERN Document Server

Walstedt, Russell E

2018-01-01

This new edition updates readers in three areas of NMR studies, namely, recent developments in high-Tc materials, heavy fermion systems and actinide oxides are presented.  The NMR probe has yielded a vast array of data for solid state materials, corresponding to different compounds, ionic sites, and nuclear species, as well as to a wide variety of experimental conditions. The last two parts of the book are completely new in this edition, while the first part has seen major updates. This edition features the latest developments for high-Tc materials, especially the advances in the area of pseudogap studies are reviewed.  An in depth overview of heavy fermion systems is presented in the second part,  notably Kondo lattices, quantum critical points and unconventional superconductivity are areas of intense research recently and are covered extensively. Finally, valuable information from NMR studies with actinide oxides will be provided. Ongoing analysis and discussion of NMR data have resulted in a wealth o...

SPATIAL UNCERTAINTY IN LINE-SURFACE INTERSECTIONS WITH APPLICATIONS TO PHOTOGRAMMETRY

Directory of Open Access Journals (Sweden)

J. Marshall

2012-07-01

Full Text Available The fields of photogrammetry and computer vision routinely use line-surface intersections to determine the point where a line intersects with a surface. The object coordinates of the intersection point can be found using standard geometric and numeric algorithms, however expressing the spatial uncertainty at the intersection point may be challenging, especially when the surface morphology is complex. This paper describes an empirical method to characterize the unknown spatial uncertainty at the intersection point by propagating random errors in the stochastic model using repeated random sampling methods. These methods accommodate complex surface morphology and nonlinearities in the functional model, however the penalty is the resulting probability density function associated with the intersection point may be non-Gaussian in nature. A formal hypothesis test is presented to show that straightforward statistical inference tools are available whether the data is Gaussian or not. The hypothesis test determines whether the computed intersection point is consistent with an externally-derived known truth point. A numerical example demonstrates the approach in a photogrammetric setting with a single frame image and a gridded terrain elevation model. The results show that uncertainties produced by the proposed empirical method are intuitive and can be assessed with conventional methods found in textbook hypothesis testing.

NMR studies of the helical antiferromagnetic compound EuCo2P2

Science.gov (United States)

Higa, N.; Ding, Q.-P.; Kubota, F.; Uehara, H.; Yogi, M.; Furukawa, Y.; Sangeetha, N. S.; Johnston, D. C.; Nakamura, A.; Hedo, M.; Nakama, T.; Ōnuki, Y.

2018-05-01

In EuCo2P2, 4f electron spins of Eu2+ ions order antiferromagnetically below a Néel temperature TN = 66.5 K . The magnetic structure below TN was reported to be helical with the helix axis along the c-axis from the neutron diffraction study. We report the results of 153Eu, 59Co and 31P nuclear magnetic resonance (NMR) measurements on EuCo2P2 using a single crystal and a powdered sample. In the antiferromagnetic (AFM) state, we succeeded in observing 153Eu, 59Co and 31P NMR spectra in zero magnetic field. The sharp 153Eu zero field NMR (ZF NMR) lines indicate homogeneous Eu ordered moment. The 59Co and 31P ZF NMR spectra showed an asymmetric spectral shape, indicating a distribution of the internal magnetic induction at each nuclear position. The AFM propagation vector k characterizing the helical AFM state can be determined from the internal magnetic induction at Co site. We have determined the model-independent value of the AFM propagation vector k distributed from (0, 0, 0.86)2π/c to (0, 0, 0.73)2π/c, where c is the lattice parameter.

Numerical simulation of NQR/NMR: Applications in quantum computing.

Science.gov (United States)

Possa, Denimar; Gaudio, Anderson C; Freitas, Jair C C

2011-04-01

A numerical simulation program able to simulate nuclear quadrupole resonance (NQR) as well as nuclear magnetic resonance (NMR) experiments is presented, written using the Mathematica package, aiming especially applications in quantum computing. The program makes use of the interaction picture to compute the effect of the relevant nuclear spin interactions, without any assumption about the relative size of each interaction. This makes the program flexible and versatile, being useful in a wide range of experimental situations, going from NQR (at zero or under small applied magnetic field) to high-field NMR experiments. Some conditions specifically required for quantum computing applications are implemented in the program, such as the possibility of use of elliptically polarized radiofrequency and the inclusion of first- and second-order terms in the average Hamiltonian expansion. A number of examples dealing with simple NQR and quadrupole-perturbed NMR experiments are presented, along with the proposal of experiments to create quantum pseudopure states and logic gates using NQR. The program and the various application examples are freely available through the link http://www.profanderson.net/files/nmr_nqr.php. Copyright © 2011 Elsevier Inc. All rights reserved.

Determining the optimal size of small molecule mixtures for high throughput NMR screening

International Nuclear Information System (INIS)

Mercier, Kelly A.; Powers, Robert

2005-01-01

High-throughput screening (HTS) using NMR spectroscopy has become a common component of the drug discovery effort and is widely used throughout the pharmaceutical industry. NMR provides additional information about the nature of small molecule-protein interactions compared to traditional HTS methods. In order to achieve comparable efficiency, small molecules are often screened as mixtures in NMR-based assays. Nevertheless, an analysis of the efficiency of mixtures and a corresponding determination of the optimum mixture size (OMS) that minimizes the amount of material and instrumentation time required for an NMR screen has been lacking. A model for calculating OMS based on the application of the hypergeometric distribution function to determine the probability of a 'hit' for various mixture sizes and hit rates is presented. An alternative method for the deconvolution of large screening mixtures is also discussed. These methods have been applied in a high-throughput NMR screening assay using a small, directed library

NMR of lignins

Science.gov (United States)

John Ralph; Larry L. Landucci

2010-01-01

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

Off-line testing of multifunctional surfaces for metal forming applications

DEFF Research Database (Denmark)

Godi, A.; Grønbæk, J.; De Chiffre, L.

2015-01-01

In this paper, Bending-Under-Tension, an off-line test method simulating deep-drawing, is chosen for investigating the effectiveness of multifunctional (MUFU) surfaces in metal forming operations. Four different MUFU surfaces, characterized by a plateau bearing area and grooves for lubricant...... retention, are manufactured, together with two polished references. During the tests, surface texture is the only variable. The results show how MUFU surfaces perform better than the polished references, which produce severe galling, while MUFU surfaces with low bearing area display no clear evidence...... of galling. Metal-to-metal contact occurs anyway, but the strip material is pulverized and deposited onto the tool instead of cold-welding to it. The pockets create a discontinuity on the texture hindering pick-up propagation....

Successful Sampling Strategy Advances Laboratory Studies of NMR Logging in Unconsolidated Aquifers

Science.gov (United States)

Behroozmand, Ahmad A.; Knight, Rosemary; Müller-Petke, Mike; Auken, Esben; Barfod, Adrian A. S.; Ferré, Ty P. A.; Vilhelmsen, Troels N.; Johnson, Carole D.; Christiansen, Anders V.

2017-11-01

The nuclear magnetic resonance (NMR) technique has become popular in groundwater studies because it responds directly to the presence and mobility of water in a porous medium. There is a need to conduct laboratory experiments to aid in the development of NMR hydraulic conductivity models, as is typically done in the petroleum industry. However, the challenge has been obtaining high-quality laboratory samples from unconsolidated aquifers. At a study site in Denmark, we employed sonic drilling, which minimizes the disturbance of the surrounding material, and extracted twelve 7.6 cm diameter samples for laboratory measurements. We present a detailed comparison of the acquired laboratory and logging NMR data. The agreement observed between the laboratory and logging data suggests that the methodologies proposed in this study provide good conditions for studying NMR measurements of unconsolidated near-surface aquifers. Finally, we show how laboratory sample size and condition impact the NMR measurements.

In situ viscosity of oil sands using low field NMR

International Nuclear Information System (INIS)

Bryan, J.; Moon, D.; Kantzas, A.

2005-01-01

In heavy oil and bitumen reservoirs, oil viscosity is a vital piece of information that will have great bearing on the chosen EOR scheme and the recovery expected. Prediction of in situ viscosity with a logging tool would he very beneficial in reservoir characterization and exploitation design. Low field NMR is a technology that has shown great potential as a tool for characterizing hydrocarbon properties in heavy oil and bitumen reservoirs. An oil viscosity correlation has previously been developed that is capable of providing order of magnitude viscosity estimates for a wide range of oils taken from various fields in Alberta. This paper presents tuning procedures to improve the NMR predictions for different viscosity ranges, and extends the NMR viscosity model to in situ heavy oil in unconsolidated sands. The results of this work show that the NMR oil peak can be de-convoluted from the in situ signals of the oil and water, and the bulk viscosity correlation that was developed for bulk oils can he applied to predict the in situ oil viscosity. These results can be translated to an NMR logging tool algorithm, allowing for in situ measurements of oil viscosity at the proper reservoir conditions. (author)

The second round of Critical Assessment of Automated Structure Determination of Proteins by NMR: CASD-NMR-2013

Energy Technology Data Exchange (ETDEWEB)

Rosato, Antonio [University of Florence, Department of Chemistry and Magnetic Resonance Center (Italy); Vranken, Wim [Vrije Universiteit Brussel, Structural Biology Brussels (Belgium); Fogh, Rasmus H.; Ragan, Timothy J. [University of Leicester, Department of Biochemistry, School of Biological Sciences (United Kingdom); Tejero, Roberto [Universidad de Valencia, Departamento de Química Física (Spain); Pederson, Kari; Lee, Hsiau-Wei; Prestegard, James H. [University of Georgia, Complex Carbohydrate Research Center and Northeast Structural Genomics Consortium (United States); Yee, Adelinda; Wu, Bin; Lemak, Alexander; Houliston, Scott; Arrowsmith, Cheryl H. [University of Toronto, Department of Medical Biophysics, Cancer Genomics and Proteomics, Ontario Cancer Institute, Northeast Structural Genomics Consortium (Canada); Kennedy, Michael [Miami University, Department of Chemistry and Biochemistry, Northeast Structural Genomics Consortium (United States); Acton, Thomas B.; Xiao, Rong; Liu, Gaohua; Montelione, Gaetano T., E-mail: guy@cabm.rutgers.edu [The State University of New Jersey, Department of Molecular Biology and Biochemistry, Center for Advanced Biotechnology and Medicine, Northeast Structural Genomics Consortium, Rutgers (United States); Vuister, Geerten W., E-mail: gv29@le.ac.uk [University of Leicester, Department of Biochemistry, School of Biological Sciences (United Kingdom)

2015-08-15

The second round of the community-wide initiative Critical Assessment of automated Structure Determination of Proteins by NMR (CASD-NMR-2013) comprised ten blind target datasets, consisting of unprocessed spectral data, assigned chemical shift lists and unassigned NOESY peak and RDC lists, that were made available in both curated (i.e. manually refined) or un-curated (i.e. automatically generated) form. Ten structure calculation programs, using fully automated protocols only, generated a total of 164 three-dimensional structures (entries) for the ten targets, sometimes using both curated and un-curated lists to generate multiple entries for a single target. The accuracy of the entries could be established by comparing them to the corresponding manually solved structure of each target, which was not available at the time the data were provided. Across the entire data set, 71 % of all entries submitted achieved an accuracy relative to the reference NMR structure better than 1.5 Å. Methods based on NOESY peak lists achieved even better results with up to 100 % of the entries within the 1.5 Å threshold for some programs. However, some methods did not converge for some targets using un-curated NOESY peak lists. Over 90 % of the entries achieved an accuracy better than the more relaxed threshold of 2.5 Å that was used in the previous CASD-NMR-2010 round. Comparisons between entries generated with un-curated versus curated peaks show only marginal improvements for the latter in those cases where both calculations converged.

The second round of Critical Assessment of Automated Structure Determination of Proteins by NMR: CASD-NMR-2013

International Nuclear Information System (INIS)

Rosato, Antonio; Vranken, Wim; Fogh, Rasmus H.; Ragan, Timothy J.; Tejero, Roberto; Pederson, Kari; Lee, Hsiau-Wei; Prestegard, James H.; Yee, Adelinda; Wu, Bin; Lemak, Alexander; Houliston, Scott; Arrowsmith, Cheryl H.; Kennedy, Michael; Acton, Thomas B.; Xiao, Rong; Liu, Gaohua; Montelione, Gaetano T.; Vuister, Geerten W.

2015-01-01

The second round of the community-wide initiative Critical Assessment of automated Structure Determination of Proteins by NMR (CASD-NMR-2013) comprised ten blind target datasets, consisting of unprocessed spectral data, assigned chemical shift lists and unassigned NOESY peak and RDC lists, that were made available in both curated (i.e. manually refined) or un-curated (i.e. automatically generated) form. Ten structure calculation programs, using fully automated protocols only, generated a total of 164 three-dimensional structures (entries) for the ten targets, sometimes using both curated and un-curated lists to generate multiple entries for a single target. The accuracy of the entries could be established by comparing them to the corresponding manually solved structure of each target, which was not available at the time the data were provided. Across the entire data set, 71 % of all entries submitted achieved an accuracy relative to the reference NMR structure better than 1.5 Å. Methods based on NOESY peak lists achieved even better results with up to 100 % of the entries within the 1.5 Å threshold for some programs. However, some methods did not converge for some targets using un-curated NOESY peak lists. Over 90 % of the entries achieved an accuracy better than the more relaxed threshold of 2.5 Å that was used in the previous CASD-NMR-2010 round. Comparisons between entries generated with un-curated versus curated peaks show only marginal improvements for the latter in those cases where both calculations converged

Medical applications of NMR imaging and NMR spectroscopy with stable isotopes. Summary

International Nuclear Information System (INIS)

Matwiyoff, N.A.

1983-01-01

The current status of NMR imaging and NMR spectroscopy are summarized. For the most part examples from the March 1983 Puerto Rico symposium are used to illustrate the utility of NMR in medicine. 18 refs., 5 figs

Medical applications of NMR imaging and NMR spectroscopy with stable isotopes. Summary

Energy Technology Data Exchange (ETDEWEB)

Matwiyoff, N.A.

1983-01-01

The current status of NMR imaging and NMR spectroscopy are summarized. For the most part examples from the March 1983 Puerto Rico symposium are used to illustrate the utility of NMR in medicine. 18 refs., 5 figs.

LC-UV-solid-phase extraction-NMR-MS combined with a cryogenic flow probe and its application to the identification of compounds present in Greek oregano

NARCIS (Netherlands)

Exarchou, V.; Godejohann, M.; Beek, van T.A.; Gerothanassis, I.P.; Vervoort, J.J.M.

2003-01-01

Structure elucidation of natural products usually relies on a combination of NMR spectroscopy with mass spectrometry whereby NMR trails MS in terms of the minimum sample amount required. In the present study, the usefulness of on-line solid-phase extraction (SPE) in LC-NMR for peak storage after the

Assigning uncertainties in the inversion of NMR relaxation data.

Science.gov (United States)

Parker, Robert L; Song, Yi-Qaio

2005-06-01

Recovering the relaxation-time density function (or distribution) from NMR decay records requires inverting a Laplace transform based on noisy data, an ill-posed inverse problem. An important objective in the face of the consequent ambiguity in the solutions is to establish what reliable information is contained in the measurements. To this end we describe how upper and lower bounds on linear functionals of the density function, and ratios of linear functionals, can be calculated using optimization theory. Those bounded quantities cover most of those commonly used in the geophysical NMR, such as porosity, T(2) log-mean, and bound fluid volume fraction, and include averages over any finite interval of the density function itself. In the theory presented statistical considerations enter to account for the presence of significant noise in the signal, but not in a prior characterization of density models. Our characterization of the uncertainties is conservative and informative; it will have wide application in geophysical NMR and elsewhere.

Part I. Generation of tailored radio-frequency pulses for NMR. Part II. Deuterium NMR studies of oriented DNA, and its interaction with water

International Nuclear Information System (INIS)

Brandes, R.

1988-01-01

A novel method for generating tailored radio-frequency pulses for use in NMR is presented. For this purpose, an inexpensive device based on analog audio filters was built. As an application, the superior selectivity of this method is shown by comparing it with a soft pulse excitation. The theoretical response of the magnetization to these tailored rf pulses is also calculated. Deuterium NMR line shapes of 2 H-labeled purine bases in solid, uniaxially oriented Li- and Na-DNA have been obtained. The spectral densities of motion were determined for the Li-DNA samples to test a model for uncorrelated, restricted base motion. For the first time, a 2 H spectrum is reported for 2 H labeled DNA in the liquid crystalline state. A procedure is outlined to separate the base motion from the DNA axis motion. In addition to the studies of DNA itself, the interaction of water (D 2 O) with samples of uniaxially oriented Na- and Li-DNA have been studied by high resolution 2 H NMR

Genome-wide association study of a nicotine metabolism biomarker in African American smokers: impact of chromosome 19 genetic influences.

Science.gov (United States)

Chenoweth, Meghan J; Ware, Jennifer J; Zhu, Andy Z X; Cole, Christopher B; Cox, Lisa Sanderson; Nollen, Nikki; Ahluwalia, Jasjit S; Benowitz, Neal L; Schnoll, Robert A; Hawk, Larry W; Cinciripini, Paul M; George, Tony P; Lerman, Caryn; Knight, Joanne; Tyndale, Rachel F

2018-03-01

The activity of CYP2A6, the major nicotine-inactivating enzyme, is measurable in smokers using the nicotine metabolite ratio (NMR; 3'hydroxycotinine/cotinine). Due to its role in nicotine clearance, the NMR is associated with smoking behaviours and response to pharmacotherapies. The NMR is highly heritable (~80%), and on average lower in African Americans (AA) versus whites. We previously identified several reduce and loss-of-function CYP2A6 variants common in individuals of African descent. Our current aim was to identify novel genetic influences on the NMR in AA smokers using genome-wide approaches. Genome-wide association study (GWAS). Multiple sites within Canada and the United States. AA smokers from two clinical trials: Pharmacogenetics of Nicotine Addiction Treatment (PNAT)-2 (NCT01314001; n = 504) and Kick-it-at-Swope (KIS)-3 (NCT00666978; n = 450). Genome-wide SNP genotyping, the NMR (phenotype) and population substructure and NMR covariates. Meta-analysis revealed three independent chromosome 19 signals (rs12459249, rs111645190 and rs185430475) associated with the NMR. The top overall hit, rs12459249 (P = 1.47e-39; beta = 0.59 per C (versus T) allele, SE = 0.045), located ~9.5 kb 3' of CYP2A6, remained genome-wide significant after controlling for the common (~10% in AA) non-functional CYP2A6*17 allele. In contrast, rs111645190 and rs185430475 were not genome-wide significant when controlling for CYP2A6*17. In total, 96 signals associated with the NMR were identified; many were not found in prior NMR GWASs in individuals of European descent. The top hits were also associated with the NMR in a third cohort of AA (KIS2; n = 480). None of the hits were in UGT or OCT2 genes. Three independent chromosome 19 signals account for ~20% of the variability in the nicotine metabolite ratio in African American smokers. The hits identified may contribute to inter-ethnic variability in nicotine metabolism, smoking behaviours and tobacco-related disease risk

Comparison of Transmission Line Methods for Surface Acoustic Wave Modeling

Science.gov (United States)

Wilson, William; Atkinson, Gary

2009-01-01

Surface Acoustic Wave (SAW) technology is low cost, rugged, lightweight, extremely low power and can be used to develop passive wireless sensors. For these reasons, NASA is investigating the use of SAW technology for Integrated Vehicle Health Monitoring (IVHM) of aerospace structures. To facilitate rapid prototyping of passive SAW sensors for aerospace applications, SAW models have been developed. This paper reports on the comparison of three methods of modeling SAWs. The three models are the Impulse Response Method (a first order model), and two second order matrix methods; the conventional matrix approach, and a modified matrix approach that is extended to include internal finger reflections. The second order models are based upon matrices that were originally developed for analyzing microwave circuits using transmission line theory. Results from the models are presented with measured data from devices. Keywords: Surface Acoustic Wave, SAW, transmission line models, Impulse Response Method.

Transcriptome-wide studies of prostate cancer cell lines in the context of medical radiation

International Nuclear Information System (INIS)

Hammer, Paul

2012-01-01

The use of radiotherapy in addition to chemotherapy and surgical removal is the most powerful instrument in the fight against malignant tumors in cancer medicine. After cardiovascular diseases, cancer is the second leading cause of death in the western world, in which prostate cancer is the most frequent male cancer. Despite continuous technological improvements in radiological instruments and prognosis, it may occur a recurrence up to many years after radiotherapy due to a high resistance capability of individual malignant cells of the locally occurring tumor. Although modern radiation biology has studied many aspects of the resistance mechanisms, questions are largely unanswered especially in regards to prognostic terms and time response of tumor cells to ionizing radiation. As cellular models four prostate cancer cell lines with different radiation sensitivities (PC3, DuCaP, DU-145, RWPE-1) were cultured and tested for their ability to survive after exposure to ionizing radiation by a trypane blue and MTT viability assay. The proliferative capacity of the four cell lines was determined using a colony formation assay. The PC3 cell line (radiation-resistant) and the DuCaP cell line (radiation-sensitive) showed the maximal differences in terms of radiation sensitivity. Based on these results the two cell lines were selected to allow identification of potential prognostic marker for predicting the effectiveness of radiation therapy via their transcriptome-wide gene expression. Furthermore, a time series experiment with the radiation-resistant PC3 cell line was performed. At 8 different time points, during the period from 00:00 - 42:53 (hh:mm) after exposure with 1 Gy, the mRNA was quantified by next generation sequencing to investigate the dynamic behavior of time-delayed gene expression and to discover resistance mechanisms. Of 10,966 expressed genes 730 were significant differentially expressed, determined by setting a fold change threshold in conjunction with a P

A robust algorithm for optimizing protein structures with NMR chemical shifts

Energy Technology Data Exchange (ETDEWEB)

Berjanskii, Mark; Arndt, David; Liang, Yongjie; Wishart, David S., E-mail: david.wishart@ualberta.ca [University of Alberta, Department of Computing Science (Canada)

2015-11-15

Over the past decade, a number of methods have been developed to determine the approximate structure of proteins using minimal NMR experimental information such as chemical shifts alone, sparse NOEs alone or a combination of comparative modeling data and chemical shifts. However, there have been relatively few methods that allow these approximate models to be substantively refined or improved using the available NMR chemical shift data. Here, we present a novel method, called Chemical Shift driven Genetic Algorithm for biased Molecular Dynamics (CS-GAMDy), for the robust optimization of protein structures using experimental NMR chemical shifts. The method incorporates knowledge-based scoring functions and structural information derived from NMR chemical shifts via a unique combination of multi-objective MD biasing, a genetic algorithm, and the widely used XPLOR molecular modelling language. Using this approach, we demonstrate that CS-GAMDy is able to refine and/or fold models that are as much as 10 Å (RMSD) away from the correct structure using only NMR chemical shift data. CS-GAMDy is also able to refine of a wide range of approximate or mildly erroneous protein structures to more closely match the known/correct structure and the known/correct chemical shifts. We believe CS-GAMDy will allow protein models generated by sparse restraint or chemical-shift-only methods to achieve sufficiently high quality to be considered fully refined and “PDB worthy”. The CS-GAMDy algorithm is explained in detail and its performance is compared over a range of refinement scenarios with several commonly used protein structure refinement protocols. The program has been designed to be easily installed and easily used and is available at http://www.gamdy.ca http://www.gamdy.ca.

31P NMR spectroscopy and HbO2 cryospectrophotometry in prediction of tumor radioresistance caused by hypoxia.

Science.gov (United States)

Rofstad, E K; DeMuth, P; Fenton, B M; Ceckler, T L; Sutherland, R M

1989-04-01

The aim of this study was to search for possible relationships between the fraction of radiobiologically hypoxic cells in tumors and their 31P NMR spectral parameters and intracapillary HbO2 saturations. Four different tumor lines, two murine sarcomas (KHT, RIF-1) and two human ovarian carcinoma xenografts (MLS, OWI), were used. When tumor volume increased from about 200 mm3 to about 2000 mm3, hypoxic fraction increased from 12 to 23% for the KHT line, from 0.9 to 1.7% for the RIF-1 line, and from 9 to 28% for the MLS line. The OWI line showed similar hypoxic fractions at 200 (17%) and 2000 mm3 (15%). Tumor bioenergetic status decreased, that is, the inorganic phosphate (Pi) resonance increased and the phosphocreatine (PCr) and nucleoside triphosphate beta (NTP beta) resonances decreased, with increasing tumor volume for the KHT, RIF-1, and MLS lines, whereas the OWI line did not show any changes in the 31P NMR spectral parameters during tumor growth. Similarly, tumor HbO2 saturation status, that is, the fraction of vessels with HbO2 saturation above 30%, decreased with increasing tumor volume for the KHT, RIF-1, and MLS lines, but remained unchanged during tumor growth for the OWI line. Although the data indicated a relationship between hypoxic fraction and tumor bioenergetic status as well as tumor HbO2 saturation status within a specific line during tumor growth, there was no correlation between hypoxic fraction and tumor bioenergetic status or tumor HbO2 saturation status across the four tumor lines. This may have occurred because cell survival time under hypoxic stress as well as fraction of non-clonogenic, but metabolically active hypoxic cells differed among the tumor lines. This indicates that 31P NMR spectroscopy and HbO2 cryospectrophotometry data have to be supplemented with other data to be useful in prediction of tumor radioresistance caused by hypoxia.

Conformational, vibrational, NMR and DFT studies of N-methylacetanilide.

Science.gov (United States)

Arjunan, V; Santhanam, R; Rani, T; Rosi, H; Mohan, S

2013-03-01

A detailed conformational, vibrational, NMR and DFT studies of N-methylacetanilide have been carried out. In DFT, B3LYP method have been used with 6-31G(**), 6-311++G(**) and cc-pVTZ basis sets. The vibrational frequencies were calculated resulting in IR and Raman frequencies together with intensities and Raman depolarisation ratios. The dipole moment derivatives were computed analytically. Owing to the complexity of the molecule, the potential energy distributions of the vibrational modes of the compound are also calculated. Isoelectronic molecular electrostatic potential surface (MEP) and electron density surface were examined. (1)H and (13)C NMR isotropic chemical shifts were calculated and the assignments made are compared with the experimental values. The energies of important MO's of the compound were also determined from TD-DFT method. Copyright © 2012 Elsevier B.V. All rights reserved.

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

NARCIS (Netherlands)

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

1990-01-01

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

Quantitative analysis of protein-ligand interactions by NMR.

Science.gov (United States)

Furukawa, Ayako; Konuma, Tsuyoshi; Yanaka, Saeko; Sugase, Kenji

2016-08-01

Protein-ligand interactions have been commonly studied through static structures of the protein-ligand complex. Recently, however, there has been increasing interest in investigating the dynamics of protein-ligand interactions both for fundamental understanding of the underlying mechanisms and for drug development. NMR is a versatile and powerful tool, especially because it provides site-specific quantitative information. NMR has widely been used to determine the dissociation constant (KD), in particular, for relatively weak interactions. The simplest NMR method is a chemical-shift titration experiment, in which the chemical-shift changes of a protein in response to ligand titration are measured. There are other quantitative NMR methods, but they mostly apply only to interactions in the fast-exchange regime. These methods derive the dissociation constant from population-averaged NMR quantities of the free and bound states of a protein or ligand. In contrast, the recent advent of new relaxation-based experiments, including R2 relaxation dispersion and ZZ-exchange, has enabled us to obtain kinetic information on protein-ligand interactions in the intermediate- and slow-exchange regimes. Based on R2 dispersion or ZZ-exchange, methods that can determine the association rate, kon, dissociation rate, koff, and KD have been developed. In these approaches, R2 dispersion or ZZ-exchange curves are measured for multiple samples with different protein and/or ligand concentration ratios, and the relaxation data are fitted to theoretical kinetic models. It is critical to choose an appropriate kinetic model, such as the two- or three-state exchange model, to derive the correct kinetic information. The R2 dispersion and ZZ-exchange methods are suitable for the analysis of protein-ligand interactions with a micromolar or sub-micromolar dissociation constant but not for very weak interactions, which are typical in very fast exchange. This contrasts with the NMR methods that are used

Perspectives of biomolecular NMR in drug discovery: the blessing and curse of versatility

International Nuclear Information System (INIS)

Jahnke, Wolfgang

2007-01-01

The versatility of NMR and its broad applicability to several stages in the drug discovery process is well known and generally considered one of the major strengths of NMR (Pellecchia et al., Nature Rev Drug Discov 1:211-219, 2002; Stockman and Dalvit, Prog Nucl Magn Reson Spectrosc 41:187-231, 2002; Lepre et al., Comb Chem High throughput screen 5:583-590, 2002; Wyss et al., Curr Opin Drug Discov Devel 5:630-647, 2002; Jahnke and Widmer, Cell Mol Life Sci 61:580-599, 2004; Huth et al., Methods Enzymol 394:549-571, 2005b; Klages et al., Mol Biosyst 2:318-332, 2006; Takeuchi and Wagner, Curr Opin Struct Biol 16:109-117, 2006; Zartler and Shapiro, Curr Pharm Des 12:3963-3972, 2006). Indeed, NMR is the only biophysical technique which can detect and quantify molecular interactions, and at the same time provide detailed structural information with atomic level resolution. NMR should therefore be ideally suited and widely requested as a tool for drug discovery research, and numerous examples of drug discovery projects which have substantially benefited from NMR contributions or were even driven by NMR have been described in the literature. However, not all pharmaceutical companies have rigorously implemented NMR as integral tool of their research processes. Some companies invest with limited resources, and others do not use biomolecular NMR at all. This discrepancy in assessing the value of a technology is striking, and calls for clarification-under which circumstances can NMR provide added value to the drug discovery process? What kind of contributions can NMR make, and how is it implemented and integrated for maximum impact? This perspectives article suggests key areas of impact for NMR, and a model of integrating NMR with other technologies to realize synergies and maximize their value for drug discovery

WaVPeak: Picking NMR peaks through wavelet-based smoothing and volume-based filtering

KAUST Repository

Liu, Zhi

2012-02-10

Motivation: Nuclear magnetic resonance (NMR) has been widely used as a powerful tool to determine the 3D structures of proteins in vivo. However, the post-spectra processing stage of NMR structure determination usually involves a tremendous amount of time and expert knowledge, which includes peak picking, chemical shift assignment and structure calculation steps. Detecting accurate peaks from the NMR spectra is a prerequisite for all following steps, and thus remains a key problem in automatic NMR structure determination. Results: We introduce WaVPeak, a fully automatic peak detection method. WaVPeak first smoothes the given NMR spectrum by wavelets. The peaks are then identified as the local maxima. The false positive peaks are filtered out efficiently by considering the volume of the peaks. WaVPeak has two major advantages over the state-of-the-art peak-picking methods. First, through wavelet-based smoothing, WaVPeak does not eliminate any data point in the spectra. Therefore, WaVPeak is able to detect weak peaks that are embedded in the noise level. NMR spectroscopists need the most help isolating these weak peaks. Second, WaVPeak estimates the volume of the peaks to filter the false positives. This is more reliable than intensity-based filters that are widely used in existing methods. We evaluate the performance of WaVPeak on the benchmark set proposed by PICKY (Alipanahi et al., 2009), one of the most accurate methods in the literature. The dataset comprises 32 2D and 3D spectra from eight different proteins. Experimental results demonstrate that WaVPeak achieves an average of 96%, 91%, 88%, 76% and 85% recall on 15N-HSQC, HNCO, HNCA, HNCACB and CBCA(CO)NH, respectively. When the same number of peaks are considered, WaVPeak significantly outperforms PICKY. The Author(s) 2012. Published by Oxford University Press.

NMR imaging and pharmaceutical sciences

International Nuclear Information System (INIS)

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

1986-01-01

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

Metabolomic profiling of the phytomedicinal constituents of Carica papaya L. leaves and seeds by 1H NMR spectroscopy and multivariate statistical analysis.

Science.gov (United States)

Gogna, Navdeep; Hamid, Neda; Dorai, Kavita

2015-11-10

Extracts from the Carica papaya L. plant are widely reported to contain metabolites with antibacterial, antioxidant and anticancer activity. This study aims to analyze the metabolic profiles of papaya leaves and seeds in order to gain insights into their phytomedicinal constituents. We performed metabolite fingerprinting using 1D and 2D 1H NMR experiments and used multivariate statistical analysis to identify those plant parts that contain the most concentrations of metabolites of phytomedicinal value. Secondary metabolites such as phenyl propanoids, including flavonoids, were found in greater concentrations in the leaves as compared to the seeds. UPLC-ESI-MS verified the presence of significant metabolites in the papaya extracts suggested by the NMR analysis. Interestingly, the concentration of eleven secondary metabolites namely caffeic, cinnamic, chlorogenic, quinic, coumaric, vanillic, and protocatechuic acids, naringenin, hesperidin, rutin, and kaempferol, were higher in young as compared to old papaya leaves. The results of the NMR analysis were corroborated by estimating the total phenolic and flavonoid content of the extracts. Estimation of antioxidant activity in leaves and seed extracts by DPPH and ABTS in-vitro assays and antioxidant capacity in C2C12 cell line also showed that papaya extracts exhibit high antioxidant activity. Copyright © 2015 Elsevier B.V. All rights reserved.

Structural Studies of Bcl-xL/ligand Complexes using {sup 19}F NMR

Energy Technology Data Exchange (ETDEWEB)

Yu Liping; Hajduk, Philip J.; Mack, Jamey; Olejniczak, Edward T. [GPRD, Abbott Laboratories, Pharmaceutical Discovery Division (United States)], E-mail: Edward.olejniczak@abbott.com

2006-04-15

Fluorine atoms are often incorporated into drug molecules as part of the lead optimization process in order to improve affinity or modify undesirable metabolic and pharmacokinetic profiles. From an NMR perspective, the abundance of fluorinated drug leads provides an exploitable niche for structural studies using {sup 19}F NMR in the drug discovery process. As {sup 19}F has no interfering background signal from biological sources, {sup 19}F NMR studies of fluorinated drugs bound to their protein receptors can yield easily interpretable and unambiguous structural constraints. {sup 19}F can also be selectively incorporated into proteins to obtain additional constraints for structural studies. Despite these advantages, {sup 19}F NMR has rarely been exploited for structural studies due to its broad lines in macromolecules and their ligand complexes, leading to weak signals in {sup 1}H/{sup 19}F heteronuclear NOE experiments. Here we demonstrate several different experimental strategies that use {sup 19}F NMR to obtain ligand-protein structural constraints for ligands bound to the anti-apoptotic protein Bcl-xL, a drug target for anti-cancer therapy. These examples indicate the applicability of these methods to typical structural problems encountered in the drug development process.

LipSpin: A New Bioinformatics Tool for Quantitative 1H NMR Lipid Profiling.

Science.gov (United States)

Barrilero, Rubén; Gil, Miriam; Amigó, Núria; Dias, Cintia B; Wood, Lisa G; Garg, Manohar L; Ribalta, Josep; Heras, Mercedes; Vinaixa, Maria; Correig, Xavier

2018-02-06

The structural similarity among lipid species and the low sensitivity and spectral resolution of nuclear magnetic resonance (NMR) have traditionally hampered the routine use of 1 H NMR lipid profiling of complex biological samples in metabolomics, which remains mostly manual and lacks freely available bioinformatics tools. However, 1 H NMR lipid profiling provides fast quantitative screening of major lipid classes (fatty acids, glycerolipids, phospholipids, and sterols) and some individual species and has been used in several clinical and nutritional studies, leading to improved risk prediction models. In this Article, we present LipSpin, a free and open-source bioinformatics tool for quantitative 1 H NMR lipid profiling. LipSpin implements a constrained line shape fitting algorithm based on voigt profiles and spectral templates from spectra of lipid standards, which automates the analysis of severely overlapped spectral regions and lipid signals with complex coupling patterns. LipSpin provides the most detailed quantification of fatty acid families and choline phospholipids in serum lipid samples by 1 H NMR to date. Moreover, analytical and clinical results using LipSpin quantifications conform with other techniques commonly used for lipid analysis.

Use of NMR in profiling of cocaine seizures

DEFF Research Database (Denmark)

Pagano, Bruno; Lauri, Ilaria; De Tito, Stefano

2013-01-01

Cocaine is the most widely used illicit drug, and its origin is always the focus of intense investigation aimed at identifying the trafficking routes. Since NMR represents a unique methodology for performing chemical identification and quantification, here it is proposed a strategy based on (1)H...... adding significant information in the process toward identification of the trafficking routes for this drug....

Measurement and Quantification of Heterogeneity, Flow, and Mass Transfer in Porous Media Using NMR Low-Field Techiques

Science.gov (United States)

Paciok, E.; Olaru, A. M.; Haber, A.; van Landeghem, M.; Haber-Pohlmeier, S.; Sucre, O. E.; Perlo, J.; Casanova, F.; Blümich, B.; RWTH Aachen Mobile Low-Field NMR

2011-12-01

Nuclear magnetic resonance (NMR) is renowned for its unique potential to both reveal and correlate spectroscopic, relaxometric, spatial and dynamic properties in a large variety of organic and inorganic systems. NMR has no restrictions regarding sample opacity and is an entirely non-invasive method, which makes it the ideal tool for the investigation of porous media. However, for years NMR research of soils was limited by the use of high-field NMR devices, which necessitated elaborate NMR experiments and were not applicable to bulky samples or on-site field measurements. The evolution of low-field NMR devices during the past 20 years has brought forth portable, small-scale NMR systems with open and closed magnet arrangements specialized to specific NMR applications. In combination with recent advances in 2D-NMR Laplace methodology [1], low-field NMR has opened up the possibility to study real-life microporous systems ranging from granular media to natural soils and oil well boreholes. Thus, information becomes available, which before has not been accessible with high-field NMR. In this work, we present our recent progress in mobile low-field NMR probe design for field measurements of natural soils: a slim-line logging tool, which can be rammed into the soil of interest on-site. The performance of the device is demonstrated in measurements of moisture profiles of model soils [2] and field measurements of relaxometric properties and moisture profiles of natural soils [3]. Moreover, an improved concept of the slim-line logging tool is shown, with a higher excitation volume and a better signal-to-noise due to an improved coil design. Furthermore, we present our recent results in 2D exchange relaxometry and simulation. These include relaxation-relaxation experiments on natural soils with varying degree of moisture saturation, where we could draw a connection between the relaxometric properties of the soil to its pore size-related diffusivity and to its clay content

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

International Nuclear Information System (INIS)

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

2005-01-01

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

InP/ZnS nanocrystals: coupling NMR and XPS for fine surface and interface description.

Science.gov (United States)

Virieux, Héloïse; Le Troedec, Marianne; Cros-Gagneux, Arnaud; Ojo, Wilfried-Solo; Delpech, Fabien; Nayral, Céline; Martinez, Hervé; Chaudret, Bruno

2012-12-05

Advanced (1)H, (13)C, and (31)P solution- and solid-state NMR studies combined with XPS were used to probe, at the molecular scale, the composition (of the core, the shell, and the interface) and the surface chemistry of InP/ZnS core/shell quantum dots prepared via a non-coordinating solvent strategy. The interface between the mismatched InP and ZnS phases is composed of an amorphous mixed oxide phase incorporating InPO(x) (with x = 3 and predominantly 4), In(2)O(3), and InO(y)(OH)(3-2y) (y = 0, 1). Thanks to the analysis of the underlying reaction mechanisms, we demonstrate that the oxidation of the upper part of the InP core is the consequence of oxidative conditions brought by decarboxylative coupling reactions (ketonization). These reactions occur during both the core preparation and the coating process, but according to different mechanisms.

THE METHOD OF ROLL SURFACE QUALITY MEASUREMENT FOR CONTINUOUS HOT DIP ZINC COATED STEEL SHEET PRODUCTION LINE

Directory of Open Access Journals (Sweden)

Ki Yong Choi

2015-01-01

Full Text Available The present paper describes a developed analyzing system of roll surface during the process of continuous hot dip zinc coated steel sheet production line, in particular, adhering problem by transferred inclusions from roll to steel sheet surface during annealing process so called the pickup. The simulated test machine for coated roll surface in processing line has been designed and performed. The system makes it possible to analyze roll surface condition according to pickup phenomena from various roll coatings concerning operating conditions of hearth rolls in annealing furnace. The algorithm of fast pickup detection on surface is developed on the base of processing of several optical images of surface. The parameters for quality estimation of surface with pickups were developed. The optical system for images registration and image processing electronics may be used in real time and embed in processing line.

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-09-01

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

Theory of NMR probe design

International Nuclear Information System (INIS)

Schnall, M.D.

1988-01-01

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

NMR in clinical practice

International Nuclear Information System (INIS)

Smith, F.W.

1987-01-01

The development of NMR for clinical use has been complicated by a number of controversies, the largest of these being the question of what is the optimum field strength for proton imaging. Many workers believe that diagnostically useful images can only be produced at high field strength (i.e. 0.5 - 2.0 T), where in fact diagnostically useful images are made using field strengths of as low as 0.02 T. Because the method is more complex than X-ray CT, which relies on the measurement of only one parameter, tissue density, many new users have difficulty in selecting the correct imaging pulse sequence to provide the most useful image for diagnosis. NMR imaging pulse sequence may be selected to produce images of the proton density, T/sub 1/ or T/sub 2/ signals, or combinations of them. When this facility is used, images which are T/sub 1/ or T/sub 2/ weighted can be selected. Inversion-recovery sequences are more appropriate for imaging the abdomen where by selecting a short TR interval the signal from subcutaneous fat, which is the major cause of image artefact in abdominal imaging, is suppressed thereby improving image quality. The use of surface receiver coils, which are applied closely to the area of the body being examined is becoming more widespread and is of particular value when examining the orbits, facial structures, neck, breast, spine and limbs. The use of these coils together with a discussion of patient selection for NMR imaging, image interpretation and data storage follow

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

International Nuclear Information System (INIS)

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

1996-01-01

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

High resolution solid-state NMR spectroscopy of the Yersinia pestis outer membrane protein Ail in lipid membranes

International Nuclear Information System (INIS)

Yao, Yong; Dutta, Samit Kumar; Park, Sang Ho; Rai, Ratan; Fujimoto, L. Miya; Bobkov, Andrey A.; Opella, Stanley J.; Marassi, Francesca M.

2017-01-01

The outer membrane protein Ail (Adhesion invasion locus) is one of the most abundant proteins on the cell surface of Yersinia pestis during human infection. Its functions are expressed through interactions with a variety of human host proteins, and are essential for microbial virulence. Structures of Ail have been determined by X-ray diffraction and solution NMR spectroscopy, but those samples contained detergents that interfere with functionality, thus, precluding analysis of the structural basis for Ail’s biological activity. Here, we demonstrate that high-resolution solid-state NMR spectra can be obtained from samples of Ail in detergent-free phospholipid liposomes, prepared with a lipid to protein molar ratio of 100. The spectra, obtained with 13 C or 1 H detection, have very narrow line widths (0.40–0.60 ppm for 13 C, 0.11–0.15 ppm for 1 H, and 0.46–0.64 ppm for 15 N) that are consistent with a high level of sample homogeneity. The spectra enable resonance assignments to be obtained for N, CO, CA and CB atomic sites from 75 out of 156 residues in the sequence of Ail, including 80% of the transmembrane region. The 1 H-detected solid-state NMR 1 H/ 15 N correlation spectra obtained for Ail in liposomes compare very favorably with the solution NMR 1 H/ 15 N TROSY spectra obtained for Ail in nanodiscs prepared with a similar lipid to protein molar ratio. These results set the stage for studies of the molecular basis of the functional interactions of Ail with its protein partners from human host cells, as well as the development of drugs targeting Ail.

Using NMR decay-time measurements to monitor and characterize DNAPL and moisture in subsurface porous media

International Nuclear Information System (INIS)

Timothy A. White; Russel C. Hertzog; Christian Straley

2007-01-01

Knowing how environmental properties affect dense nonaqueous phase liquid (DNAPL) solvent flow in the subsurface is essential for developing models of flow and transport in the vadose zone necessary for designing remediation and long-term stewardship strategies. For example, one must know if solvents are flowing in water-wetted or solvent-wetted environments, the pore-size distribution of the region containing DNAPLs, and the impact of contaminated plumes and their transport mechanisms in porous media. Our research investigates the capability and limitations of low-field proton nuclear magnetic resonance (NMR) relaxation decay-rate measurements for determining environmental properties affecting DNAPL solvent flow in the subsurface. The measurements that can be performed with the laboratory low-field system can also be performed in situ in the field with the current generation of commercial borehole logging tools. The oil and gas industry uses NMR measurements in deep subsurface, consolidated formations to determine porosity and hydrocarbon content and to estimate formation permeability. These determinations rely on the ability of NMR to distinguish between water and hydrocarbons in the pore space and to obtain the distribution of pore sizes from relaxation decay-rate distributions. In this paper we will show how NMR measurement techniques can be used to characterize, monitor, and evaluate the dynamics of mixed-fluids (water-DNAPL) in unconsolidated near-surface porous environments and describe the use of proton NMR T2 (spin-spin relaxation time) measurements in unconsolidated sandy-soil samples to identify and characterize the presence of DNAPLs in these environments. The potential of NMR decay-rate distributions for characterizing DNAPL fluids in the subsurface and understanding their flow mechanisms has not previously been exploited; however, near-surface unsaturated vadose zone environments do provide unique challenges for using NMR measurements. These

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

Directory of Open Access Journals (Sweden)

Jude Abia

2015-03-01

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

Determination of Hydrogen and Carbon contents in crude oil and Petroleum fractions by NMR Spectroscopy

International Nuclear Information System (INIS)

Khadim, Mohammad A.; Wolny, R.A.; Al-Dhuwaihi, Abdullah S.; Al-Hajri, E.A.; Al-Ghamdi, M.A.

2003-01-01

Proton and carbon-13 NMR spectroscopic methods were developed for determining hydrogen and carbon contents in petroleum products. These methods are applicable to a wide of petroleum streams. A new reference standard, bis (trimethylsilyl) methane, BTMSM, is introduced fro both proton and carbon-13 NMR for the first time, which offers several advantages over those customarily employed. These methods are important for the calculation of the mass balance and hydrogen consumption in pilot plant studies. Unlike the ASTM D-5291 combustion method, the NMR methods also allow for the measurement of hydrogen and carbon content in low boiling fractions and those containing hydrogen as low as 1%. The NMR methods can also determine aromatic and aliphatic hydrogens carbons in a given sample without additional experimentation. The precision and accuracy of the newly developed NMR methods are compared with those of currently employed ASTM D-5291 combustion method. Using the proton NMR method, hydrogen content was determined in fifteen model compounds and sixty-eight petroleum fractions. The NMR and ASTM methods show an agreement within +5%for 48 out of a total number of 68 oil fractions. Using carbon-13 NMR, the carbon content was determined for four representative compounds and three fractions of crude oil. Both carbon-13 NMR and ASTM methods give comparable carbon content in model compounds and crude oil fractions. (author)

Classical and quantum molecular dynamics in NMR spectra

CERN Document Server

Szymański, Sławomir

2018-01-01

The book provides a detailed account of how condensed-phase molecular dynamics are reflected in the line shapes of NMR spectra. The theories establishing connections between random, time-dependent molecular processes and lineshape effects are exposed in depth. Special emphasis is placed on the theoretical aspects, involving in particular intermolecular processes in solution, and molecular symmetry issues. The Liouville super-operator formalism is briefly introduced and used wherever it is beneficial for the transparency of presentation. The proposed formal descriptions of the discussed problems are sufficiently detailed to be implemented on a computer. Practical applications of the theory in solid- and liquid-phase studies are illustrated with appropriate experimental examples, exposing the potential of the lineshape method in elucidating molecular dynamics NMR-observable molecular phenomena where quantization of the spatial nuclear degrees of freedom is crucial are addressed in the last part of the book. As ...

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

Science.gov (United States)

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

2015-08-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Supra-molecular structure of TGBC* phases studied by means of Deuterium NMR line-shape analysis

Czech Academy of Sciences Publication Activity Database

Domenici, V.; Veracini, C.A.; Hamplová, Věra; Kašpar, Miroslav

2008-01-01

Roč. 495, č. 11 (2008), s. 133-144 ISSN 1542-1406 Institutional research plan: CEZ:AV0Z10100520 Keywords : banana -shaped * deuterium NMR * magnetic field * rod-like * smectic * twist grain boundary Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.537, year: 2008

Quali- and quantitative analysis of commercial coffee by NMR

International Nuclear Information System (INIS)

Tavares, Leila Aley; Ferreira, Antonio Gilberto

2006-01-01

Coffee is one of the beverages most widely consumed in the world and the 'cafezinho' is normally prepared from a blend of roasted powder of two species, Coffea arabica and Coffea canephora. Each one exhibits differences in their taste and in the chemical composition, especially in the caffeine percentage. There are several procedures proposed in the literature for caffeine determination in different samples like soft drinks, coffee, medicines, etc but most of them need a sample workup which involves at least one step of purification. This work describes the quantitative analysis of caffeine using 1 H NMR and the identification of the major components in commercial coffee samples using 1D and 2D NMR techniques without any sample pre-treatment. (author)

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

NARCIS (Netherlands)

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

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

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

KAUST Repository

Chu, Shidong

2010-11-01

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

A novel in situ electrochemical NMR cell with a palisade gold film electrode

Science.gov (United States)

Ni, Zu-Rong; Cui, Xiao-Hong; Cao, Shuo-Hui; Chen, Zhong

2017-08-01

In situ electrochemical nuclear magnetic resonance (EC-NMR) has attracted considerable attention because of its ability to directly observe real-time electrochemical processes. Therefore, minimizing the incompatibility between the electrochemical device and NMR detection has become an important challenge. A circular thin metal film deposited on the outer surface of a glass tube with a thickness considerably less than the metal skin depth is considered to be the ideal working electrode. In this study, we demonstrate that such a thin film electrode still has a great influence on the radio frequency field homogeneity in the detective zone of the NMR spectrometer probe and provide theoretical and experimental confirmation of its electromagnetic shielding. Furthermore, we propose a novel palisade gold film device to act as the working electrode. The NMR nutation behavior of protons shows that the uniformity of the radio frequency field is greatly improved, increasing the sensitivity in NMR detection. Another advantage of the proposed device is that an external reference standard adapted to the reaction compound can be inserted as a probe to determine the fluctuation of the physico-chemical environment and achieve high-accuracy quantitative NMR analysis. A three-chamber electrochemical device based on the palisade gold film design was successfully fabricated and the in situ electrochemical NMR performance was validated in a standard 5 mm NMR probe by acquiring voltammograms and high-resolution NMR spectra to characterize the electrochemically generated species. The evolution of in situ EC-NMR spectrum monitoring of the redox transformation between p-benzoquinone and hydroquinone demonstrates the ability of the EC-NMR device to simultaneously quantitatively determine the reactants and elucidate the reaction mechanism at the molecular level.

A novel in situ electrochemical NMR cell with a palisade gold film electrode

Directory of Open Access Journals (Sweden)

Zu-Rong Ni

2017-08-01

Full Text Available In situ electrochemical nuclear magnetic resonance (EC-NMR has attracted considerable attention because of its ability to directly observe real-time electrochemical processes. Therefore, minimizing the incompatibility between the electrochemical device and NMR detection has become an important challenge. A circular thin metal film deposited on the outer surface of a glass tube with a thickness considerably less than the metal skin depth is considered to be the ideal working electrode. In this study, we demonstrate that such a thin film electrode still has a great influence on the radio frequency field homogeneity in the detective zone of the NMR spectrometer probe and provide theoretical and experimental confirmation of its electromagnetic shielding. Furthermore, we propose a novel palisade gold film device to act as the working electrode. The NMR nutation behavior of protons shows that the uniformity of the radio frequency field is greatly improved, increasing the sensitivity in NMR detection. Another advantage of the proposed device is that an external reference standard adapted to the reaction compound can be inserted as a probe to determine the fluctuation of the physico-chemical environment and achieve high-accuracy quantitative NMR analysis. A three-chamber electrochemical device based on the palisade gold film design was successfully fabricated and the in situ electrochemical NMR performance was validated in a standard 5 mm NMR probe by acquiring voltammograms and high-resolution NMR spectra to characterize the electrochemically generated species. The evolution of in situ EC-NMR spectrum monitoring of the redox transformation between p-benzoquinone and hydroquinone demonstrates the ability of the EC-NMR device to simultaneously quantitatively determine the reactants and elucidate the reaction mechanism at the molecular level.

{sup 13} C-NMR of mesquite gum

Energy Technology Data Exchange (ETDEWEB)

Andrade, Cristina T; Garcia, Rosangela B [Universidade Federal, Rio de Janeiro, RJ (Brazil). Inst. de Macromoleculas

1992-12-31

Mesquite and guar gums are galactomannans extracted from the seeds of Proposis Juliflora and Cyamopsis tetragonolobus, respectively. An experimental sample of mesquite gum and a commercial sample of guar gum were partially depolymerized by ultrasonic radiation and the produce analysed by high resolution {sup 13} C-NMR spectroscopy. The different carbon lines were resolved and their assignments were done as those reported in the literature. The galactose to mannose ratios (G/M) were estimated from the relative peak areas of the C-1 lines as G/M=61 for mesquite and G/M=0.54 for guar gum. The next nearest-neighbour probabilities (diad frequencies) of the D-galactosyl substitution to the D-mannose backbone were evaluated by integrating C-4 mannose splitted peaks. (author) 9 refs., 2 figs., 2 tabs.

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

Energy Technology Data Exchange (ETDEWEB)

Schot, Gijs van der [Uppsala University, Laboratory of Molecular Biophysics, Department of Cell and Molecular Biology (Sweden); Bonvin, Alexandre M. J. J., E-mail: a.m.j.j.bonvin@uu.nl [Utrecht University, Faculty of Science – Chemistry, Bijvoet Center for Biomolecular Research (Netherlands)

2015-08-15

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Rheo-NMR - how nuclear magnetic resonance is providing new insight regarding complex fluid rheology

International Nuclear Information System (INIS)

Callaghan, P.T.

2000-01-01

Over the past five decades, NMR has revolutionised chemistry, and has found widespread application in condensed matter physics, in molecular biology, in medicine and in food technology. Most recently NMR has made a significant impact in chemical engineering, where it is being extensively used for the non-invasive study of dispersion and flow in porous media. One of the most recent applications of NMR in materials science concerns its use in the study of the mechanical properties of complex fluids. This particular aspect of NMR has been extensively developed in research carried out at Massey University in New Zealand. In this short article, some of the ideas behind this work and the applications which have resulted, will be described. These examples provide a glimpse of possible applications of Nuclear Magnetic Resonance to the study of complex fluid rheology. While this is a very new field of research in which only a handful of groups presently participate, the potential exists for a substantial increase in Rheo-NMR research activity. Systems studied to date include polymer melts and semi-dilute solutions, thermotropic and lyotropic liquid crystals and liquid crystalline polymers, micellar solutions, food materials and colloidal suspensions. Rheo-NMR suffers in a number of respects by comparison with optical methods. It is expensive, it is difficult to use, it suffers from poor signal-to-noise ratios and the effective interpretation of spectra often depends on familiarity with the nuclear spin Hamiltonian and the associated effects of spin dynamics. Nonetheless NMR offers some unique advantages, including the ability to work with opaque materials, the ability to combine velocimetry with localised spectroscopy, and the ability to access a wide range of molecular properties relating to organisation, orientation and dynamics. Rheo-NMR has been able to provide a direct window on a variety of behaviours, including slip, shear-thinning, shear banding, yield stress

Direct Comparison of 19F qNMR and 1H qNMR by Characterizing Atorvastatin Calcium Content

Directory of Open Access Journals (Sweden)

Yang Liu

2016-01-01

Full Text Available Quantitative nuclear magnetic resonance (qNMR is a powerful tool in measuring drug content because of its high speed, sensitivity, and precision. Most of the reports were based on proton qNMR (1H qNMR and only a few fluorine qNMR (19F qNMR were reported. No research has been conducted to directly compare the advantage and disadvantage between these two methods. In the present study, both 19F and 1H qNMR were performed to characterize the content of atorvastatin calcium with the same internal standard. Linearity, precision, and results from two methods were compared. Results showed that 19F qNMR has similar precision and sensitivity to 1H qNMR. Both methods generate similar results compared to mass balance method. Major advantage from 19F qNMR is that the analyte signal is with less or no interference from impurities. 19F qNMR is an excellent approach to quantify fluorine-containing analytes.

Electrokinetic transport of water and methanol in Nafion membranes as observed by NMR spectroscopy

International Nuclear Information System (INIS)

Hallberg, Fredrik; Vernersson, Thomas; Pettersson, Erik Thyboll; Dvinskikh, Sergey V.; Lindbergh, Goeran; Furo, Istvan

2010-01-01

Electrophoretic NMR (eNMR) and pulsed-field-gradient NMR (PFG-NMR) methods were used to study transport processes in situ and in a chemically resolved manner in the electrolyte of an experimental direct methanol fuel cell (DMFC) setup, constituted of several layers of Nafion 117. The measurements were conducted at room temperature for membranes fully swollen by methanol-water mixtures over a wide concentration interval. The experimental setup and the experimental protocol for the eNMR experiments are discussed in detail. The magnitude of the water and methanol self-diffusion coefficients show a good agreement with previously published data while the ratio of the two self-diffusion coefficients may indicate an imperfect mixing of the two solvent molecules. On the molecular level, the drag of water and methanol molecules by protons is roughly of the same magnitude, with the drag of methanol molecules increasing with increasing methanol content. The electro-osmotic drag defined on mass-flow basis increased for methanol from a low level with increasing methanol concentration while that of water remained roughly constant.

Validation of in-line surface characterization by light scattering in Robot Assisted Polishing

DEFF Research Database (Denmark)

Pilny, Lukas; Bissacco, Giuliano; De Chiffre, Leonardo

2014-01-01

The suitability of a commercial scattered light sensor for in-line characterization of fine surfaces in the roughness range Sa 1 – 30 nm generated by the Robot Assisted Polishing (RAP) was investigated and validated. A number of surfaces were generated and directly measured with the scattered light...

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

International Nuclear Information System (INIS)

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

1994-01-01

Wide-pore zeolites modified by gallium oxide has been prepared for catalytic use. Its physico-chemical and catalytic properties have been studied. The structure changes of the catalyst have been investigated by means of MAS NMR spectroscopy. Spectra of 29 Si has been described and discussed

Radiation-induced polymerization of 1, 3-butadiene in urea canal complex as studied by broad line NMR

International Nuclear Information System (INIS)

Yoshii, Fumio; Hayakawa, Naohiro; Abe, Toshihiko

1975-01-01

Dependence of the NMR spectrum on the molar ratio of 1,3-butadiene to urea, temperature dependence of the spectrum and changes of the spectrum during polymerization were observed. The results were discussed in comparison with previously reported results for the canal polymerization of acrylonitrile and vinyl chloride. 1,3-butadiene formes a canal complex with the molar ratio of 1 to 4 for 1,3-butadiene to urea. The urea canal complex is decomposed at -15 0 C. The spectrum of 1,3-butadiene in urea canal complex shows existence of a remarkably mobile component which was not observed on the spectra of acrylonitrile - urea of vinyl chloride - urea canal complex. The line width of 1,3-butadiene in the urea canal complex except the very narrow component was broader than that for vinyl chloride in the urea canal complex over an observed temperature range. The line width of urea formed the canal decreases at lower temperature than those of urea in vinyl chloride - urea canal complex. The post-polymerization of 1,3-butadiene in the urea canal complex started clearly from -78 0 C and completes when the temperature was raised to 20 0 C. The polymerization will be proceeded by the such way that monomer molecules move to the active center in the canal, as considered in the case of the polymerization of acrylonitrile and vinyl chloride in the canal complex. The crystal structure of the urea canal was maintained during polymerization and than the polybutadiene - urea canal complex was necessarily formed after the polymerization. The formation of the polymer - urea canal complex has distinct difference between 1,3-butadiene and acrylonitrile or vinyl chloride. For acrylonitrile and vinyl chloride the canals around the polymer formed are destroyed. The structure of polybutadiene - urea canal complex was hexagonal having a=8.21, c=10.50 A. (auth.)

Surface inspection of flat products by means of texture analysis: on-line implementation using neural networks

Science.gov (United States)

Fernandez, Carlos; Platero, Carlos; Campoy, Pascual; Aracil, Rafael

1994-11-01

This paper describes some texture-based techniques that can be applied to quality assessment of flat products continuously produced (metal strips, wooden surfaces, cork, textile products, ...). Since the most difficult task is that of inspecting for product appearance, human-like inspection ability is required. A common feature to all these products is the presence of non- deterministic texture on their surfaces. Two main subjects are discussed: statistical techniques for both surface finishing determination and surface defect analysis as well as real-time implementation for on-line inspection in high-speed applications. For surface finishing determination a Gray Level Difference technique is presented to perform over low resolution images, that is, no-zoomed images. Defect analysis is performed by means of statistical texture analysis over defective portions of the surface. On-line implementation is accomplished by means of neural networks. When a defect arises, textural analysis is applied which result in a data-vector, acting as input of a neural net, previously trained in a supervised way. This approach tries to reach on-line performance in automated visual inspection applications when texture is presented in flat product surfaces.

Stick-Slip Motion of Moving Contact Line on Chemically Patterned Surfaces

KAUST Repository

Wu, Congmin; Lei, Siulong; Qian, Tiezheng; Wang, Xiaoping

2009-01-01

Based on our continuum hydrodynamic model for immiscible two-phase flows at solid surfaces, the stick-slip motion has been predicted for moving contact line at chemically patterned surfaces [Wang et al., J. Fluid Mech., 605 (2008), pp. 59-78]. In this paper we show that the continuum predictions can be quantitatively verified by molecular dynamics (MD) simulations. Our MD simulations are carried out for two immiscible Lennard-Jones fluids confined by two planar solid walls in Poiseuille flow geometry. In particular, one solid surface is chemically patterned with alternating stripes. For comparison, the continuum model is numerically solved using material parameters directly measured in MD simulations. From oscillatory fluid-fluid interface to intermittent stick-slip motion of moving contact line, we have quantitative agreement between the continuum and MD results. This agreement is attributed to the accurate description down to molecular scale by the generalized Navier boundary condition in our continuum model. Numerical results are also presented for the relaxational dynamics of fluid-fluid interface, in agreement with a theoretical analysis based on the Onsager principle of minimum energy dissipation. © 2010 Global-Science Press.

Ionizing radiation modulates the surface expression of human leukocyte antigen-G in a human melanoma cell line

Energy Technology Data Exchange (ETDEWEB)

Michelin, S.; Gallegos, C.E.; Dubner, D. [Radiopathology Laboratory, Nuclear Regulatory Authority, Buenos Aires (Argentina); Favier, B.; Carosella, E.D. [CEA, I2BM, Hopital Saint-Louis, IUH, Service de Recherches en Hemato-Immunologie, Paris (France)

2009-07-01

Human leukocyte antigen G (HLA-G) is a nonclassical HLA class I molecule involved in fetus protection from the maternal immune system, transplant tolerance, and viral and tumoral immune escape. Tumor-specific HLA-G expression has been described for a wide variety of malignancies, including melanomas. The aim of this study was to evaluate whether ionizing radiation (IR) could modulate the surface expression of HLA-G1 in a human melanoma cell line that expresses endogenously membrane-bound HLA-G1. For this purpose, cells were exposed to increasing doses of {gamma}-irradiation (0-20 Gy) and HLA-G1 levels at the plasma membrane were analyzed at different times postirradiation by flow cytometry. HLA-G total expression and the presence of the soluble form of HLA-G1 (sHLA-G1) in the culture medium of irradiated cells were also evaluated. IR was capable of down regulating cell surface and total HLA-G levels, with a concomitant increase of sHLA-G1 in the medium. These results could indicate that {gamma}-irradiation decreases HLA-G1 surface levels by enhancing the proteolytic cleavage of this molecule. (authors)

Ionizing radiation modulates the surface expression of human leukocyte antigen-G in a human melanoma cell line

International Nuclear Information System (INIS)

Michelin, S.; Gallegos, C.E.; Dubner, D.; Favier, B.; Carosella, E.D.

2009-01-01

Human leukocyte antigen G (HLA-G) is a nonclassical HLA class I molecule involved in fetus protection from the maternal immune system, transplant tolerance, and viral and tumoral immune escape. Tumor-specific HLA-G expression has been described for a wide variety of malignancies, including melanomas. The aim of this study was to evaluate whether ionizing radiation (IR) could modulate the surface expression of HLA-G1 in a human melanoma cell line that expresses endogenously membrane-bound HLA-G1. For this purpose, cells were exposed to increasing doses of γ-irradiation (0-20 Gy) and HLA-G1 levels at the plasma membrane were analyzed at different times postirradiation by flow cytometry. HLA-G total expression and the presence of the soluble form of HLA-G1 (sHLA-G1) in the culture medium of irradiated cells were also evaluated. IR was capable of down regulating cell surface and total HLA-G levels, with a concomitant increase of sHLA-G1 in the medium. These results could indicate that γ-irradiation decreases HLA-G1 surface levels by enhancing the proteolytic cleavage of this molecule. (authors)

Characteristics of Speed Line Cutter and Fringe Analysis of Workpiece Surface

Directory of Open Access Journals (Sweden)

Shuai Wang

2014-02-01

Full Text Available Easy to operate, speed line cutter has a high machining cost performance, so is very popular among the majority of users. The precision of guide rails, screws and nuts used in most of the machines is not high, and the machine control cannot compensate for the screw pitch error, clearance during the transmission and machining error due to electrode wear. Furthermore, control signal may also be lost in control process. The development of speed line cutter focuses on the quality and machining stability of CNC speed line cutter. This article makes an analysis about the impact of machine’s inherent characteristics on machining workpiece surface, and concludes that analysis shall be made on the irregular fringe, therefore to heighten the machining precision.

CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

International Nuclear Information System (INIS)

Skinner, Simon P.; Fogh, Rasmus H.; Boucher, Wayne; Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W.

2016-01-01

NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

CcpNmr AnalysisAssign: a flexible platform for integrated NMR analysis

Energy Technology Data Exchange (ETDEWEB)

Skinner, Simon P.; Fogh, Rasmus H. [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom); Boucher, Wayne [University of Cambridge, Department of Biochemistry (United Kingdom); Ragan, Timothy J.; Mureddu, Luca G.; Vuister, Geerten W., E-mail: gv29@le.ac.uk [University of Leicester, Department of Molecular and Cell Biology, Leicester Institute for Structural- and Chemical Biology (United Kingdom)

2016-10-15

NMR spectroscopy is an indispensably powerful technique for the analysis of biomolecules under ambient conditions, both for structural- and functional studies. However, in practice the complexity of the technique has often frustrated its application by non-specialists. In this paper, we present CcpNmr version-3, the latest software release from the Collaborative Computational Project for NMR, for all aspects of NMR data analysis, including liquid- and solid-state NMR data. This software has been designed to be simple, functional and flexible, and aims to ensure that routine tasks can be performed in a straightforward manner. We have designed the software according to modern software engineering principles and leveraged the capabilities of modern graphics libraries to simplify a variety of data analysis tasks. We describe the process of backbone assignment as an example of the flexibility and simplicity of implementing workflows, as well as the toolkit used to create the necessary graphics for this workflow. The package can be downloaded from www.ccpn.ac.uk/v3-software/downloads http://www.ccpn.ac.uk/v3-software/downloads and is freely available to all non-profit organisations.

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

Science.gov (United States)

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

2002-06-01

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

Precise predictions of H2O line shapes over a wide pressure range using simulations corrected by a single measurement

Science.gov (United States)

Ngo, N. H.; Nguyen, H. T.; Tran, H.

2018-03-01

In this work, we show that precise predictions of the shapes of H2O rovibrational lines broadened by N2, over a wide pressure range, can be made using simulations corrected by a single measurement. For that, we use the partially-correlated speed-dependent Keilson-Storer (pcsdKS) model whose parameters are deduced from molecular dynamics simulations and semi-classical calculations. This model takes into account the collision-induced velocity-changes effects, the speed dependences of the collisional line width and shift as well as the correlation between velocity and internal-state changes. For each considered transition, the model is corrected by using a parameter deduced from its broadening coefficient measured for a single pressure. The corrected-pcsdKS model is then used to simulate spectra for a wide pressure range. Direct comparisons of the corrected-pcsdKS calculated and measured spectra of 5 rovibrational lines of H2O for various pressures, from 0.1 to 1.2 atm, show very good agreements. Their maximum differences are in most cases well below 1%, much smaller than residuals obtained when fitting the measurements with the Voigt line shape. This shows that the present procedure can be used to predict H2O line shapes for various pressure conditions and thus the simulated spectra can be used to deduce the refined line-shape parameters to complete spectroscopic databases, in the absence of relevant experimental values.

NMR investigations of the melting behaviour of mesogen compounds

International Nuclear Information System (INIS)

Limmer, S.; Grande, S.; Loesche, A.

1977-01-01

Proton NMR spectra of mesogen compounds in the solid phase are recorded. Between 20 and 40 K and 4 and 12 K below the melting point they exhibit a very narrow central line with a structure caused by the chemical shift, which is superimposed to the broad structureless line normally expected from polycrystalline solid phases. It is concluded that it originates from ''quasi-liquid'' molecules whose intensity grows drastically with increasing temperature and involves a maximum of about 2.5% of the whole intensity of the spectrum. In the region close to the melting point appears another lineshape, the so-called ''super-Lorentzian'' line, whose intensity increases still stronger than that of the narrow line. It can be shown that it is due to the existence of mesomorphic clusters the directors of which are statistically distributed in the sample. The impurity dependence of these effects is investigated and an attempt is made to explain them. (author)

Solid-phase extraction NMR studies of chromatographic fractions of saponins from Quillaja saponaria.

Science.gov (United States)

Nyberg, Nils T; Baumann, Herbert; Kenne, Lennart

2003-01-15

The saponin mixture QH-B from the tree Quillaja saponaria var. Molina was fractionated by RP-HPLC in several steps. The fractions were analyzed by solid-phase extraction NMR (SPE-NMR), a technique combining the workup by solid-phase extraction with on-line coupling to an NMR flow probe. Together with MALDI-TOF mass spectrometry and comparison with chemical shifts of similar saponins, the structures of both major and minor components in QH-B could be obtained. The procedure described is a simple method to determine the structure of components in a complex mixture. The two major fractions of the mixture were found to contain at least 28 saponins, differing in the carbohydrate substructures. Eight of these have not previously been determined. The 28 saponins formed 14 equilibrium pairs by the migration of an O-acyl group between two adjacent positions on a fucosyl residue.

High resolution solid-state NMR spectroscopy of the Yersinia pestis outer membrane protein Ail in lipid membranes

Energy Technology Data Exchange (ETDEWEB)

Yao, Yong; Dutta, Samit Kumar [Sanford Burnham Prebys Medical Discovery Institute (United States); Park, Sang Ho; Rai, Ratan [University of California San Diego, Department of Chemistry and Biochemistry (United States); Fujimoto, L. Miya; Bobkov, Andrey A. [Sanford Burnham Prebys Medical Discovery Institute (United States); Opella, Stanley J. [University of California San Diego, Department of Chemistry and Biochemistry (United States); Marassi, Francesca M., E-mail: fmarassi@sbp.edu [Sanford Burnham Prebys Medical Discovery Institute (United States)

2017-03-15

The outer membrane protein Ail (Adhesion invasion locus) is one of the most abundant proteins on the cell surface of Yersinia pestis during human infection. Its functions are expressed through interactions with a variety of human host proteins, and are essential for microbial virulence. Structures of Ail have been determined by X-ray diffraction and solution NMR spectroscopy, but those samples contained detergents that interfere with functionality, thus, precluding analysis of the structural basis for Ail’s biological activity. Here, we demonstrate that high-resolution solid-state NMR spectra can be obtained from samples of Ail in detergent-free phospholipid liposomes, prepared with a lipid to protein molar ratio of 100. The spectra, obtained with {sup 13}C or {sup 1}H detection, have very narrow line widths (0.40–0.60 ppm for {sup 13}C, 0.11–0.15 ppm for {sup 1}H, and 0.46–0.64 ppm for {sup 15}N) that are consistent with a high level of sample homogeneity. The spectra enable resonance assignments to be obtained for N, CO, CA and CB atomic sites from 75 out of 156 residues in the sequence of Ail, including 80% of the transmembrane region. The {sup 1}H-detected solid-state NMR {sup 1}H/{sup 15}N correlation spectra obtained for Ail in liposomes compare very favorably with the solution NMR {sup 1}H/{sup 15}N TROSY spectra obtained for Ail in nanodiscs prepared with a similar lipid to protein molar ratio. These results set the stage for studies of the molecular basis of the functional interactions of Ail with its protein partners from human host cells, as well as the development of drugs targeting Ail.

CASD-NMR 2: robust and accurate unsupervised analysis of raw NOESY spectra and protein structure determination with UNIO

International Nuclear Information System (INIS)

Guerry, Paul; Duong, Viet Dung; Herrmann, Torsten

2015-01-01

UNIO is a comprehensive software suite for protein NMR structure determination that enables full automation of all NMR data analysis steps involved—including signal identification in NMR spectra, sequence-specific backbone and side-chain resonance assignment, NOE assignment and structure calculation. Within the framework of the second round of the community-wide stringent blind NMR structure determination challenge (CASD-NMR 2), we participated in two categories of CASD-NMR 2, namely using either raw NMR spectra or unrefined NOE peak lists as input. A total of 15 resulting NMR structure bundles were submitted for 9 out of 10 blind protein targets. All submitted UNIO structures accurately coincided with the corresponding blind targets as documented by an average backbone root mean-square deviation to the reference proteins of only 1.2 Å. Also, the precision of the UNIO structure bundles was virtually identical to the ensemble of reference structures. By assessing the quality of all UNIO structures submitted to the two categories, we find throughout that only the UNIO–ATNOS/CANDID approach using raw NMR spectra consistently yielded structure bundles of high quality for direct deposition in the Protein Data Bank. In conclusion, the results obtained in CASD-NMR 2 are another vital proof for robust, accurate and unsupervised NMR data analysis by UNIO for real-world applications

Solid-state NMR, electrophysiology and molecular dynamics characterization of human VDAC2

International Nuclear Information System (INIS)

Gattin, Zrinka; Schneider, Robert; Laukat, Yvonne; Giller, Karin; Maier, Elke; Zweckstetter, Markus; Griesinger, Christian; Benz, Roland; Becker, Stefan; Lange, Adam

2015-01-01

The voltage-dependent anion channel (VDAC) is the most abundant protein of the outer mitochondrial membrane and constitutes the major pathway for the transport of ADP, ATP, and other metabolites. In this multidisciplinary study we combined solid-state NMR, electrophysiology, and molecular dynamics simulations, to study the structure of the human VDAC isoform 2 in a lipid bilayer environment. We find that the structure of hVDAC2 is similar to the structure of hVDAC1, in line with recent investigations on zfVDAC2. However, hVDAC2 appears to exhibit an increased conformational heterogeneity compared to hVDAC1 which is reflected in broader solid-state NMR spectra and less defined electrophysiological profiles

Solid-state NMR, electrophysiology and molecular dynamics characterization of human VDAC2

Energy Technology Data Exchange (ETDEWEB)

Gattin, Zrinka; Schneider, Robert; Laukat, Yvonne; Giller, Karin [Max Planck Institute for Biophysical Chemistry (Germany); Maier, Elke [Theodor-Boveri-Institut (Biozentrum) der Universität Würzburg, Lehrstuhl für Biotechnologie (Germany); Zweckstetter, Markus; Griesinger, Christian [Max Planck Institute for Biophysical Chemistry (Germany); Benz, Roland [Theodor-Boveri-Institut (Biozentrum) der Universität Würzburg, Lehrstuhl für Biotechnologie (Germany); Becker, Stefan; Lange, Adam, E-mail: alange@fmp-berlin.de [Max Planck Institute for Biophysical Chemistry (Germany)

2015-04-15

The voltage-dependent anion channel (VDAC) is the most abundant protein of the outer mitochondrial membrane and constitutes the major pathway for the transport of ADP, ATP, and other metabolites. In this multidisciplinary study we combined solid-state NMR, electrophysiology, and molecular dynamics simulations, to study the structure of the human VDAC isoform 2 in a lipid bilayer environment. We find that the structure of hVDAC2 is similar to the structure of hVDAC1, in line with recent investigations on zfVDAC2. However, hVDAC2 appears to exhibit an increased conformational heterogeneity compared to hVDAC1 which is reflected in broader solid-state NMR spectra and less defined electrophysiological profiles.

{sup 77}Se NMR study of nonmagnetic-magnetic transition in (TMTSF){sub 2}X

Energy Technology Data Exchange (ETDEWEB)

Mito, T., E-mail: mito_takeshi@hotmail.co [Graduate School of Material Science, University of Hyogo, Hyogo 678-1297 (Japan); Nishiyama, K.; Koyama, T.; Ueda, K.; Kohara, T.; Takeuchi, K.; Akutsu, H.; Yamada, J. [Graduate School of Material Science, University of Hyogo, Hyogo 678-1297 (Japan); Kornilov, A.; Pudalov, V.M. [P.N. Lebedev Physics Institute, Moscow 119991 (Russian Federation); Qualls, J.S. [Sonoma State University, Rohnert Park, CA 94928 (United States)

2010-12-15

{sup 77}Se NMR measurements have been carried out on (TMTSF){sub 2}X (X = PF{sub 6} and AsF{sub 6}) single crystals. For both compounds, NMR lines split into double-peaked spectra in the SDW state, which is explained with sinusoidal internal field at Se nucleus positions having the same incommensurate wave number with that of the SDW order. No change in the lineshape was observed at T{sub x} at which the spin-relaxation rate shows a kink, suggesting that this anomaly does not cause significant static changes in internal field at the Se-site.

Picosecond wide-field time-correlated single photon counting fluorescence microscopy with a delay line anode detector

Energy Technology Data Exchange (ETDEWEB)

Hirvonen, Liisa M.; Le Marois, Alix; Suhling, Klaus, E-mail: klaus.suhling@kcl.ac.uk [Department of Physics, King' s College London, Strand, London WC2R 2LS (United Kingdom); Becker, Wolfgang; Smietana, Stefan [Becker & Hickl GmbH, Nahmitzer Damm 30, 12277 Berlin (Germany); Milnes, James; Conneely, Thomas [Photek Ltd., 26 Castleham Rd, Saint Leonards-on-Sea TN38 9NS (United Kingdom); Jagutzki, Ottmar [Institut für Kernphysik, Max-von-Laue-Str. 1, 60438 Frankfurt (Germany)

2016-08-15

We perform wide-field time-correlated single photon counting-based fluorescence lifetime imaging (FLIM) with a crossed delay line anode image intensifier, where the pulse propagation time yields the photon position. This microchannel plate-based detector was read out with conventional fast timing electronics and mounted on a fluorescence microscope with total internal reflection (TIR) illumination. The picosecond time resolution of this detection system combines low illumination intensity of microwatts with wide-field data collection. This is ideal for fluorescence lifetime imaging of cell membranes using TIR. We show that fluorescence lifetime images of living HeLa cells stained with membrane dye di-4-ANEPPDHQ exhibit a reduced lifetime near the coverslip in TIR compared to epifluorescence FLIM.

Specific binding of a naturally occurring amyloidogenic fragment of Streptococcus mutans adhesin P1 to intact P1 on the cell surface characterized by solid state NMR spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Tang, Wenxing; Bhatt, Avni [University of Florida, Department of Biochemistry and Molecular Biology, College of Medicine (United States); Smith, Adam N. [University of Florida, Department of Chemistry, College of Liberal Arts and Sciences (United States); Crowley, Paula J.; Brady, L. Jeannine, E-mail: jbrady@dental.ufl.edu [University of Florida, Department of Oral Biology, College of Dentistry (United States); Long, Joanna R., E-mail: jrlong@ufl.edu [University of Florida, Department of Biochemistry and Molecular Biology, College of Medicine (United States)

2016-02-15

The P1 adhesin (aka Antigen I/II or PAc) of the cariogenic bacterium Streptococcus mutans is a cell surface-localized protein involved in sucrose-independent adhesion and colonization of the tooth surface. The immunoreactive and adhesive properties of S. mutans suggest an unusual functional quaternary ultrastructure comprised of intact P1 covalently attached to the cell wall and interacting with non-covalently associated proteolytic fragments thereof, particularly the ∼57-kDa C-terminal fragment C123 previously identified as Antigen II. S. mutans is capable of amyloid formation when grown in a biofilm and P1 is among its amyloidogenic proteins. The C123 fragment of P1 readily forms amyloid fibers in vitro suggesting it may play a role in the formation of functional amyloid during biofilm development. Using wild-type and P1-deficient strains of S. mutans, we demonstrate that solid state NMR (ssNMR) spectroscopy can be used to (1) globally characterize cell walls isolated from a Gram-positive bacterium and (2) characterize the specific binding of heterologously expressed, isotopically-enriched C123 to cell wall-anchored P1. Our results lay the groundwork for future high-resolution characterization of the C123/P1 ultrastructure and subsequent steps in biofilm formation via ssNMR spectroscopy, and they support an emerging model of S. mutans colonization whereby quaternary P1-C123 interactions confer adhesive properties important to binding to immobilized human salivary agglutinin.

Specific binding of a naturally occurring amyloidogenic fragment of Streptococcus mutans adhesin P1 to intact P1 on the cell surface characterized by solid state NMR spectroscopy

International Nuclear Information System (INIS)

Tang, Wenxing; Bhatt, Avni; Smith, Adam N.; Crowley, Paula J.; Brady, L. Jeannine; Long, Joanna R.

2016-01-01

The P1 adhesin (aka Antigen I/II or PAc) of the cariogenic bacterium Streptococcus mutans is a cell surface-localized protein involved in sucrose-independent adhesion and colonization of the tooth surface. The immunoreactive and adhesive properties of S. mutans suggest an unusual functional quaternary ultrastructure comprised of intact P1 covalently attached to the cell wall and interacting with non-covalently associated proteolytic fragments thereof, particularly the ∼57-kDa C-terminal fragment C123 previously identified as Antigen II. S. mutans is capable of amyloid formation when grown in a biofilm and P1 is among its amyloidogenic proteins. The C123 fragment of P1 readily forms amyloid fibers in vitro suggesting it may play a role in the formation of functional amyloid during biofilm development. Using wild-type and P1-deficient strains of S. mutans, we demonstrate that solid state NMR (ssNMR) spectroscopy can be used to (1) globally characterize cell walls isolated from a Gram-positive bacterium and (2) characterize the specific binding of heterologously expressed, isotopically-enriched C123 to cell wall-anchored P1. Our results lay the groundwork for future high-resolution characterization of the C123/P1 ultrastructure and subsequent steps in biofilm formation via ssNMR spectroscopy, and they support an emerging model of S. mutans colonization whereby quaternary P1-C123 interactions confer adhesive properties important to binding to immobilized human salivary agglutinin

Specific binding of a naturally occurring amyloidogenic fragment of Streptococcus mutans adhesin P1 to intact P1 on the cell surface characterized by solid state NMR spectroscopy.

Science.gov (United States)

Tang, Wenxing; Bhatt, Avni; Smith, Adam N; Crowley, Paula J; Brady, L Jeannine; Long, Joanna R

2016-02-01

The P1 adhesin (aka Antigen I/II or PAc) of the cariogenic bacterium Streptococcus mutans is a cell surface-localized protein involved in sucrose-independent adhesion and colonization of the tooth surface. The immunoreactive and adhesive properties of S. mutans suggest an unusual functional quaternary ultrastructure comprised of intact P1 covalently attached to the cell wall and interacting with non-covalently associated proteolytic fragments thereof, particularly the ~57-kDa C-terminal fragment C123 previously identified as Antigen II. S. mutans is capable of amyloid formation when grown in a biofilm and P1 is among its amyloidogenic proteins. The C123 fragment of P1 readily forms amyloid fibers in vitro suggesting it may play a role in the formation of functional amyloid during biofilm development. Using wild-type and P1-deficient strains of S. mutans, we demonstrate that solid state NMR (ssNMR) spectroscopy can be used to (1) globally characterize cell walls isolated from a Gram-positive bacterium and (2) characterize the specific binding of heterologously expressed, isotopically-enriched C123 to cell wall-anchored P1. Our results lay the groundwork for future high-resolution characterization of the C123/P1 ultrastructure and subsequent steps in biofilm formation via ssNMR spectroscopy, and they support an emerging model of S. mutans colonization whereby quaternary P1-C123 interactions confer adhesive properties important to binding to immobilized human salivary agglutinin.

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

DEFF Research Database (Denmark)

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

2013-01-01

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

NMR for chemists and biologists

CERN Document Server

Carbajo, Rodrigo J

2013-01-01

This book offers a concise introduction to the field of nuclear magnetic resonance or NMR. It presents the basic foundations of NMR in a non-mathematical way and provides an overview of both recent and important biological applications of NMR.

Compact NMR

Energy Technology Data Exchange (ETDEWEB)

Bluemich, Bernhard; Haber-Pohlmeier, Sabina; Zia, Wasif [RWTH Aachen Univ. (Germany). Inst. fuer Technische und Makromolekulare Chemie (ITMC)

2014-06-01

Nuclear Magnetic Resonance (NMR) spectroscopy is the most popular method for chemists to analyze molecular structures, while Magnetic Resonance Imaging (MRI) is a non-invasive diagnostic tool for medical doctors that provides high-contrast images of biological tissue. In both applications, the sample (or patient) is positioned inside a large, superconducting magnet to magnetize the atomic nuclei. Interrogating radio-frequency pulses result in frequency spectra that provide the chemist with molecular information, the medical doctor with anatomic images, and materials scientist with NMR relaxation parameters. Recent advances in magnet technology have led to a variety of small permanent magnets to allow compact and low-cost instruments. The goal of this book is to provide an introduction to the practical use of compact NMR at a level nearly as basic as the operation of a smart phone.

Development and Investigation of NMR tools for chiral compound identification

Energy Technology Data Exchange (ETDEWEB)

Alam, Todd Michael [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States). Electronic, Optical and Nano Materials; Lansdon, Rick [Oak Ridge Inst. for Science and Education (ORISE), Oak Ridge, TN (United States)

2014-09-01

The goal behind the assigned summer project was to investigate the ability of nuclear magnetic resonance spectroscopy (NMR) to identify enantiomers of select chiral organo-fluorophosphates (OFPs) compounds which are analogs of chemical warfare agents (CWAs, e.g. Sarin). This involved investigations utilizing chiral solvating agents (CSAs) and characterizing the binding phenomena with cyclodextrins. The resolution of OFPs enantiomers using NMR would be useful for research into toxicodynamics and toxicokinetics in biological systems due to the widely differing properties of the CWA enantiomers [1]. The optimization of decontamination abilities in the case of a CWA events, with this method’s potential rapidity and robustness, as well as the development of models correlating chiral compounds with CSAs for optimal resolution are all rational benefits of this research.

Dynamics of Gradient Bioceramic Composite Coating on Surface of Titanium Alloy by Wide-Band Laser Cladding

Institute of Scientific and Technical Information of China (English)

LIU Qi-bin; ZOU Long-jiang; ZHU Wei-dong; LI Hai-tao; DONG Chuang

2004-01-01

The gradient bioceramic coating was prepared on the surface of titanium alloy using wide-band laser cladding. The dynamics of gradient bioceramic composite coating containing hydroxyapatite (HA) prepared with mixture of CaHPO4*2H2O and CaCO3 under the condition of wide-band laser was studied theoretically. The corresponding mathematical model and its numerical solution were presented. The examination experiment showed that HA bioceramic composite coatings can be obtained by appropriately choosing wide-band laser cladding parameters. The microstructure and surface morphology of HA bioceramic coating were observed by SEM and X-ray diffraction. The experimental results showed that the bioceramic coating is composed of HA, β-TCP, CaO, CaTiO3 and TiO2. The surface of bioceramic coating takes coral-shaped structure or short-rod piled structure, which helps osteoblast grow into bioceramic and improves the biocompatibility.

Precise NMR measurement and stabilization system of magnetic field of a superconducting 7 T wave length shifter

CERN Document Server

Borovikov, V M; Karpov, G V; Korshunov, D A; Kuper, E A; Kuzin, M V; Mamkin, V R; Medvedko, A S; Mezentsev, N A; Repkov, V V; Shkaruba, V A; Shubin, E I; Veremeenko, V F

2001-01-01

The system of measurement and stabilization of the magnetic field in the superconducting 7 T wave length shifter (WLS), designed at Budker Institute of Nuclear Physics are described. The measurements are performed by nuclear magnetic resonance (NMR) magnetometer at two points of the WLS magnetic field. Stabilization of the field is provided by the current pumping system. The stabilization system is based on precise NMR measurement of magnetic field as a feedback signal for computer code which control currents inside the superconducting coils. The problem of the magnetic field measurements with NMR method consists in wide spread of field in the measured area (up to 50 Gs/mm), wide temperature range of WLS operating, small space for probe and influence of iron hysteresis. Special solid-state probes were designed to satisfy this requirements. The accuracy of magnetic field measurements at probe locations is not worse than 20 ppm. For the WLS field of 7 T the reproducibility of the magnetic field of 30 ppm has be...

Drop evaporation on superhydrophobic PTFE surfaces driven by contact line dynamics.

Science.gov (United States)

Ramos, S M M; Dias, J F; Canut, B

2015-02-15

In the present study, we experimentally study the evaporation modes and kinetics of sessile drops of water on highly hydrophobic surfaces (contact angle ∼160°), heated to temperatures ranging between 40° and 70 °C. These surfaces were initially constructed by means of controlled tailoring of polytetrafluoroethylene (PTFE) substrates. The evaporation of droplets was observed to occur in three distinct phases, which were the same for the different substrate temperatures. The drops started to evaporate in the constant contact radius (CCR) mode, then switched to a more complex mode characterized by a set of stick-slip events accompanied by a decrease in contact angle, and finally shifted to a mixed mode in which the contact radius and contact angle decreased simultaneously until the drops had completely evaporated. It is shown that in the case of superhydrophobic surfaces, the energy barriers (per unit length) associated with the stick-slip motion of a drop ranges in the nJ m(-1) scale. Furthermore, analysis of the evaporation rates, determined from experimental data show that, even in the CCR mode, a linear relationship between V(2/3) and the evaporation time is verified. The values of the evaporation rate constants are found to be higher in the pinned contact line regime (the CCR mode) than in the moving contact line regime. This behavior is attributed to the drop's higher surface to volume ratio in the CCR mode. Copyright © 2014 Elsevier Inc. All rights reserved.

Contact angle and local wetting at contact line.

Science.gov (United States)

Li, Ri; Shan, Yanguang

2012-11-06

This theoretical study was motivated by recent experiments and theoretical work that had suggested the dependence of the static contact angle on the local wetting at the triple-phase contact line. We revisit this topic because the static contact angle as a local wetting parameter is still not widely understood and clearly known. To further clarify the relationship of the static contact angle with wetting, two approaches are applied to derive a general equation for the static contact angle of a droplet on a composite surface composed of heterogeneous components. A global approach based on the free surface energy of a thermodynamic system containing the droplet and solid surface shows the static contact angle as a function of local surface chemistry and local wetting state at the contact line. A local approach, in which only local forces acting on the contact line are considered, results in the same equation. The fact that the local approach agrees with the global approach further demonstrates the static contact angle as a local wetting parameter. Additionally, the study also suggests that the wetting described by the Wenzel and Cassie equations is also the local wetting of the contact line rather than the global wetting of the droplet.

High-resolution, high-sensitivity NMR of nano-litre anisotropic samples by coil spinning

Energy Technology Data Exchange (ETDEWEB)

Sakellariou, D [CEA Saclay, DSM, DRECAM, SCM, Lab Struct and Dynam Resonance Magnet, CNRS URA 331, F-91191 Gif Sur Yvette, (France); Le Goff, G; Jacquinot, J F [CEA Saclay, DSM, DRECAM, SPEC: Serv Phys Etat Condense, CNRS URA 2464, F-91191 Gif Sur Yvette, (France)

2007-07-01

accordingly expect that it will facilitate the development of novel solid-state NMR methodologies and find wide use in high-throughput chemical and biomedical analysis. (authors)

An interaction analysis of twin surface cracks by the line-spring model

International Nuclear Information System (INIS)

Kim, Y.J.; Yang, W.H.; Choy, Y.S.; Lee, J.S.

1992-01-01

The fracture mechanics analysis of surface cracks is important for the integrity evaluation of flawed structural components. The objective of this paper is to numerically investigate the interaction effect of twin surface cracks in plate and cylindrical geometrie. First the usefulness of the line-spring model is verified by analyzing a single surface crack in a plate, and then the model is extended to twin surface crack in plate and cylindrical geometries. For the case of a finite plate under uniaxial loading, the effect of crack spacing on the stress intensity factor is negligible. However, for the case of a cylinder under moderate internal pressure, a significant increase in stress intensity factor is observed at the deepest point of the surface crack. (orig.)

A surface containing a line and a circle through each point is a quadric

KAUST Repository

Nilov, Fedor K.; Skopenkov, Mikhail

2012-01-01

We prove that a surface in 3-dimensional Euclidean space containing a line and a circle through each point is a quadric. We also give some particular results on the classification of surfaces containing several circles through each point. © 2012 Springer Science+Business Media B.V.

A surface containing a line and a circle through each point is a quadric

KAUST Repository

Nilov, Fedor K.

2012-06-20

We prove that a surface in 3-dimensional Euclidean space containing a line and a circle through each point is a quadric. We also give some particular results on the classification of surfaces containing several circles through each point. © 2012 Springer Science+Business Media B.V.

ASIC-based design of NMR system health monitor for mission/safety-critical applications.

Science.gov (United States)

Balasubramanian, P

2016-01-01

N-modular redundancy (NMR) is a generic fault tolerance scheme that is widely used in safety-critical circuit/system designs to guarantee the correct operation with enhanced reliability. In passive NMR, at least a majority (N + 1)/2 out of N function modules is expected to operate correctly at any time, where N is odd. Apart from a conventional realization of the NMR system, it would be useful to provide a concurrent indication of the system's health so that an appropriate remedial action may be initiated depending upon an application's safety criticality. In this context, this article presents the novel design of a generic NMR system health monitor which features: (i) early fault warning logic, that is activated upon the production of a conflicting result by even one output of any arbitrary function module, and (ii) error signalling logic, which signals an error when the number of faulty function modules unfortunately attains a majority and the system outputs may no more be reliable. Two sample implementations of NMR systems viz. triple modular redundancy and quintuple modular redundancy with the proposed system health monitoring are presented in this work, with a 4-bit ALU used for the function modules. The simulations are performed using a 32/28 nm CMOS process technology.

Cortical surface registration using spherical thin-plate spline with sulcal lines and mean curvature as features.

Science.gov (United States)

Park, Hyunjin; Park, Jun-Sung; Seong, Joon-Kyung; Na, Duk L; Lee, Jong-Min

2012-04-30

Analysis of cortical patterns requires accurate cortical surface registration. Many researchers map the cortical surface onto a unit sphere and perform registration of two images defined on the unit sphere. Here we have developed a novel registration framework for the cortical surface based on spherical thin-plate splines. Small-scale composition of spherical thin-plate splines was used as the geometric interpolant to avoid folding in the geometric transform. Using an automatic algorithm based on anisotropic skeletons, we extracted seven sulcal lines, which we then incorporated as landmark information. Mean curvature was chosen as an additional feature for matching between spherical maps. We employed a two-term cost function to encourage matching of both sulcal lines and the mean curvature between the spherical maps. Application of our registration framework to fifty pairwise registrations of T1-weighted MRI scans resulted in improved registration accuracy, which was computed from sulcal lines. Our registration approach was tested as an additional procedure to improve an existing surface registration algorithm. Our registration framework maintained an accurate registration over the sulcal lines while significantly increasing the cross-correlation of mean curvature between the spherical maps being registered. Copyright © 2012 Elsevier B.V. All rights reserved.

Structural Biology: Practical NMR Applications

CERN Document Server

Teng, Quincy

2005-01-01

This textbook begins with an overview of NMR development and applications in biological systems. It describes recent developments in instrument hardware and methodology. Chapters highlight the scope and limitation of NMR methods. While detailed math and quantum mechanics dealing with NMR theory have been addressed in several well-known NMR volumes, chapter two of this volume illustrates the fundamental principles and concepts of NMR spectroscopy in a more descriptive manner. Topics such as instrument setup, data acquisition, and data processing using a variety of offline software are discussed. Chapters further discuss several routine stategies for preparing samples, especially for macromolecules and complexes. The target market for such a volume includes researchers in the field of biochemistry, chemistry, structural biology and biophysics.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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

Science.gov (United States)

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

2003-01-01

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

Ligand-receptor Interactions by NMR Spectroscopy

Directory of Open Access Journals (Sweden)

Novak. P.

2008-04-01

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

NMR spectroscopy study of agar-based polymers electrolytes

Energy Technology Data Exchange (ETDEWEB)

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

2012-07-01

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

International school on high field NMR spectroscopy for solids and liquids

Energy Technology Data Exchange (ETDEWEB)

Marion, D.; Meier, B.; Keeler, J.; Berthault, P.; Vedrine, P.; Grandinetti, P.; Delsuc, M.A.; Spiess, H

2006-07-01

The aim of the school is to offer high-level pedagogical courses on a wide range of liquid- and solid-state NMR concepts and techniques: theory, instrumentation (magnets and probes), data acquisition, processing and analysis, measurement of dipolar and quadrupolar couplings, spin relaxation and hyper-polarization. This document gathers only the slides of most presentations.

International school on high field NMR spectroscopy for solids and liquids

International Nuclear Information System (INIS)

Marion, D.; Meier, B.; Keeler, J.; Berthault, P.; Vedrine, P.; Grandinetti, P.; Delsuc, M.A.; Spiess, H.

2006-01-01

The aim of the school is to offer high-level pedagogical courses on a wide range of liquid- and solid-state NMR concepts and techniques: theory, instrumentation (magnets and probes), data acquisition, processing and analysis, measurement of dipolar and quadrupolar couplings, spin relaxation and hyper-polarization. This document gathers only the slides of most presentations

Solid-state NMR of the Yersinia pestis outer membrane protein Ail in lipid bilayer nanodiscs sedimented by ultracentrifugation

International Nuclear Information System (INIS)

Ding, Yi; Fujimoto, L. Miya; Yao, Yong; Marassi, Francesca M.

2015-01-01

Solid-state NMR studies of sedimented soluble proteins has been developed recently as an attractive approach for overcoming the size limitations of solution NMR spectroscopy while bypassing the need for sample crystallization or precipitation (Bertini et al. Proc Natl Acad Sci USA 108(26):10396–10399, 2011). Inspired by the potential benefits of this method, we have investigated the ability to sediment lipid bilayer nanodiscs reconstituted with a membrane protein. In this study, we show that nanodiscs containing the outer membrane protein Ail from Yersinia pestis can be sedimented for solid-state NMR structural studies, without the need for precipitation or lyophilization. Optimized preparations of Ail in phospholipid nanodiscs support both the structure and the fibronectin binding activity of the protein. The same sample can be used for solution NMR, solid-state NMR and activity assays, facilitating structure–activity correlation experiments across a wide range of timescales

Solid-state NMR of the Yersinia pestis outer membrane protein Ail in lipid bilayer nanodiscs sedimented by ultracentrifugation

Energy Technology Data Exchange (ETDEWEB)

Ding, Yi; Fujimoto, L. Miya; Yao, Yong; Marassi, Francesca M., E-mail: fmarassi@sbmri.org [Sanford-Burnham Medical Research Institute (United States)

2015-04-15

Solid-state NMR studies of sedimented soluble proteins has been developed recently as an attractive approach for overcoming the size limitations of solution NMR spectroscopy while bypassing the need for sample crystallization or precipitation (Bertini et al. Proc Natl Acad Sci USA 108(26):10396–10399, 2011). Inspired by the potential benefits of this method, we have investigated the ability to sediment lipid bilayer nanodiscs reconstituted with a membrane protein. In this study, we show that nanodiscs containing the outer membrane protein Ail from Yersinia pestis can be sedimented for solid-state NMR structural studies, without the need for precipitation or lyophilization. Optimized preparations of Ail in phospholipid nanodiscs support both the structure and the fibronectin binding activity of the protein. The same sample can be used for solution NMR, solid-state NMR and activity assays, facilitating structure–activity correlation experiments across a wide range of timescales.

Final Report: DoE SBIR Phase 2 Low-Cost Small Diameter NMR Technologies for In-Situ Subsurface Characterization and Monitoring

Energy Technology Data Exchange (ETDEWEB)

Walsh, David Oliver [Vista Clara Inc., Mukilteo, WA (United States)

2010-09-03

In this Phase 2 SBIR program, Vista Clara successfully developed and field-tested small diameter NNR logging tools for subsurface characterization and monitoring. This effort involved the design and development surface electronics, a winch with 470ft cable, and three interchangeable downhole probes: a 3.5â diameter borehole NMR probe, a 1.67â diameter borehole NMR probe, and a 2.5â diameter NMR probe that can be deployed using a Geoprobe direct push machine. The 3.5â probe was tested extensively over a 6 week period including 4â to 8â boreholes in Washington, Idaho, Nebraska, Colorado, Kansas, Connecticut and Massachusetts. The field test campaign was highly successful. The 1.67â probe was assembled, tested and calibrated in the laboratory. The 2.5â Geoprobe probe is in final assembly and testing at the time of this report. The completed Phase 2 R&D program has resulted in the first NMR logging tool that can be deployed in boreholes of 4â diameter, the first NMR logging tool that can be deployed in boreholes on 2â diameter, and the first NMR logging tool that can be deployed by a direct push machine. These small diameter tools make NMR logging technically and economically feasible, for the first time. Previously available NMR logging tools were developed for oilfield applications and are prohibitively large and expensive for the majority of near surface groundwater characterization problems.

Two dimensional solid state NMR

International Nuclear Information System (INIS)

Kentgens, A.P.M.

1987-01-01

This thesis illustrates, by discussing some existing and newly developed 2D solid state experiments, that two-dimensional NMR of solids is a useful and important extension of NMR techniques. Chapter 1 gives an overview of spin interactions and averaging techniques important in solid state NMR. As 2D NMR is already an established technique in solutions, only the basics of two dimensional NMR are presented in chapter 2, with an emphasis on the aspects important for solid spectra. The following chapters discuss the theoretical background and applications of specific 2D solid state experiments. An application of 2D-J resolved NMR, analogous to J-resolved spectroscopy in solutions, to natural rubber is given in chapter 3. In chapter 4 the anisotropic chemical shift is mapped out against the heteronuclear dipolar interaction to obtain information about the orientation of the shielding tensor in poly-(oxymethylene). Chapter 5 concentrates on the study of super-slow molecular motions in polymers using a variant of the 2D exchange experiment developed by us. Finally chapter 6 discusses a new experiment, 2D nutation NMR, which makes it possible to study the quadrupole interaction of half-integer spins. 230 refs.; 48 figs.; 8 tabs

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

International Nuclear Information System (INIS)

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

2010-01-01

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

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

International Nuclear Information System (INIS)

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

1990-01-01

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

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

KAUST Repository

Zhang, Xiaoming

2016-03-16

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

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

KAUST Repository

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

2016-01-01

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

On the Nodal Lines of Eisenstein Series on Schottky Surfaces

Science.gov (United States)

Jakobson, Dmitry; Naud, Frédéric

2017-04-01

On convex co-compact hyperbolic surfaces {X=Γ backslash H2}, we investigate the behavior of nodal curves of real valued Eisenstein series {F_λ(z,ξ)}, where {λ} is the spectral parameter, {ξ} the direction at infinity. Eisenstein series are (non-{L^2}) eigenfunctions of the Laplacian {Δ_X} satisfying {Δ_X F_λ=(1/4+λ^2)F_λ}. As {λ} goes to infinity (the high energy limit), we show that, for generic {ξ}, the number of intersections of nodal lines with any compact segment of geodesic grows like {λ}, up to multiplicative constants. Applications to the number of nodal domains inside the convex core of the surface are then derived.

{sup 103}Rh NMR investigation of the superconductor Rh{sub 17}S{sub 15}

Energy Technology Data Exchange (ETDEWEB)

Koyama, T., E-mail: t-koyama@sci.u-hyogo.ac.j [Graduate School of Material Science, University of Hyogo, Kamigori, Hyogo 678-1297 (Japan); Kanda, K.; Motoyama, G.; Ueda, K.; Mito, T.; Kohara, T. [Graduate School of Material Science, University of Hyogo, Kamigori, Hyogo 678-1297 (Japan); Nakamura, H. [Department of Materials Science and Engineering, Kyoto University, Kyoto 606-8501 (Japan)

2010-12-15

We present {sup 103}Rh NMR studies for the superconductor Rh{sub 17}S{sub 15} (T{sub c} 5.4 K). We have identified the observed NMR lines corresponding to four different Rh sites in the cubic unit cell and deduced the temperature (T) dependence of the Knight shift components in Rh 24m site whose point symmetry is not axial. The isotropic part of the Knight shift K decreases with T in the normal state, indicating the negative hyperfine coupling and the enhancement of the spin susceptibility at lower T. The sudden change of K below T{sub c} is an indication of the spin-singlet Cooper paring.

Recent Advances in Characterization of Lignin Polymer by Solution-State Nuclear Magnetic Resonance (NMR Methodology

Directory of Open Access Journals (Sweden)

Run-Cang Sun

2013-01-01

Full Text Available The demand for efficient utilization of biomass induces a detailed analysis of the fundamental chemical structures of biomass, especially the complex structures of lignin polymers, which have long been recognized for their negative impact on biorefinery. Traditionally, it has been attempted to reveal the complicated and heterogeneous structure of lignin by a series of chemical analyses, such as thioacidolysis (TA, nitrobenzene oxidation (NBO, and derivatization followed by reductive cleavage (DFRC. Recent advances in nuclear magnetic resonance (NMR technology undoubtedly have made solution-state NMR become the most widely used technique in structural characterization of lignin due to its versatility in illustrating structural features and structural transformations of lignin polymers. As one of the most promising diagnostic tools, NMR provides unambiguous evidence for specific structures as well as quantitative structural information. The recent advances in two-dimensional solution-state NMR techniques for structural analysis of lignin in isolated and whole cell wall states (in situ, as well as their applications are reviewed.

Functional studies using NMR

International Nuclear Information System (INIS)

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

1986-01-01

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

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

CERN Document Server

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

2003-01-01

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

Symmetry Breaking in NMR Spectroscopy: The Elucidation of Hidden Molecular Rearrangement Processes

Directory of Open Access Journals (Sweden)

Michael J. McGlinchey

2014-08-01

Full Text Available Variable-temperature NMR spectroscopy is probably the most convenient and sensitive technique to monitor changes in molecular structure in solution. Rearrangements that are rapid on the NMR time-scale exhibit simplified spectra, whereby non-equivalent nuclear environments yield time-averaged resonances. At lower temperatures, when the rate of exchange is sufficiently reduced, these degeneracies are split and the underlying “static” molecular symmetry, as seen by X-ray crystallography, becomes apparent. Frequently, however, such rearrangement processes are hidden, even when they become slow on the NMR time-scale, because the molecular point group remains unchanged. Judicious symmetry breaking, such as by substitution of a molecular fragment by a similar, but not identical moiety, or by the incorporation of potentially diastereotopic (chemically non-equivalent nuclei, allows the elucidation of the kinetics and energetics of such processes. Examples are chosen that include a wide range of rotations, migrations and other rearrangements in organic, inorganic and organometallic chemistry.

Flow-through lipid nanotube arrays for structure-function studies of membrane proteins by solid-state NMR spectroscopy.

Science.gov (United States)

Chekmenev, Eduard Y; Gor'kov, Peter L; Cross, Timothy A; Alaouie, Ali M; Smirnov, Alex I

2006-10-15

A novel method for studying membrane proteins in a native lipid bilayer environment by solid-state NMR spectroscopy is described and tested. Anodic aluminum oxide (AAO) substrates with flow-through 175 nm wide and 60-mum-long nanopores were employed to form macroscopically aligned peptide-containing lipid bilayers that are fluid and highly hydrated. We demonstrate that the surfaces of both leaflets of such bilayers are fully accessible to aqueous solutes. Thus, high hydration levels as well as pH and desirable ion and/or drug concentrations could be easily maintained and modified as desired in a series of experiments with the same sample. The method allows for membrane protein NMR experiments in a broad pH range that could be extended to as low as 1 and as high as 12 units for a period of up to a few hours and temperatures as high as 70 degrees C without losing the lipid alignment or bilayers from the nanopores. We demonstrate the utility of this method by a solid-state 19.6 T (17)O NMR study of reversible binding effects of mono- and divalent ions on the chemical shift properties of the Leu(10) carbonyl oxygen of transmembrane pore-forming peptide gramicidin A (gA). We further compare the (17)O shifts induced by binding metal ions to the binding of protons in the pH range from 1 to 12 and find a significant difference. This unexpected result points to a difference in mechanisms for ion and proton conduction by the gA pore. We believe that a large number of solid-state NMR-based studies, including structure-function, drug screening, proton exchange, pH, and other titration experiments, will benefit significantly from the method described here.

NMR study of Y2(Co1-xFex)14B compounds

International Nuclear Information System (INIS)

Maruyama, F.; Ichinose, K.; Nagai, H.; Adachi, K.; Misawa, M.; Tsujimura, A.

1992-01-01

59 Co and 89 Y NMR of Y 2 (Co 1-x Fe x ) 14 B compounds has been measured at 4.2 K. The line positions shift rapidly to higher frequency for x≤0.3 and are almost constant for 0.3 1 and 8j 2 sites give a large contribution to the anisotropy of the 3d sublattice. (orig.)

NMR study of CeTe at low temperatures

Energy Technology Data Exchange (ETDEWEB)

Hinderer, J. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland)]. E-mail: hinderer@phys.ethz.ch; Weyeneth, S.M. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland); Weller, M. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland); Gavilano, J.L. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland); Felder, E. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland); Hulliger, F. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland); Ott, H.R. [Laboratorium fuer Festkoerperphysik, ETH Zuerich, CH-8093 Zurich (Switzerland)

2006-05-01

We present {sup 125}Te NMR measurements on CeTe powder at temperatures between 1 and 150K and in magnetic fields between 5 and 8T. CeTe is a rocksalt-type intermetallic compound. It orders antiferromagnetically at T{sub N}{approx}2.2K with a much reduced ordered moment [H.R. Ott, J.K. Kjems, F. Hulliger, Phys. Rev. Lett. 42 20 (1979) 1378]. From our low-temperature NMR spectra we infer the presence of at least three inequivalent Te sites at low temperatures. Considering the crystal structure this result is completely unexpected. The linewidths and the Knight shifts of the individual lines are significantly different and increase substantially with decreasing temperature. They follow the temperature dependence of the magnetic susceptibility above 20K. Above T{sub N}, hyperfine fields of 1.6, 0.8 and 0.0T at the three Te sites per Bohr magneton of Ce moment are deduced from Knight shift vs. magnetic susceptibility data. These values are typical for transferred hyperfine fields via conduction electrons.

A global analysis of NMR distance constraints from the PDB

International Nuclear Information System (INIS)

Vranken, Wim

2007-01-01

Information obtained from Nuclear Magnetic Resonance (NMR) experiments is encoded as a set of constraint lists when calculating three-dimensional structures for a protein. With the amount of constraint data from the world wide Protein Data Bank (wwPDB) that is now available, it is possible to do a global, large-scale analysis using only information from the constraints, without taking the coordinate information into account. This article describes such an analysis of distance constraints from NOE data based on a set of 1834 NMR PDB entries containing 1909 protein chains. In order to best represent the quality and extent of the data that is currently deposited at the wwPDB, only the original data as deposited by the authors was used, and no attempt was made to 'clean up' and further interpret this information. Because the constraint lists provide a single set of data, and not an ensemble of structural solutions, they are easier to analyse and provide a reduced form of structural information that is relevant for NMR analysis only. The online resource resulting from this analysis makes it possible to check, for example, how often a particular contact occurs when assigning NOESY spectra, or to find out whether a particular sequence fragment is likely to be difficult to assign. In this respect it formalises information that scientists with experience in spectrum analysis are aware of but cannot necessarily quantify. The analysis described here illustrates the importance of depositing constraints (and all other possible NMR derived information) along with the structure coordinates, as this type of information can greatly assist the NMR community

15N and 31P solid-state NMR study of transmembrane domain alignment of M2 protein of influenza A virus in hydrated cylindrical lipid bilayers confined to anodic aluminum oxide nanopores.

Science.gov (United States)

Chekmenev, Eduard Y; Hu, Jun; Gor'kov, Peter L; Brey, William W; Cross, Timothy A; Ruuge, Andres; Smirnov, Alex I

2005-04-01

This communication reports the first example of a high resolution solid-state 15N 2D PISEMA NMR spectrum of a transmembrane peptide aligned using hydrated cylindrical lipid bilayers formed inside nanoporous anodic aluminum oxide (AAO) substrates. The transmembrane domain SSDPLVVA(A-15N)SIIGILHLILWILDRL of M2 protein from influenza A virus was reconstituted in hydrated 1,2-dimyristoyl-sn-glycero-3-phosphatidylcholine bilayers that were macroscopically aligned by a conventional micro slide glass support or by the AAO nanoporous substrate. 15N and 31P NMR spectra demonstrate that both the phospholipids and the protein transmembrane domain are uniformly aligned in the nanopores. Importantly, nanoporous AAO substrates may offer several advantages for membrane protein alignment in solid-state NMR studies compared to conventional methods. Specifically, higher thermal conductivity of aluminum oxide is expected to suppress thermal gradients associated with inhomogeneous radio frequency heating. Another important advantage of the nanoporous AAO substrate is its excellent accessibility to the bilayer surface for exposure to solute molecules. Such high accessibility achieved through the substrate nanochannel network could facilitate a wide range of structure-function studies of membrane proteins by solid-state NMR.

Wide-Baseline Stereo-Based Obstacle Mapping for Unmanned Surface Vehicles

Science.gov (United States)

Mou, Xiaozheng; Wang, Han

2018-01-01

This paper proposes a wide-baseline stereo-based static obstacle mapping approach for unmanned surface vehicles (USVs). The proposed approach eliminates the complicated calibration work and the bulky rig in our previous binocular stereo system, and raises the ranging ability from 500 to 1000 m with a even larger baseline obtained from the motion of USVs. Integrating a monocular camera with GPS and compass information in this proposed system, the world locations of the detected static obstacles are reconstructed while the USV is traveling, and an obstacle map is then built. To achieve more accurate and robust performance, multiple pairs of frames are leveraged to synthesize the final reconstruction results in a weighting model. Experimental results based on our own dataset demonstrate the high efficiency of our system. To the best of our knowledge, we are the first to address the task of wide-baseline stereo-based obstacle mapping in a maritime environment. PMID:29617293

Development of real-time measurement of methanol-concentration in polymer electrolyte membrane using a local NMR sensor

International Nuclear Information System (INIS)

Ogawa, Kuniyasu; Ito, Kohei; Haishi, Tomoyuki

2007-01-01

A real-time sensor to measure methanol concentration in polymer electrolyte membrane (PEM) was developed for reducing methanol cross-over in Direct Methanol Fuel Cell (DMFC). The principle of the methanol sensor is based on the chemical shift of CH and OH species under high magnetic field. The sensor consists of a planar surface coil of 1.3 mm outside diameter. NMR signal from PEM being exposed to CH3OH solvent was measured using NMR sensor. Time-dependence changes of methanol concentration in PEM were obtained from analyzing spectrum of NMR signal. (author)

Recent Advances in Targeted and Untargeted Metabolomics by NMR and MS/NMR Methods

Energy Technology Data Exchange (ETDEWEB)

Bingol, Kerem

2018-04-18

Metabolomics has made significant progress in multiple fronts in the last 18 months. This minireview aimed to give an overview of these advancements in the light of their contribution to targeted and untargeted metabolomics. New computational approaches have emerged to overcome manual absolute quantitation step of metabolites in 1D 1H NMR spectra. This provides more consistency between inter-laboratory comparisons. Integration of 2D NMR metabolomics databases under a unified web server allowed very accurate identification of the metabolites that have been catalogued in these databases. For the remaining uncatalogued and unknown metabolites, new cheminformatics approaches have been developed by combining NMR and mass spectrometry. These hybrid NMR/MS approaches accelerated the identification of unknowns in untargeted studies, and now they are allowing to profile ever larger number of metabolites in application studies.

Fluorine dynamics in BaF2 superionic conductors investigated by NMR

International Nuclear Information System (INIS)

Gumann, Patryk

2008-01-01

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

Characterizing Surfaces of the Wide Bandgap Semiconductor Ilmenite with Scanning Probe Microcopies

Science.gov (United States)

Wilkins, R.; Powell, Kirk St. A.

1997-01-01

Ilmenite (FeTiO3) is a wide bandgap semiconductor with an energy gap of about 2.5eV. Initial radiation studies indicate that ilmenite has properties suited for radiation tolerant applications, as well as a variety of other electronic applications. Two scanning probe microscopy methods have been used to characterize the surface of samples taken from Czochralski grown single crystals. The two methods, atomic force microscopy (AFM) and scanning tunneling microscopy (STM), are based on different physical principles and therefore provide different information about the samples. AFM provides a direct, three-dimensional image of the surface of the samples, while STM give a convolution of topographic and electronic properties of the surface. We will discuss the differences between the methods and present preliminary data of each method for ilmenite samples.

Exploring inclusion complexes of ionic liquids with α- and β- cyclodextrin by NMR, IR, mass, density, viscosity, surface tension and conductance study

Science.gov (United States)

Barman, Biraj Kumar; Rajbanshi, Biplab; Yasmin, Ananya; Roy, Mahendra Nath

2018-05-01

The formation of the host-guest inclusion complexes of ionic liquids namely [BMIm]Cl and [HMIm]Cl with α-CD and β-CD were studied by means of physicochemical and spectroscopic methods. Conductivity and surface tension study were in good agreement with the 1H NMR and FT-IR studies which confirm the formation of the inclusion complexes. The Density and viscosity study also supported the formation of the ICs. Further the stoichiometry was determined 1:1 for each case and the association constants and thermodynamic parameters derived supported the most feasible formation of the [BMIm]Cl- β-CD inclusion complex.

A Cassie-Like Law Using Triple Phase Boundary Line Fractions for Faceted Droplets on Chemically Heterogeneous Surfaces

DEFF Research Database (Denmark)

Larsen, Simon Tylsgaard; Taboryski, Rafael Jozef

2009-01-01

We present experimental contact angle data for surfaces, which were surface-engineered with a hydrophobic micropattern of hexagonal geometry. The chemically heterogeneous surface of the same hexagonal pattern of defects resulted in faceted droplets of hexagonal shape. When measuring the advancing...... contact angles with a viewing position aligned parallel to rows of defects, we found that an area averaged Cassie-law failed in describing the data. By replacing the area fractions by line fractions of the triple phase boundary Line segments in the Cassie equation, we found excellent agreement with data....

NMR-based milk metabolomics

DEFF Research Database (Denmark)

Sundekilde, Ulrik; Larsen, Lotte Bach; Bertram, Hanne Christine S.

2013-01-01

and processing capabilities of bovine milk is closely associated to milk composition. Metabolomics is ideal in the study of the low-molecular-weight compounds in milk, and this review focuses on the recent nuclear magnetic resonance (NMR)-based metabolomics trends in milk research, including applications linking...... compounds. Furthermore, metabolomics applications elucidating how the differential regulated genes affects milk composition are also reported. This review will highlight the recent advances in NMR-based metabolomics on milk, as well as give a brief summary of when NMR spectroscopy can be useful for gaining...

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-04-15

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

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

Science.gov (United States)

Paik, Younkee

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

NMR imaging of cerebral infarction

International Nuclear Information System (INIS)

Takusagawa, Yoshihiko; Yamaoka, Naoki; Doi, Kazuaki; Okada, Keisei

1987-01-01

One hundred and five patients with cerebral infarction were studied by nuclear magnetic resonance (NMR) CT (resistive type of magnet with strength of 0.1 tesla) and X-ray CT. Pulse sequences used saturation recovery (Tr = 600 mSec), Inversion recovery (Tr = 500 mSec, Td = 300 mSec) and spin echo (Tr = 1500 mSec, Te = 40, 80, 120, 160 mSec). Fifteen cases were examined by NMR-CT within 24 hours from onset. Proton NMR imaging could not detect cerebral ischemia as early as 2 hours after onset, but except could detect the lesions in Se image the area of cerebral infarct 3 hours after onset. After 5 hours from onset image changes in SE were evident and corresponded to the area of cerebral infarct, but image changes in IR could not fully delineate the infarcted area. NMR images of 41 year-old woman with cerebral embolism by MCA trunck occlusion associated with mitral stenosis were presented, and NMR-CT was examined 10 hours, 9th and 43th days after episode of MCA occlusion. Sixty patents (64 times) with lacunar infarction were studied by NMR-CT and X-ray CT. The inversion recovery images were used mainly for detection of lesions and comparison with X-ray CT. In 160 lesions which were detected by NMR-CT or X-ray CT, could 156 lesions be detected by NMR-CT and 78 lesions by X-ray CT. Inversion recovery images were more useful for detection of lacunes than X-ray CT. Calculated T1 and T2 values prolonged with time course from onset. (author)

Multinuclear NMR studies of single lipid bilayers supported in cylindrical aluminum oxide nanopores.

Science.gov (United States)

Gaede, Holly C; Luckett, Keith M; Polozov, Ivan V; Gawrisch, Klaus

2004-08-31

Lipid bilayers were deposited inside the 0.2 microm pores of anodic aluminum oxide (AAO) filters by extrusion of multilamellar liposomes and their properties studied by 2H, 31P, and 1H solid-state NMR. Only the first bilayer adhered strongly to the inner surface of the pores. Additional layers were washed out easily by a flow of water as demonstrated by 1H magic angle spinning NMR experiments with addition of Pr3+ ions to shift accessible lipid headgroup resonances. A 13 mm diameter Anopore filter of 60 microm thickness oriented approximately 2.5 x 10(-7) mol of lipid as a single bilayer, corresponding to a total membrane area of about 500 cm2. The 2H NMR spectra of chain deuterated POPC are consistent with adsorption of wavy, tubular bilayers to the inner pore surface. By NMR diffusion experiments, we determined the average length of those lipid tubules to be approximately 0.4 microm. There is evidence for a thick water layer between lipid tubules and the pore surface. The ends of tubules are well sealed against the pore such that Pr3+ ions cannot penetrate into the water underneath the bilayers. We successfully trapped poly(ethylene glycol) (PEG) with a molecular weight of 8000 in this water layer. From the quantity of trapped PEG, we calculated an average water layer thickness of 3 nm. Lipid order parameters and motional properties are unperturbed by the solid support, in agreement with existence of a water layer. Such unperturbed, solid supported membranes are ideal for incorporation of membrane-spanning proteins with large intra- and extracellular domains. The experiments suggest the promise of such porous filters as membrane support in biosensors.

Probing hot-electron effects in wide area plasmonic surfaces using X-ray photoelectron spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Ayas, Sencer; Cupallari, Andi; Dana, Aykutlu, E-mail: aykutlu@unam.bilkent.edu.tr [UNAM Institute of Materials Science and Nanotechnology, Bilkent University, 06800 Ankara (Turkey)

2014-12-01

Plasmon enhanced hot carrier formation in metallic nanostructures increasingly attracts attention due to potential applications in photodetection, photocatalysis, and solar energy conversion. Here, hot-electron effects in nanoscale metal-insulator-metal (MIM) structures are investigated using a non-contact X-ray photoelectron spectroscopy based technique using continuous wave X-ray and laser excitations. The effects are observed through shifts of the binding energy of the top metal layer upon excitation with lasers of 445, 532, and 650 nm wavelength. The shifts are polarization dependent for plasmonic MIM grating structures fabricated by electron beam lithography. Wide area plasmonic MIM surfaces fabricated using a lithography free route by the dewetting of evaporated Ag on HfO{sub 2} exhibit polarization independent optical absorption and surface photovoltage. Using a simple model and making several assumptions about the magnitude of the photoemission current, the responsivity and external quantum efficiency of wide area plasmonic MIM surfaces are estimated as 500 nA/W and 11 × 10{sup −6} for 445 nm illumination.

Comparison of multiple crystal structures with NMR data for engrailed homeodomain

Energy Technology Data Exchange (ETDEWEB)

Religa, Tomasz L. [MRC Centre for Protein Engineering (United Kingdom)], E-mail: tlr25@mrc-lmb.cam.ac.uk

2008-03-15

Two methods are currently available to solve high resolution protein structures-X-ray crystallography and nuclear magnetic resonance (NMR). Both methods usually produce highly similar structures, but small differences between both solutions are always observed. Here the raw NMR data as well as the solved NMR structure were compared to the multiple crystal structures solved for the WT 60 residue three helix bundle engrailed homeodomain (EnHD) and single point mutants. There was excellent agreement between TALOS-predicted and crystal structure-observed dihedral angles and a good agreement for the {sup 3}J(H{sup N}H{sup {alpha}}) couplings for the multiple crystal structures. Around 1% of NOEs were violated for any crystal structure, but no NOE was inconsistent with all of the crystal structures. Violations usually occurred for surface residues or for residues for which multiple discreet conformations were observed between the crystal structures. Comparison of the disorder shown in the multiple crystal structures shows little correlation with dynamics under native conditions for this protein.

β-NMR sample optimization

CERN Document Server

Zakoucka, Eva

2013-01-01

During my summer student programme I was working on sample optimization for a new β-NMR project at the ISOLDE facility. The β-NMR technique is well-established in solid-state physics and just recently it is being introduced for applications in biochemistry and life sciences. The β-NMR collaboration will be applying for beam time to the INTC committee in September for three nuclei: Cu, Zn and Mg. Sample optimization for Mg was already performed last year during the summer student programme. Therefore sample optimization for Cu and Zn had to be completed as well for the project proposal. My part in the project was to perform thorough literature research on techniques studying Cu and Zn complexes in native conditions, search for relevant binding candidates for Cu and Zn applicable for ß-NMR and eventually evaluate selected binding candidates using UV-VIS spectrometry.

Low field NMR surface relaxivity studies of chalk and argillaceous sandstones

DEFF Research Database (Denmark)

Katika, Konstantina; Fordsmand, Henrik; Fabricius, Ida Lykke

2017-01-01

the accuracy of predictions of petrophysical properties of various rocks with the use of NMR spectrometry. We perform laboratory transverse relaxation (T2) measurements on water saturated Gorm field chalk, Stevns Klint chalk, Solsort field greensand and Berea sandstone. These rocks are of particular interest...... field chalk and Solsort field greensand have higher ρ at higher Larmor frequency. By contrast, ρ of the purely calcitic Stevns chalk and quartzitic Berea sandstone proved not to be affected by the changes in frequency. T2 distributions at temperatures ranging from 10 °C to 60 °C provided comparison...

Unraveling the meaning of chemical shifts in protein NMR.

Science.gov (United States)

Berjanskii, Mark V; Wishart, David S

2017-11-01

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

Microprocessorized NMR measurement

International Nuclear Information System (INIS)

Rijllart, A.

1984-01-01

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

Two superconducting phases in CePt{sub 3}Si confirmed by NMR

Energy Technology Data Exchange (ETDEWEB)

Ueda, Koh-ichi; Motoyama, Gaku; Kohara, Takao, E-mail: ueda@sci.u-hyogo.ac.j [Graduate School of Material Science, University of Hyogo, Kamigori-cho, Ako-gun, Hyogo 678-1297 (Japan)

2009-03-01

Recent specific heat experiments in CePt{sub 3}Si of good quality gave an evidence of coexistence of two phases, which have distinct T{sub c} and T{sub n} for each phase. NMR spectrum of {sup 29}Si also showed a complicated line shape due to a co-existence of two phases below T{sub n}. One phase is an ordinary AF state and the other is a paramagnetic like phase, in which the internal field is somewhat small. The AF internal field deduced by NMR is expected to be parallel to the c-axis at Si site. With decreasing temperature below T{sub c}, 1/T{sub 1} measured at the satellite peak decreased rapidly followed by T{sup 3} with no enhancement just below T{sub c}.

Fourier transform n.m.r. spectroscopy

International Nuclear Information System (INIS)

Shaw, D.

1976-01-01

This book is orientated to techniques rather than applications. The basic theory of n.m.r. is dealt with in a unified approach to the Fourier theory. The middle section of the book concentrates on the practical aspects of Fourier n.m.r., both instrumental and experimental. The final chapters briefly cover general application of n.m.r., but concentrate strongly on those areas where Fourier n.m.r. can give information which is not available by conventional techniques

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

CERN Document Server

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

2000-01-01

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

Fundamentals of Protein NMR Spectroscopy

CERN Document Server

Rule, Gordon S

2006-01-01

NMR spectroscopy has proven to be a powerful technique to study the structure and dynamics of biological macromolecules. Fundamentals of Protein NMR Spectroscopy is a comprehensive textbook that guides the reader from a basic understanding of the phenomenological properties of magnetic resonance to the application and interpretation of modern multi-dimensional NMR experiments on 15N/13C-labeled proteins. Beginning with elementary quantum mechanics, a set of practical rules is presented and used to describe many commonly employed multi-dimensional, multi-nuclear NMR pulse sequences. A modular analysis of NMR pulse sequence building blocks also provides a basis for understanding and developing novel pulse programs. This text not only covers topics from chemical shift assignment to protein structure refinement, as well as the analysis of protein dynamics and chemical kinetics, but also provides a practical guide to many aspects of modern spectrometer hardware, sample preparation, experimental set-up, and data pr...

Permeability in Rotliegend gas sandstones to gas and brine as predicted from NMR, mercury injection and image analysis

DEFF Research Database (Denmark)

Rosenbrand, Esther; Fabricius, Ida Lykke; Fisher, Quentin

2015-01-01

Permeability characterisation of low permeability, clay-rich gas sandstones is part of production forecasting and reservoir management. The physically based Kozeny (1927) equation linking permeability with porosity and pore size is derived for a porous medium with a homogeneous pore size, whereas...... the pore sizes in tight sandstones can range from nm to μm. Nuclear magnetic resonance (NMR) transverse relaxation was used to estimate a pore size distribution for 63 samples of Rotliegend sandstone. The surface relaxation parameter required to relate NMR to pore size is estimated by combination of NMR...

NMR-based metabolomics of mammalian cell and tissue cultures

International Nuclear Information System (INIS)

Aranibar, Nelly; Borys, Michael; Mackin, Nancy A.; Ly, Van; Abu-Absi, Nicholas; Abu-Absi, Susan; Niemitz, Matthias; Schilling, Bernhard; Li, Zheng Jian; Brock, Barry; Russell, Reb J.; Tymiak, Adrienne; Reily, Michael D.

2011-01-01

NMR spectroscopy was used to evaluate growth media and the cellular metabolome in two systems of interest to biomedical research. The first of these was a Chinese hamster ovary cell line engineered to express a recombinant protein. Here, NMR spectroscopy and a quantum mechanical total line shape analysis were utilized to quantify 30 metabolites such as amino acids, Krebs cycle intermediates, activated sugars, cofactors, and others in both media and cell extracts. The impact of bioreactor scale and addition of anti-apoptotic agents to the media on the extracellular and intracellular metabolome indicated changes in metabolic pathways of energy utilization. These results shed light into culture parameters that can be manipulated to optimize growth and protein production. Second, metabolomic analysis was performed on the superfusion media in a common model used for drug metabolism and toxicology studies, in vitro liver slices. In this study, it is demonstrated that two of the 48 standard media components, choline and histidine are depleted at a faster rate than many other nutrients. Augmenting the starting media with extra choline and histidine improves the long-term liver slice viability as measured by higher tissues levels of lactate dehydrogenase (LDH), glutathione and ATP, as well as lower LDH levels in the media at time points out to 94 h after initiation of incubation. In both models, media components and cellular metabolites are measured over time and correlated with currently accepted endpoint measures.

NMR-based metabolomics of mammalian cell and tissue cultures

Energy Technology Data Exchange (ETDEWEB)

Aranibar, Nelly; Borys, Michael; Mackin, Nancy A.; Ly, Van; Abu-Absi, Nicholas; Abu-Absi, Susan [Bristol-Myers Squibb Company (United States); Niemitz, Matthias [PERCH Solutions Ltd. (Finland); Schilling, Bernhard; Li, Zheng Jian; Brock, Barry; Russell, Reb J.; Tymiak, Adrienne; Reily, Michael D., E-mail: michael.reily@bms.com [Bristol-Myers Squibb Company (United States)

2011-04-15

NMR spectroscopy was used to evaluate growth media and the cellular metabolome in two systems of interest to biomedical research. The first of these was a Chinese hamster ovary cell line engineered to express a recombinant protein. Here, NMR spectroscopy and a quantum mechanical total line shape analysis were utilized to quantify 30 metabolites such as amino acids, Krebs cycle intermediates, activated sugars, cofactors, and others in both media and cell extracts. The impact of bioreactor scale and addition of anti-apoptotic agents to the media on the extracellular and intracellular metabolome indicated changes in metabolic pathways of energy utilization. These results shed light into culture parameters that can be manipulated to optimize growth and protein production. Second, metabolomic analysis was performed on the superfusion media in a common model used for drug metabolism and toxicology studies, in vitro liver slices. In this study, it is demonstrated that two of the 48 standard media components, choline and histidine are depleted at a faster rate than many other nutrients. Augmenting the starting media with extra choline and histidine improves the long-term liver slice viability as measured by higher tissues levels of lactate dehydrogenase (LDH), glutathione and ATP, as well as lower LDH levels in the media at time points out to 94 h after initiation of incubation. In both models, media components and cellular metabolites are measured over time and correlated with currently accepted endpoint measures.

A Finite Element Method for Free-Surface Flows of Incompressible Fluids in Three Dimensions, Part II: Dynamic Wetting Lines

Energy Technology Data Exchange (ETDEWEB)

Baer, T.A.; Cairncross, R.A.; Rao, R.R.; Sackinger, P.A.; Schunk, P.R.

1999-01-29

To date, few researchers have solved three-dimensional free-surface problems with dynamic wetting lines. This paper extends the free-surface finite element method described in a companion paper [Cairncross, R.A., P.R. Schunk, T.A. Baer, P.A. Sackinger, R.R. Rao, "A finite element method for free surface flows of incompressible fluid in three dimensions, Part I: Boundary-Fitted mesh motion.", to be published (1998)] to handle dynamic wetting. A generalization of the technique used in two dimensional modeling to circumvent double-valued velocities at the wetting line, the so-called kinematic paradox, is presented for a wetting line in three dimensions. This approach requires the fluid velocity normal to the contact line to be zero, the fluid velocity tangent to the contact line to be equal to the tangential component of web velocity, and the fluid velocity into the web to be zero. In addition, slip is allowed in a narrow strip along the substrate surface near the dynamic contact line. For realistic wetting-line motion, a contact angle which varies with wetting speed is required because contact lines in three dimensions typically advance or recede a different rates depending upon location and/or have both advancing and receding portions. The theory is applied to capillary rise of static fluid in a corner, the initial motion of a Newtonian droplet down an inclined plane, and extrusion of a Newtonian fluid from a nozzle onto a moving substrate. The extrusion results are compared to experimental visualization. Subject Categories

NMR Detection of Semi-Specific Antibody Interactions in Serum Environments

Directory of Open Access Journals (Sweden)

Saeko Yanaka

2017-09-01

Full Text Available Although antibody functions are executed in heterogeneous blood streams characterized by molecular crowding and promiscuous intermolecular interaction, detailed structural characterizations of antibody interactions have thus far been performed under homogeneous in vitro conditions. NMR spectroscopy potentially has the ability to study protein structures in heterogeneous environments, assuming that the target protein can be labeled with NMR-active isotopes. Based on our successful development of isotope labeling of antibody glycoproteins, here we apply NMR spectroscopy to characterize antibody interactions in heterogeneous extracellular environments using mouse IgG-Fc as a test molecule. In human serum, many of the HSQC peaks originating from the Fc backbone exhibited attenuation in intensity of various magnitudes. Similar spectral changes were induced by the Fab fragment of polyclonal IgG isolated from the serum, but not by serum albumin, indicating that a subset of antibodies reactive with mouse IgG-Fc exists in human serum without preimmunization. The metaepitopes recognized by serum polyclonal IgG cover the entire molecular surface of Fc, including the binding sites to Fc receptors and C1q. In-serum NMR observation will offer useful tools for the detailed characterization of biopharamaceuticals, including therapeutic antibodies in physiologically relevant heterogeneous environments, also giving deeper insight into molecular recognition by polyclonal antibodies in the immune system.

Functional studies using NMR

International Nuclear Information System (INIS)

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

1987-01-01

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

The xGa{sub 2}O{sub 3}–(100 − x)NaPO{sub 3} glass system: Preparation, properties and structural analysis by solid state NMR

Energy Technology Data Exchange (ETDEWEB)

Caron, A. [UCCS UMR-CNRS 8181, Université de Lille1, Villeneuve d' Ascq (France); Doumert, B. [IMMCL, Université de Lille1, Villeneuve d' Ascq (France); Tricot, G., E-mail: gregory.tricot@univ-lille1.fr [UCCS UMR-CNRS 8181, Université de Lille1, Villeneuve d' Ascq (France); LASIR UMR-CNRS 8516, Université de Lille1, Villeneuve d' Ascq (France)

2014-10-15

Insertion of Ga{sub 2}O{sub 3} in sodium metaphosphate glasses has been investigated in this paper. Materials containing up to 30 mol% of Ga{sub 2}O{sub 3} have been prepared using the standard melt-quenching technique within the xGa{sub 2}O{sub 3}–(100 − x)NaPO{sub 3} composition line. Macroscopic properties (glass transition temperature, density and molar volume) are significantly affected by the Ga{sub 2}O{sub 3} insertion. 1D {sup 71}Ga and {sup 31}P magic angle spinning nuclear magnetic resonance (MAS-NMR) performed at very high field (18.8 T) indicate a strong evolution of the gallium coordination state around the x = 15 composition and a continuous evolution of the phosphate network organisation. In addition, {sup 71}Ga({sup 31}P) D-HMQC NMR technique was used for the first time to highlight the presence of mixed P–O–Ga linkages within the glass structure. The impact of gallium insertion is finally discussed and compared to the effect of the widely used aluminum and boron elements. If gallium and aluminum elements present similar effect on the macroscopic properties, some discrepancies can be observed concerning their structural effect. - Highlights: • Glasses with 30 mol% of Ga{sub 2}O{sub 3} have been prepared in the NaPO{sub 3}–Ga{sub 2}O{sub 3} line. • T{sub g} and density are affected by the Ga{sup 3+} insertion. • Presence of mixed Ga/P species have been highlighted by 2D correlation NMR.

Experimental Study of Thermo-hydraulic Characteristics of Surfaces with In-line Dimple Arrangement

Directory of Open Access Journals (Sweden)

S. A. Burtsev

2015-01-01

Full Text Available The paper presents a conducted experimental study of the heat exchange intensification on the surfaces covered with a regular vortex-generating relief that is an in-line array of the shallow hemispherical dimples. Using 12 configuration options with the Reynolds numbers in the range of (0.2-7.0 106 as an example, it analyses how a longitudinal and cross step of the in-line dimple array (density dimples effects on the processes of heat exchange intensification and resistance.The monocomponent strain-gauge balance allows us to define a value of the resistance coefficient by direct weighing of models (located in parallel in a flow of "relief" and smooth "reference" ones being under study. Distribution fields of heat – transfer factor are determined by recording a cooling process of the surface of studied models having high spatial and temporary resolution. All researches were conducted with one-shot data record of these thermal and hydraulic measurements for the smooth (reference surfaces and the studied surfaces covered with a regular vortex-generating relief (dimples. The error of determined parameters was no more than ±5%.The oil-sooty method allows us to visualize flow around a regular relief and obtain a flow pattern for 12 options of dimples configuration. The analysis has been carried out and a compliance of the flow patterns with the field of heat-transfer factors has been obtained.It has been found that for the in-line configuration a Reynolds analogy factor for most models is nonlinearly dependent on the Reynolds number. The friction intensification, at first, falls (to some Reynolds number and, further, starts increasing, tending to the friction intensification value with self-similarity flow around. Thus with increasing Reynolds number, the heattransfer factor intensification falls (more slowly than resistance intensification.

Analysis and Application of River Surface Line in Hilly Area based on Hec-ras Model

Directory of Open Access Journals (Sweden)

Yang Congshan

2017-01-01

Full Text Available For example—Cixian Fuyang River Regulation Project. Due to the character that Fuyang River is located in hilly areas of Cixian, we use the Hex-ras software to calculate the status of the river water surface line for the goal of determining the final treatment plan. We maintain the present situation of the river channel design as principle, select the most appropriate pushed water level and roughnessas the basic, and we combine the classification calculation of crossing structures of backwater and the encryption calculation section to get the more accurate result. We compare the water level elevation and the calculation of cross strait, analyze the design parameters, calculate repeated the water line section, analyze the rationality of the design plan, and then finally determine the applicability of Hex-rac software in the large continuous variation of cross section of embankment of river river surface line.

Combined In Situ Illumination-NMR-UV/Vis Spectroscopy: A New Mechanistic Tool in Photochemistry.

Science.gov (United States)

Seegerer, Andreas; Nitschke, Philipp; Gschwind, Ruth M

2018-06-18

Synthetic applications in photochemistry are booming. Despite great progress in the development of new reactions, mechanistic investigations are still challenging. Therefore, we present a fully automated in situ combination of NMR spectroscopy, UV/Vis spectroscopy, and illumination to allow simultaneous and time-resolved detection of paramagnetic and diamagnetic species. This optical fiber-based setup enables the first acquisition of combined UV/Vis and NMR spectra in photocatalysis, as demonstrated on a conPET process. Furthermore, the broad applicability of combined UVNMR spectroscopy for light-induced processes is demonstrated on a structural and quantitative analysis of a photoswitch, including rate modulation and stabilization of transient species by temperature variation. Owing to the flexibility regarding the NMR hardware, temperature, and light sources, we expect wide-ranging applications of this setup in various research fields. © 2018 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

NMR Study on the Inclusion Complexes of β-Cyclodextrin with Isoflavones

Directory of Open Access Journals (Sweden)

Rui Zhao

2016-03-01

Full Text Available The structure of the inclusion complexes of β-cyclodextrin (β-CD with daidzein and daidzin in D2O were investigated using NMR spectroscopy. For the β-CD and daidzein system, two types of 1:1 complexes were formed with the daidzein deeply inserted into the CD cavity with different orientations. For the β-CD/daidzin system, a 1:1 complex was formed with the flavonoid part of daidzin entering the CD cavity from the wide rim. The inclusion complexes determined by NMR were constructed using molecular docking. Furthermore, the mixture of puerarin, daidzein and daidzin, which are the major isoflavonoid components present in Radix puerariae, was analyzed by diffusion-ordered spectroscopy (DOSY alone and upon addition of β-CD in order to mimic chromatographic conditions and compare their binding affinities.

NMR in structure-based drug design.

Science.gov (United States)

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

2017-11-08

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

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

Energy Technology Data Exchange (ETDEWEB)

Gumann, Patryk

2008-07-01

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

NMR diffusion and relaxation measurements of organic molecules adsorbed in porous media

International Nuclear Information System (INIS)

Gjerdaaker, Lars

2002-01-01

a bipolar form of the pulsed field gradient has proved to be an efficient method for both reducing the cross-term between the applied and internal gradient and reducing the eddy current dead time. Without the use of a bipolar sequence, the measured diffusivities are likely to be underestimated. In order to get sufficient attenuation of the signal a stimulated-echo sequence together with magnetic field gradients have been used. It was then possible to increase the z-storage period to compensate for insufficient gradient strength. However, the employed diffusion probe and gradient power supply are able to generate magnetic field gradients that make the z-storage period unnecessary. In this work we also present a spin-echo analogue to the 13-interval PFGSTE sequence presented by Cotts et al., a so-called 11-interval bipolar PFGSE sequence. Conclusions: The molecular dynamics of four organic adsorbates confined in porous materials have been investigated. The confinement gives rise to substantial changes in the phase behaviour and molecular dynamics. From the line shape of the confined substances a narrow-line component superimposed on a broad resonance is observed at temperatures well below the transition point of the bulk material. This narrow-line component is, in the freezing region, attributed to the surface layer and the undercooled liquid in the smaller pores that remains unfrozen. In the low-temperature region, the narrow-line component corresponds to the surface layer, while the broad component originates from the crystalline phase at the centre of the pores. The persistent surface layer does not appear to crystallize at all, and a relatively high diffusion rate of this liquid-like phase is observed over a wide temperature range, even well below the transition point of the bulk material. However, with decreasing temperature T2 of the molecules in the surface layer becomes shorter and the contribution to the NMR signal decreases gradually. For pivalic acid and

Lectures on pulsed NMR

International Nuclear Information System (INIS)

Pines, A.

1986-09-01

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

Investigating the Dissolution Performance of Amorphous Solid Dispersions Using Magnetic Resonance Imaging and Proton NMR

Directory of Open Access Journals (Sweden)

Francesco Tres

2015-09-01

Full Text Available We have investigated the dissolution performance of amorphous solid dispersions of poorly water-soluble bicalutamide in a Kollidon VA64 polymeric matrix as a function of the drug loading (5% vs. 30% bicalutamide. A combined suite of state-of-the-art analytical techniques were employed to obtain a clear picture of the drug release, including an integrated magnetic resonance imaging UV-Vis flow cell system and 1H-NMR. Off-line 1H-NMR was used for the first time to simultaneously measure the dissolution profiles and rates of both the drug and the polymer from a solid dispersion. MRI and 1H-NMR data showed that the 5% drug loading compact erodes linearly, and that bicalutamide and Kollidon VA64 are released at approximately the same rate from the molecular dispersion. For the 30% extrudate, data indicated a slower water ingress into the compact which corresponds to a slower dissolution rate of both bicalutamide and Kollidon VA64.

Evaluation of surface nuclear magnetic resonance-estimated subsurface water content

International Nuclear Information System (INIS)

Mueller-Petke, M; Dlugosch, R; Yaramanci, U

2011-01-01

The technique of nuclear magnetic resonance (NMR) has found widespread use in geophysical applications for determining rock properties (e.g. porosity and permeability) and state variables (e.g. water content) or to distinguish between oil and water. NMR measurements are most commonly made in the laboratory and in boreholes. The technique of surface NMR (or magnetic resonance sounding (MRS)) also takes advantage of the NMR phenomenon, but by measuring subsurface rock properties from the surface using large coils of some tens of meters and reaching depths as much as 150 m. We give here a brief review of the current state of the art of forward modeling and inversion techniques. In laboratory NMR a calibration is used to convert measured signal amplitudes into water content. Surface NMR-measured amplitudes cannot be converted by a simple calibration. The water content is derived by comparing a measured amplitude with an amplitude calculated for a given subsurface water content model as input for a forward modeling that must account for all relevant physics. A convenient option to check whether the measured signals are reliable or the forward modeling accounts for all effects is to make measurements in a well-defined environment. Therefore, measurements on top of a frozen lake were made with the latest-generation surface NMR instruments. We found the measured amplitudes to be in agreement with the calculated amplitudes for a model of 100 % water content. Assuming then both the forward modeling and the measurement to be correct, the uncertainty of the model is calculated with only a few per cent based on the measurement uncertainty.

NMR spectroscopy using liquid crystal solvents

CERN Document Server

Emsley, JW

2013-01-01

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

NMR studies of isotopically labeled RNA

Energy Technology Data Exchange (ETDEWEB)

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

1994-12-01

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

1H-NMR, 1H-NMR T2-edited, and 2D-NMR in bipolar disorder metabolic profiling.

Science.gov (United States)

Sethi, Sumit; Pedrini, Mariana; Rizzo, Lucas B; Zeni-Graiff, Maiara; Mas, Caroline Dal; Cassinelli, Ana Cláudia; Noto, Mariane N; Asevedo, Elson; Cordeiro, Quirino; Pontes, João G M; Brasil, Antonio J M; Lacerda, Acioly; Hayashi, Mirian A F; Poppi, Ronei; Tasic, Ljubica; Brietzke, Elisa

2017-12-01

The objective of this study was to identify molecular alterations in the human blood serum related to bipolar disorder, using nuclear magnetic resonance (NMR) spectroscopy and chemometrics. Metabolomic profiling, employing 1 H-NMR, 1 H-NMR T 2 -edited, and 2D-NMR spectroscopy and chemometrics of human blood serum samples from patients with bipolar disorder (n = 26) compared with healthy volunteers (n = 50) was performed. The investigated groups presented distinct metabolic profiles, in which the main differential metabolites found in the serum sample of bipolar disorder patients compared with those from controls were lipids, lipid metabolism-related molecules (choline, myo-inositol), and some amino acids (N-acetyl-L-phenyl alanine, N-acetyl-L-aspartyl-L-glutamic acid, L-glutamine). In addition, amygdalin, α-ketoglutaric acid, and lipoamide, among other compounds, were also present or were significantly altered in the serum of bipolar disorder patients. The data presented herein suggest that some of these metabolites differentially distributed between the groups studied may be directly related to the bipolar disorder pathophysiology. The strategy employed here showed significant potential for exploring pathophysiological features and molecular pathways involved in bipolar disorder. Thus, our findings may contribute to pave the way for future studies aiming at identifying important potential biomarkers for bipolar disorder diagnosis or progression follow-up.

Lectures on pulsed NMR

International Nuclear Information System (INIS)

Pines, A.

1988-08-01

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

Resistively detected NMR line shapes in a quasi-one-dimensional electron system

Science.gov (United States)

Fauzi, M. H.; Singha, A.; Sahdan, M. F.; Takahashi, M.; Sato, K.; Nagase, K.; Muralidharan, B.; Hirayama, Y.

2017-06-01

We observe variation in the resistively detected nuclear magnetic resonance (RDNMR) line shapes in quantum Hall breakdown. The breakdown occurs locally in a gate-defined quantum point contact (QPC) region. Of particular interest is the observation of a dispersive line shape occurring when the bulk two-dimensional electron gas (2DEG) set to νb=2 and the QPC filling factor to the vicinity of νQPC=1 , strikingly resemble the dispersive line shape observed on a 2D quantum Hall state. This previously unobserved line shape in a QPC points to a simultaneous occurrence of two hyperfine-mediated spin flip-flop processes within the QPC. Those events give rise to two different sets of nuclei polarized in the opposite direction and positioned at a separate region with different degrees of electronic spin polarization.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

NMR metabolomics of thrips (Frankliniella occidentalis) resistance in Senecio hybrids.

Science.gov (United States)

Leiss, Kirsten A; Choi, Young H; Abdel-Farid, Ibrahim B; Verpoorte, Robert; Klinkhamer, Peter G L

2009-02-01

Western flower thrips (Frankliniella occidentalis) has become a key insect pest of agricultural and horticultural crops worldwide. Little is known about host plant resistance to thrips. In this study, we investigated thrips resistance in F (2) hybrids of Senecio jacobaea and Senecio aquaticus. We identified thrips-resistant hybrids applying three different bioassays. Subsequently, we compared the metabolomic profiles of these hybrids applying nuclear magnetic resonance spectroscopy (NMR). The new developments of NMR facilitate a wide range coverage of the metabolome. This makes NMR especially suitable if there is no a priori knowledge of the compounds related to herbivore resistance and allows a holistic approach analyzing different chemical compounds simultaneously. We show that the metabolomes of thrips-resistant and -susceptible hybrids differed considerably. Thrips-resistant hybrids contained higher amounts of the pyrrolizidine alkaloids (PA), jacobine, and jaconine, especially in younger leaves. Also, a flavanoid, kaempferol glucoside, accumulated in the resistant plants. Both PAs and kaempferol are known for their inhibitory effect on herbivores. In resistant and susceptible F (2) hybrids, young leaves showed less thrips damage than old leaves. Consistent with the optimal plant defense theory, young leaves contained increased levels of primary metabolites such as sucrose, raffinose, and stachyose, but also accumulated jacaranone as a secondary plant defense compound. Our results prove NMR as a promising tool to identify different metabolites involved in herbivore resistance. It constitutes a significant advance in the study of plant-insect relationships, providing key information on the implementation of herbivore resistance breeding strategies in plants.

Solid-state NMR basic principles and practice

CERN Document Server

Apperley, David C; Hodgkinson, Paul

2014-01-01

Nuclear Magnetic Resonance (NMR) has proved to be a uniquely powerful and versatile tool for analyzing and characterizing chemicals and materials of all kinds. This book focuses on the latest developments and applications for "solid-state" NMR, which has found new uses from archaeology to crystallography to biomaterials and pharmaceutical science research. The book will provide materials engineers, analytical chemists, and physicists, in and out of lab, a survey of the techniques and the essential tools of solid-state NMR, together with a practical guide on applications. In this concise introduction to the growing field of solid-state nuclear magnetic resonance spectroscopy The reader will find: * Basic NMR concepts for solids, including guidance on the spin-1/2 nuclei concept * Coverage of the quantum mechanics aspects of solid state NMR and an introduction to the concept of quadrupolar nuclei * An understanding relaxation, exchange and quantitation in NMR * An analysis and interpretation of NMR data, with e...

High resolution NMR theory and chemical applications

CERN Document Server

Becker, Edwin D

1999-01-01

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

Genome-wide nucleosome occupancy and DNA methylation profiling of four human cell lines

Directory of Open Access Journals (Sweden)

Aaron L. Statham

2015-03-01

Full Text Available DNA methylation and nucleosome positioning are two key mechanisms that contribute to the epigenetic control of gene expression. During carcinogenesis, the expression of many genes is altered alongside extensive changes in the epigenome, with repressed genes often being associated with local DNA hypermethylation and gain of nucleosomes at their promoters. However the spectrum of alterations that occur at distal regulatory regions has not been extensively studied. To address this we used Nucleosome Occupancy and Methylation sequencing (NOMe-seq to compare the genome-wide DNA methylation and nucleosome occupancy profiles between normal and cancer cell line models of the breast and prostate. Here we describe the bioinformatic pipeline and methods that we developed for the processing and analysis of the NOMe-seq data published by (Taberlay et al., 2014 [1] and deposited in the Gene Expression Omnibus with accession GSE57498.

In vivo NMR spectroscopy of ripening avocado

International Nuclear Information System (INIS)

Bennett, A.B.; Smith, G.M.; Nichols, B.

1987-01-01

Ripening of avocado fruit is associated with a dramatic increase in respiration. Previous studies have indicated that the increase in respiration is brought about by activation of the glycolytic reaction catalyzing the conversion of fructose-6-phosphate to fructose 1,6-bisphosphate. The authors reinvestigated the proposed role of glycolytic regulation in the respiratory increase using in vivo 31 P nuclear magnetic resonance (NMR) spectroscopy using an external surface coil and analysis of phosphofructokinase (PFK), phosphofructophosphotransferase (PFP), and fructose 2,6-bisphosphate (fru 2,6-P 2 ) levels in ripening avocado fruit. In vivo 31 P NMR spectroscopy revealed large increases in ATP levels accompanying the increase in respiration. Both glycolytic enzymes, PFK and PFP, were present in avocado fruit, with the latter activity being highly stimulated by fru 2,6-P 2 . Fructose 2,6-bisphosphate levels increased approximately 90% at the onset of ripening, indicating that the respiratory increase in ripening avocado may be regulated by the activation of PFP brought about by an increase in fru 2,6-P 2

A 55Mn NMR study of the La0.75Sr0.25MnO3 nanoparticles

International Nuclear Information System (INIS)

Rybicki, D.; Sikora, M.; Kapusta, Cz.; Riedi, P.C.; Jirak, Z.; Knizek, K.; Marysko, M.; Pollert, E.; Veverka, P.

2006-01-01

We report on a 55 Mn NMR study of the La 0.75 Sr 0.25 MnO 3 nanoparticles of the average grain size 33 nm and 114 nm at 4.2 K and 77 K and at applied field of 0, 0.2 and 0.5T. A dominant signal from the double exchange (DE) controlled metallic ferromagnetic interior of the grains as well as a small signal from insulating ferromagnetic regions is observed. From a comparison with bulk magnetization measurement the thickness of the nonferromagnetic outer layer of the grains and the amount of the ferromagnetic insulating phase was determined. The relative amount of these phases with respect to the ferromagnetic metallic phase increases with decreasing grain size. The DE line in the NMR spectrum shows a frequency shift with applied field according to a full 55 Mn gyromagnetic ratio. A value of the demagnetizing field close to zero is obtained, which indicates a single domain state of the nanoparticles. For the sample with larger grains a higher NMR enhancement is observed, which indicates a higher magnetic susceptibility of the sample at the NMR frequencies. A comparison with the NMR data obtained on a microcrystalline material is made. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

EASY: a simple tool for simultaneously removing background, deadtime and acoustic ringing in quantitative NMR spectroscopy--part I: basic principle and applications.

Science.gov (United States)

Jaeger, Christian; Hemmann, Felix

2014-01-01

Elimination of Artifacts in NMR SpectroscopY (EASY) is a simple but very effective tool to remove simultaneously any real NMR probe background signal, any spectral distortions due to deadtime ringdown effects and -specifically- severe acoustic ringing artifacts in NMR spectra of low-gamma nuclei. EASY enables and maintains quantitative NMR (qNMR) as only a single pulse (preferably 90°) is used for data acquisition. After the acquisition of the first scan (it contains the wanted NMR signal and the background/deadtime/ringing artifacts) the same experiment is repeated immediately afterwards before the T1 waiting delay. This second scan contains only the background/deadtime/ringing parts. Hence, the simple difference of both yields clean NMR line shapes free of artefacts. In this Part I various examples for complete (1)H, (11)B, (13)C, (19)F probe background removal due to construction parts of the NMR probes are presented. Furthermore, (25)Mg EASY of Mg(OH)2 is presented and this example shows how extremely strong acoustic ringing can be suppressed (more than a factor of 200) such that phase and baseline correction for spectra acquired with a single pulse is no longer a problem. EASY is also a step towards deadtime-free data acquisition as these effects are also canceled completely. EASY can be combined with any other NMR experiment, including 2D NMR, if baseline distortions are a big problem. © 2013 Published by Elsevier Inc.

Improvements of high-power diode laser line generators open up new application fields

Science.gov (United States)

Meinschien, J.; Bayer, A.; Bruns, P.; Aschke, L.; Lissotschenko, V. N.

2009-02-01

Beam shaping improvements of line generators based on high power diode lasers lead to new application fields as hardening, annealing or cutting of various materials. Of special interest is the laser treatment of silicon. An overview of the wide variety of applications is presented with special emphasis of the relevance of unique laser beam parameters like power density and beam uniformity. Complementary to vision application and plastic processing, these new application markets become more and more important and can now be addressed by high power diode laser line generators. Herewith, a family of high power diode laser line generators is presented that covers this wide spectrum of application fields with very different requirements, including new applications as cutting of silicon or glass, as well as the beam shaping concepts behind it. A laser that generates a 5m long and 4mm wide homogeneous laser line is shown with peak intensities of 0.2W/cm2 for inspection of railway catenaries as well as a laser that generates a homogeneous intensity distribution of 60mm x 2mm size with peak intensities of 225W/cm2 for plastic processing. For the annealing of silicon surfaces, a laser was designed that generates an extraordinary uniform intensity distribution with residual inhomogeneities (contrast ratio) of less than 3% over a line length of 11mm and peak intensities of up to 75kW/cm2. Ultimately, a laser line is shown with a peak intensity of 250kW/cm2 used for cutting applications. Results of various application tests performed with the above mentioned lasers are discussed, particularly the surface treatment of silicon and the cutting of glass.

Cys-Ph-TAHA: a lanthanide binding tag for RDC and PCS enhanced protein NMR

NARCIS (Netherlands)

Peters, Fabian; Maestre-Martinez, M.; Leonov, A.; Kovacic, L.; Becker, S.; Boelens, R.; Griesinger, C.

2011-01-01

Here we present Cys-Ph-TAHA, a new nonadentate lanthanide tag for the paramagnetic labelling of proteins. The tag can be easily synthesized and is stereochemically homogenous over a wide range of temperatures, yielding NMR spectra with a single set of peaks. Bound to ubiquitin, it induced large

Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy.

Science.gov (United States)

Prietzel, Jörg; Müller, Svenja; Kögel-Knabner, Ingrid; Thieme, Jürgen; Jaye, Cherno; Fischer, Daniel

2018-07-01

We compared synchrotron-based C near-edge X-ray absorption fine structure (NEXAFS) and CPMAS 13 C nuclear magnetic resonance (NMR) spectroscopy with respect to their precision and accuracy to quantify different organic carbon (OC) species in defined mixtures of soil organic matter source compounds. We also used both methods to quantify different OC species in organic surface horizons of a Histic Leptosol as well as in mineral topsoil and subsoil horizons of two soils with different parent material, stage of pedogenesis, and OC content (Cambisol: 15-30 OC mgg -1 , Podzol: 0.9-7 OC mgg -1 ). CPMAS 13 C NMR spectroscopy was more accurate and precise (mean recovery of different C functional groups 96-103%) than C NEXAFS spectroscopy (mean recovery 92-113%). For organic surface and topsoil samples, NMR spectroscopy consistently yielded larger O-alkyl C percentages and smaller alkyl C percentages than C NEXAFS spectroscopy. For the Cambisol subsoil samples both methods performed well and showed similar C speciation results. NEXAFS spectroscopy yielded excellent spectra with a high signal-to-noise ratio also for OC-poor Podzol subsoil samples, whereas this was not the case for CPMAS 13 C NMR spectroscopy even after sample treatment with HF. Our results confirm the analytical power of CPMAS 13 C NMR spectroscopy for a reliable quantitative OC speciation in soils with >10mgOCg -1 . Moreover, they highlight the potential of synchrotron-based C NEXAFS spectroscopy as fast, non-invasive method to semi-quantify different C functional groups in soils with low C content (0.9-10mgg -1 ). Copyright © 2018 Elsevier B.V. All rights reserved.

International symposium on NMR spectroscopy

International Nuclear Information System (INIS)

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

Surface topography and morphology characterization of PIII irradiated silicon surface

International Nuclear Information System (INIS)

Sharma, Satinder K.; Barthwal, Sumit

2008-01-01

The effect of plasma immersion ion implantation (PIII) treatment on silicon surfaces was investigated by micro-Raman and atomic force microscopy (AFM) technique. The surface damage was given by the implantation of carbon, nitrogen, oxygen and argon ions using an inductively coupled plasma (ICP) source at low pressure. AFM studies show that surface topography of the PIII treated silicon wafers depend on the physical and chemical nature of the implanted species. Micro-Raman spectra indicate that the significant reduction of intensity of Raman peak after PIII treatment. Plasma immersion ion implantation is a non-line-of-sight ion implantation method, which allows 3D treatment of materials. Therefore, PIII based surface modification and plasma immersion ion deposition (PIID) coatings are applied in a wide range of situations.

Moving contact lines on vibrating surfaces

Science.gov (United States)

Solomenko, Zlatko; Spelt, Peter; Scott, Julian

2017-11-01

Large-scale simulations of flows with moving contact lines for realistic conditions generally requires a subgrid scale model (analyses based on matched asymptotics) to account for the unresolved part of the flow, given the large range of length scales involved near contact lines. Existing models for the interface shape in the contact-line region are primarily for steady flows on homogeneous substrates, with encouraging results in 3D simulations. Introduction of complexities would require further investigation of the contact-line region, however. Here we study flows with moving contact lines on planar substrates subject to vibrations, with applications in controlling wetting/dewetting. The challenge here is to determine the change in interface shape near contact lines due to vibrations. To develop further insight, 2D direct numerical simulations (wherein the flow is resolved down to an imposed slip length) have been performed to enable comparison with asymptotic theory, which is also developed further. Perspectives will also be presented on the final objective of the work, which is to develop a subgrid scale model that can be utilized in large-scale simulations. The authors gratefully acknowledge the ANR for financial support (ANR-15-CE08-0031) and the meso-centre FLMSN for use of computational resources. This work was Granted access to the HPC resources of CINES under the allocation A0012B06893 made by GENCI.

Changes in Specific Surface as observed by NMR, caused by saturation of Chalk with porewater bearing divalent Ions

DEFF Research Database (Denmark)

Katika, Konstantina; Addassi, Mouadh; Alam, Mohammad Monzurul

2014-01-01

Nuclear Magnetic Resonance (NMR) spectrometry has proved to be a good technique for determining the petrophysical properties of reservoir rocks; such as porosity and pore size distribution. We investigated how pore water rich in divalent ions affect the NMR signal from chalk with two different de......-to-volume ratio of the pore space. The results of this work could benefit the ongoing study on the optimization of the water composition for Enhanced Oil Recovery (EOR) methods and shed light on how it can affect the mechanical and physical properties of the rock....

Dihydrochalcone Compounds Isolated from Crabapple Leaves Showed Anticancer Effects on Human Cancer Cell Lines

Directory of Open Access Journals (Sweden)

Xiaoxiao Qin

2015-11-01

Full Text Available Seven dihydrochalcone compounds were isolated from the leaves of Malus crabapples, cv. “Radiant”, and their chemical structures were elucidated by UV, IR, ESI-MS, 1H-NMR and 13C-NMR analyses. These compounds, which include trilobatin (A1, phloretin (A2, 3-hydroxyphloretin (A3, phloretin rutinoside (A4, phlorizin (A5, 6′′-O-coumaroyl-4′-O-glucopyranosylphloretin (A6, and 3′′′-methoxy-6′′-O-feruloy-4′-O-glucopyranosyl-phloretin (A7, all belong to the phloretin class and its derivatives. Compounds A6 and A7 are two new rare dihydrochalcone compounds. The results of a MTT cancer cell growth inhibition assay demonstrated that phloretin and these derivatives showed significant positive anticancer activities against several human cancer cell lines, including the A549 human lung cancer cell line, Bel 7402 liver cancer cell line, HepG2 human ileocecal cancer cell line, and HT-29 human colon cancer cell line. A7 had significant effects on all cancer cell lines, suggesting potential applications for phloretin and its derivatives. Adding a methoxyl group to phloretin dramatically increases phloretin’s anticancer activity.

Oriented solid-state NMR spectrosocpy

DEFF Research Database (Denmark)

Bertelsen, Kresten

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

A low cost surface plasmon resonance biosensor using a laser line generator

Science.gov (United States)

Chen, Ruipeng; Wang, Manping; Wang, Shun; Liang, Hao; Hu, Xinran; Sun, Xiaohui; Zhu, Juanhua; Ma, Liuzheng; Jiang, Min; Hu, Jiandong; Li, Jianwei

2015-08-01

Due to the instrument designed by using a common surface plasmon resonance biosensor is extremely expensive, we established a portable and cost-effective surface plasmon resonance biosensing system. It is mainly composed of laser line generator, P-polarizer, customized prism, microfluidic cell, and line Charge Coupled Device (CCD) array. Microprocessor PIC24FJ128GA006 with embedded A/D converter, communication interface circuit and photoelectric signal amplifier circuit are used to obtain the weak signals from the biosensing system. Moreover, the line CCD module is checked and optimized on the number of pixels, pixels dimension, output amplifier and the timing diagram. The micro-flow cell is made of stainless steel with a high thermal conductivity, and the microprocessor based Proportional-Integral-Derivative (PID) temperature-controlled algorithm was designed to keep the constant temperature (25 °C) of the sample solutions. Correspondingly, the data algorithms designed especially to this biosensing system including amplitude-limiting filtering algorithm, data normalization and curve plotting were programmed efficiently. To validate the performance of the biosensor, ethanol solution samples at the concentrations of 5%, 7.5%, 10%, 12.5% and 15% in volumetric fractions were used, respectively. The fitting equation ΔRU = - 752987.265 + 570237.348 × RI with the R-Square of 0.97344 was established by delta response units (ΔRUs) to refractive indexes (RI). The maximum relative standard deviation (RSD) of 4.8% was obtained.

An improved ultrafast 2D NMR experiment: Towards atom-resolved real-time studies of protein kinetics at multi-Hz rates

International Nuclear Information System (INIS)

Gal, Maayan; Kern, Thomas; Schanda, Paul; Frydman, Lucio; Brutscher, Bernhard

2009-01-01

Multidimensional NMR spectroscopy is a well-established technique for the characterization of structure and fast-time-scale dynamics of highly populated ground states of biological macromolecules. The investigation of short-lived excited states that are important for molecular folding, misfolding and function, however, remains a challenge for modern biomolecular NMR techniques. Off-equilibrium real-time kinetic NMR methods allow direct observation of conformational or chemical changes by following peak positions and intensities in a series of spectra recorded during a kinetic event. Because standard multidimensional NMR methods required to yield sufficient atom-resolution are intrinsically time-consuming, many interesting phenomena are excluded from real-time NMR analysis. Recently, spatially encoded ultrafast 2D NMR techniques have been proposed that allow one to acquire a 2D NMR experiment within a single transient. In addition, when combined with the SOFAST technique, such ultrafast experiments can be repeated at high rates. One of the problems detected for such ultrafast protein NMR experiments is related to the heteronuclear decoupling during detection with interferences between the pulses and the oscillatory magnetic field gradients arising in this scheme. Here we present a method for improved ultrafast data acquisition yielding higher signal to noise and sharper lines in single-scan 2D NMR spectra. In combination with a fast-mixing device, the recording of 1 H- 15 N correlation spectra with repetition rates of up to a few Hertz becomes feasible, enabling real-time studies of protein kinetics occurring on time scales down to a few seconds

Mechanism for microwave heating of 1-(4'-cyanophenyl)-4-propylcyclohexane characterized by in situ microwave irradiation NMR spectroscopy.

Science.gov (United States)

Tasei, Yugo; Yamakami, Takuya; Kawamura, Izuru; Fujito, Teruaki; Ushida, Kiminori; Sato, Motoyasu; Naito, Akira

2015-05-01

Microwave heating is widely used to accelerate organic reactions and enhance the activity of enzymes. However, the detailed molecular mechanism for the effect of microwave on chemical reactions is not yet fully understood. To investigate the effects of microwave heating on organic compounds, we have developed an in situ microwave irradiation NMR spectroscopy. (1)H NMR spectra of 1-(4'-cyanophenyl)-4-propylcyclohexane (PCH3) in the liquid crystalline and isotropic phases were observed under microwave irradiation. When the temperature was regulated at slightly higher than the phase transition temperature (Tc=45 °C) under a gas flow temperature control system, liquid crystalline phase mostly changed to the isotropic phase. Under microwave irradiation and with the gas flow temperature maintained at 20 °C, which is 25 °C below the Tc, the isotropic phase appeared stationary as an approximately 2% fraction in the liquid crystalline phase. The temperature of the liquid crystalline state was estimated to be 38 °C according to the line width, which is at least 7 °C lower than the Tc. The temperature of this isotropic phase should be higher than 45 °C, which is considered to be a non-equilibrium local heating state induced by microwave irradiation. Microwaves at a power of 195 W were irradiated to the isotropic phase of PCH3 at 50 °C and after 2 min, the temperature reached 220 °C. The temperature of PCH3 under microwave irradiation was estimated by measurement of the chemical shift changes of individual protons in the molecule. These results demonstrate that microwave heating generates very high temperature within a short time using an in situ microwave irradiation NMR spectrometer. Copyright © 2015 Elsevier Inc. All rights reserved.

An On-Line Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Perfluoroalkyl Acids in Drinking and Surface Waters

Directory of Open Access Journals (Sweden)

Michela Mazzoni

2015-01-01

Full Text Available An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms. This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between −34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters.

An On-Line Solid Phase Extraction-Liquid Chromatography-Tandem Mass Spectrometry Method for the Determination of Perfluoroalkyl Acids in Drinking and Surface Waters

Science.gov (United States)

Mazzoni, Michela; Rusconi, Marianna; Valsecchi, Sara; Martins, Claudia P. B.; Polesello, Stefano

2015-01-01

An UHPLC-MS/MS multiresidue method based on an on-line solid phase extraction (SPE) procedure was developed for the simultaneous determination of 9 perfluorinated carboxylates (from 4 to 12 carbon atoms) and 3 perfluorinated sulphonates (from 4 to 8 carbon atoms). This work proposes using an on-line solid phase extraction before chromatographic separation and analysis to replace traditional methods of off-line SPE before direct injection to LC-MS/MS. Manual sample preparation was reduced to sample centrifugation and acidification, thus eliminating several procedural errors and significantly reducing time-consuming and costs. Ionization suppression between target perfluorinated analytes and their coeluting SIL-IS were detected for homologues with a number of carbon atoms less than 9, but the quantitation was not affected. Total matrix effect corrected by SIL-IS, inclusive of extraction efficacy, and of ionization efficiency, ranged between −34 and +39%. The percentage of recoveries, between 76 and 134%, calculated in different matrices (tap water and rivers impacted by different pollutions) was generally satisfactory. LODs and LOQs of this on-line SPE method, which also incorporate recovery losses, ranged from 0.2 to 5.0 ng/L and from 1 to 20 ng/L, respectively. Validated on-line SPE-LC/MS/MS method has been applied in a wide survey for the determination of perfluoroalkyl acids in Italian surface and ground waters. PMID:25834752

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

NARCIS (Netherlands)

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

2017-01-01

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

Uniform surface-to-line integral reduction of physical optics for curved surfaces by modified edge representation with higher-order correction

Science.gov (United States)

Lyu, Pengfei; Ando, Makoto

2017-09-01

The modified edge representation is one of the equivalent edge currents approximation methods for calculating the physical optics surface radiation integrals in diffraction analysis. The Stokes' theorem is used in the derivation of the modified edge representation from the physical optics for the planar scatterer case, which implies that the surface integral is rigorously reduced into the line integral of the modified edge representation equivalent edge currents, defined in terms of the local shape of the edge. On the contrary, for curved surfaces, the results of radiation integrals depend upon the global shape of the scatterer. The physical optics surface integral consists of two components, from the inner stationary phase point and the edge. The modified edge representation is defined independently from the orientation of the actual edge, and therefore, it could be available not only at the edge but also at the arbitrary points on the scatterer except the stationary phase point where the modified edge representation equivalent edge currents becomes infinite. If stationary phase point exists inside the illuminated region, the physical optics surface integration is reduced into two kinds of the modified edge representation line integrations, along the edge and infinitesimally small integration around the inner stationary phase point, the former and the latter give the diffraction and reflection components, respectively. The accuracy of the latter has been discussed for the curved surfaces and published. This paper focuses on the errors of the former and discusses its correction. It has been numerically observed that the modified edge representation works well for the physical optics diffraction in flat and concave surfaces; errors appear especially for the observer near the reflection shadow boundary if the frequency is low for the convex scatterer. This paper gives the explicit expression of the higher-order correction for the modified edge representation.

High Accuracy Potential Energy Surface, Dipole Moment Surface, Rovibrational Energies and Line List Calculations for ^{14}NH_3

Science.gov (United States)

Coles, Phillip; Yurchenko, Sergei N.; Polyansky, Oleg; Kyuberis, Aleksandra; Ovsyannikov, Roman I.; Zobov, Nikolay Fedorovich; Tennyson, Jonathan

2017-06-01

We present a new spectroscopic potential energy surface (PES) for ^{14}NH_3, produced by refining a high accuracy ab initio PES to experimental energy levels taken predominantly from MARVEL. The PES reproduces 1722 matched J=0-8 experimental energies with a root-mean-square error of 0.035 cm-1 under 6000 cm^{-1} and 0.059 under 7200 cm^{-1}. In conjunction with a new DMS calculated using multi reference configuration interaction (MRCI) and H=aug-cc-pVQZ, N=aug-cc-pWCVQZ basis sets, an infrared (IR) line list has been computed which is suitable for use up to 2000 K. The line list is used to assign experimental lines in the 7500 - 10,500 cm^{-1} region and previously unassigned lines in HITRAN in the 6000-7000 cm^{-1} region. Oleg L. Polyansky, Roman I. Ovsyannikov, Aleksandra A. Kyuberis, Lorenzo Lodi, Jonathan Tennyson, Andrey Yachmenev, Sergei N. Yurchenko, Nikolai F. Zobov, J. Mol. Spec., 327 (2016) 21-30 Afaf R. Al Derzia, Tibor Furtenbacher, Jonathan Tennyson, Sergei N. Yurchenko, Attila G. Császár, J. Quant. Spectrosc. Rad. Trans., 161 (2015) 117-130

Determining the parity of a permutation using an experimental NMR qutrit

International Nuclear Information System (INIS)

Dogra, Shruti; Arvind,; Dorai, Kavita

2014-01-01

We present the NMR implementation of a recently proposed quantum algorithm to find the parity of a permutation. In the usual qubit model of quantum computation, it is widely believed that computational speedup requires the presence of entanglement and thus cannot be achieved by a single qubit. On the other hand, a qutrit is qualitatively more quantum than a qubit because of the existence of quantum contextuality and a single qutrit can be used for computing. We use the deuterium nucleus oriented in a liquid crystal as the experimental qutrit. This is the first experimental exploitation of a single qutrit to carry out a computational task. - Highlights: • NMR implementation of a quantum algorithm to determine the parity of a permutation. • Algorithm implemented on a single qutrit. • Computational speedup achieved without quantum entanglement. • Single qutrit shows quantum contextuality

Satellite NMR in Cu doped with transition impurities

International Nuclear Information System (INIS)

Slichter, C.P.

1979-01-01

Measurements were made of the conduction electron spin magnetization density, M/sub sigma/(R vector) near iron group atoms (Sc through Ni) in Cu. M/sub sigma/(R vector) produces an additional effective local field which shifts the NMR frequency of nearby shells of Cu nuclei relative to Cu nuclei far from all impurities. Resonances of nearby shells appear as weak satellites to the strong resonance of distant Cu nuclei (the main line). M/sub sigma/(R vector) at a given site is proportional through know constants to the splitting of the satellite from the main line. The shell was identified giving rise to the satellite in many cases by use of single crystals. A good approximation M/sub sigma/(R vector) is proportional to the spin susceptibility chi/sub s/ of the impurity. For CuCr we find a large temperature independent chi/sub s/, in contrast to CuMn and CuFe. The results lead to a picture of the electronic structure of Cr, Mn, and Fe along the lines of Schrieffer and Hirst as ions with integral numbers of d-electrons, possessing crystal field and spin-orbit couplings

Annual reports on NMR spectroscopy

CERN Document Server

Webb, Graham A; McCarthy, M J

1995-01-01

Over recent years, no other technique has grown to such importance as that of NMR spectroscopy. It is used in all branches of science where precise structural determination is required and where the nature of interactions and reactions in solution is being studied. Annual Reports on NMR Spectroscopy has established itself as a means for the specialist and non-specialist alike to become familiar with new applications of the technique in all branches of chemistry, including biochemistry, and pharmaceutics. This volume focuses on theoretical aspects of NMR nuclear shielding and on applications of

Functional dynamics of cell surface membrane proteins.

Science.gov (United States)

Nishida, Noritaka; Osawa, Masanori; Takeuchi, Koh; Imai, Shunsuke; Stampoulis, Pavlos; Kofuku, Yutaka; Ueda, Takumi; Shimada, Ichio

2014-04-01

Cell surface receptors are integral membrane proteins that receive external stimuli, and transmit signals across plasma membranes. In the conventional view of receptor activation, ligand binding to the extracellular side of the receptor induces conformational changes, which convert the structure of the receptor into an active conformation. However, recent NMR studies of cell surface membrane proteins have revealed that their structures are more dynamic than previously envisioned, and they fluctuate between multiple conformations in an equilibrium on various timescales. In addition, NMR analyses, along with biochemical and cell biological experiments indicated that such dynamical properties are critical for the proper functions of the receptors. In this review, we will describe several NMR studies that revealed direct linkage between the structural dynamics and the functions of the cell surface membrane proteins, such as G-protein coupled receptors (GPCRs), ion channels, membrane transporters, and cell adhesion molecules. Copyright © 2013 Elsevier Inc. All rights reserved.

Piercing the water surface with a blade: Singularities of the contact line

Energy Technology Data Exchange (ETDEWEB)

Alimov, Mars M. [Kazan Federal University, Kazan 420008 (Russian Federation); Kornev, Konstantin G. [Department of Materials Science & Engineering, Clemson University, Clemson, South Carolina 29634 (United States)

2016-01-15

An external meniscus on a narrow blade with a slit-like cross section is studied using the hodograph formulation of the Laplace nonlinear equation of capillarity. On narrow blades, the menisci are mostly shaped by the wetting and capillary forces; gravity plays a secondary role. To describe a meniscus in this asymptotic case, the model of Alimov and Kornev [“Meniscus on a shaped fibre: Singularities and hodograph formulation,” Proc. R. Soc. A 470, 20140113 (2014)] has been employed. It is shown that at the sharp edges of the blade, the contact line makes a jump. In the wetting case, the contact line sitting at each side of the blade is lifted above the points where the meniscus first meets the blade edges. In the non-wetting case, the contact line is lowered below these points. The contours of the constant height emanating from the blade edges generate unusual singularities with infinite curvatures at some points at the blade edges. The meniscus forms a unique surface made of two mirror-symmetric sheets fused together. Each sheet is supported by the contact line sitting at each side of the blade.

Piercing the water surface with a blade: Singularities of the contact line

International Nuclear Information System (INIS)

Alimov, Mars M.; Kornev, Konstantin G.

2016-01-01

An external meniscus on a narrow blade with a slit-like cross section is studied using the hodograph formulation of the Laplace nonlinear equation of capillarity. On narrow blades, the menisci are mostly shaped by the wetting and capillary forces; gravity plays a secondary role. To describe a meniscus in this asymptotic case, the model of Alimov and Kornev [“Meniscus on a shaped fibre: Singularities and hodograph formulation,” Proc. R. Soc. A 470, 20140113 (2014)] has been employed. It is shown that at the sharp edges of the blade, the contact line makes a jump. In the wetting case, the contact line sitting at each side of the blade is lifted above the points where the meniscus first meets the blade edges. In the non-wetting case, the contact line is lowered below these points. The contours of the constant height emanating from the blade edges generate unusual singularities with infinite curvatures at some points at the blade edges. The meniscus forms a unique surface made of two mirror-symmetric sheets fused together. Each sheet is supported by the contact line sitting at each side of the blade

SICS. A Sensor-Based In-Line Control System for the Surfaces of Continuously Cast Slabs

Energy Technology Data Exchange (ETDEWEB)

Chang, Tzyy-Shuh [OG Technologies, Inc., Ann Arbor, MI (United States)

2013-09-23

The Phase II project has been carried out in accordance to the proposed tasks and budget, based on the original and extended schedule. The R&D team designed and implemented the test unit for the full width coverage, installed the unit in a caster. The development work further included enhanced image processing, in-depth defect study and process control models. The function, operation, and maintenance of the SICS was thoroughly studied during the Phase II research. The experience indicates additional hardware and procedures are required to make the SICS a commercially ready product in operation and maintenance aspect. Such developments have been finished and the team is contacting potential customers for the first commercial installation of SICS. Additionally, OGT is exploring the possibility to team up with a US company that specializes in surface cleaning for slabs/blooms/billets such that the in-line surface inspection can be integrated with in-line surface clean up for the maximum benefit to the steel industry.

Ground-state magnetization of the molecular cluster Mn12O12-acetate as seen by proton NMR

International Nuclear Information System (INIS)

Furukawa, Y.; Watanabe, K.; Kumagai, K.; Jang, Z. H.; Lascialfari, A.; Borsa, F.; Gatteschi, D.

2000-01-01

1 H nuclear magnetic resonance (NMR) measurements have been carried out in Mn 12 O 12 -acetate clusters at low temperature in order to investigate microscopically the static and dynamic magnetic properties of the molecule in its high-spin S=10 ground state. Below liquid helium temperature it is found that the local hyperfine fields at the proton sites are static as expected for the very slow superparamagnetic relaxation of Mn 12 O 12 at low temperature. The magnitude and distribution of the hyperfine fields can be reproduced to a good approximation by considering only the dipolar interaction of protons with the local Mn magnetic moments and by assigning the magnitude and orientation of the local moments of the different Mn 3+ and Mn 4+ ions according to an accepted coupling scheme for the total S=10 ground state. The relaxation time of the macroscopic magnetization of the cluster was measured by monitoring the change of the intensity of the 1 H-NMR shifted lines following inversion of the applied magnetic field. This is possible because the sudden change of the field orientation changes the sign of the shift of the NMR lines in the proton spectrum. Although important differences are noticed, the relaxation time of the magnetization as measured indirectly by the 1 H-NMR method is comparable to the one obtained directly with a superconducting quantum interference device magnetometer. In particular we could reproduce the minima in the relaxation time as a function of magnetic field at the fields for level crossing, minima which are considered to be a signature of the quantum tunneling of the magnetization

Solid-state NMR spectroscopy on complex biomolecules

NARCIS (Netherlands)

Renault, M.A.M.; Cukkemane, A.A.; Baldus, M.

2010-01-01

Biomolecular applications of NMR spectroscopy are often merely associated with soluble molecules or magnetic resonance imaging. However, since the late 1970s, solid-state NMR (ssNMR) spectroscopy has demonstrated its ability to provide atomic-level insight into complex biomolecular systems ranging

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

Directory of Open Access Journals (Sweden)

Guillaume D.

1999-07-01

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

Detecting unfrozen sediments below thermokarst lakes with surface nuclear magnetic resonance

Science.gov (United States)

Parsekian, Andrew D.; Grosse, Guido; Walbrecker, Jan O.; Müller-Petke, Mike; Keating, Kristina; Liu, Lin; Jones, Benjamin M.; Knight, Rosemary

2013-01-01

A talik is a layer or body of unfrozen ground that occurs in permafrost due to an anomaly in thermal, hydrological, or hydrochemical conditions. Information about talik geometry is important for understanding regional surface water and groundwater interactions as well as sublacustrine methane production in thermokarst lakes. Due to the direct measurement of unfrozen water content, surface nuclear magnetic resonance (NMR) is a promising geophysical method for noninvasively estimating talik dimensions. We made surface NMR measurements on thermokarst lakes and terrestrial permafrost near Fairbanks, Alaska, and confirmed our results using limited direct measurements. At an 8 m deep lake, we observed thaw bulb at least 22 m below the surface; at a 1.4 m deep lake, we detected a talik extending between 5 and 6 m below the surface. Our study demonstrates the value that surface NMR may have in the cryosphere for studies of thermokarst lake hydrology and their related role in the carbon cycle.

Thermal Stress of Surface of Mold Cavities and Parting Line of Silicone Molds

Directory of Open Access Journals (Sweden)

Bajčičák Martin

2014-06-01

Full Text Available The paper is focused on the study of thermal stress of surface of mold cavities and parting line of silicone molds after pouring. The silicone mold White SD - THT was thermally stressed by pouring of ZnAl4Cu3 zinc alloy with pouring cycle 20, 30 and 40 seconds. The most thermally stressed part of surface at each pouring cycle is gating system and mold cavities. It could be further concluded that linear increase of the pouring cycle time leads to the exponential increasing of the maximum temperature of mold surface after its cooling. The elongated pouring cycle increases the temperature accumulated on the surface of cavities and the ability of silicone mold to conduct the heat on its surface decreases, because the low thermal conductivity of silicone molds enables the conduction of larger amount of heat into ambient environment.

Integrative NMR for biomolecular research

International Nuclear Information System (INIS)

Lee, Woonghee; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L.

2016-01-01

NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download_packages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

Integrative NMR for biomolecular research

Energy Technology Data Exchange (ETDEWEB)

Lee, Woonghee, E-mail: whlee@nmrfam.wisc.edu; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R.; Tonelli, Marco; Westler, William M.; Butcher, Samuel E.; Henzler-Wildman, Katherine A.; Markley, John L., E-mail: markley@nmrfam.wisc.edu [University of Wisconsin-Madison, National Magnetic Resonance Facility at Madison and Biochemistry Department (United States)

2016-04-15

NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download-packages.html http://pine.nmrfam.wisc.edu/download{sub p}ackages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html http://pine.nmrfam.wisc.edu/integrative.html ).

Coupling Fluid and Solute Dynamics Within the Ocular Surface Tear Film: A Modelling Study of Black Line Osmolarity

KAUST Repository

Zubkov, V. S.

2012-07-06

We present a mathematical model describing the spatial distribution of tear film osmolarity across the ocular surface of a human eye during one blink cycle, incorporating detailed fluid and solute dynamics. Based on the lubrication approximation, our model comprises three coupled equations tracking the depth of the aqueous layer of the tear film, the concentration of the polar lipid, and the concentration of physiological salts contained in the aqueous layer. Diffusive boundary layers in the salt concentration occur at the thinnest regions of the tear film, the black lines. Thus, despite large Peclet numbers, diffusion ameliorates osmolarity around the black lines, but nonetheless is insufficient to eliminate the build-up of solute in these regions. More generally, a heterogeneous distribution of solute concentration is predicted across the ocular surface, indicating that measurements of lower meniscus osmolarity are not globally representative, especially in the presence of dry eye. Vertical saccadic eyelid motion can reduce osmolarity at the lower black line, raising the prospect that select eyeball motions more generally can assist in alleviating tear film hyperosmolarity. Finally, our results indicate that measured evaporative rates will induce excessive hyperosmolarity at the black lines, even for the healthy eye. This suggests that further evaporative retardation at the black lines, for instance due to the cellular glycocalyx at the ocular surface or increasing concentrations of mucus, will be important for controlling hyperosmolarity as the black line thins. © 2012 Society for Mathematical Biology.

Quartz Crystal Temperature Sensor for MAS NMR

Science.gov (United States)

Simon, Gerald

1997-10-01

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

Grape juice quality control by means of {sup 1}H NMR spectroscopy and chemometric analyses

Energy Technology Data Exchange (ETDEWEB)

Grandizoli, Caroline Werner Pereira da Silva; Campos, Francinete Ramos; Simonelli, Fabio; Barison, Andersson [Universidade Federal do Paraná (UFPR), Curitiba (Brazil). Departamento de Química

2014-07-01

This work shows the application of {sup 1}H NMR spectroscopy and chemometrics for quality control of grape juice. A wide range of quality assurance parameters were assessed by single {sup 1}H NMR experiments acquired directly from juice. The investigation revealed that conditions and time of storage should be revised and indicated on all labels. The sterilization process of homemade grape juices was efficient, making it possible to store them for long periods without additives. Furthermore, chemometric analysis classified the best commercial grape juices to be similar to homemade grape juices, indicating that this approach can be used to determine the authenticity after adulteration. (author)

Basics of spectroscopic instruments. Hardware of NMR spectrometer

International Nuclear Information System (INIS)

Sato, Hajime

2009-01-01

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

33S NMR cryogenic probe for taurine detection

Science.gov (United States)

Hobo, Fumio; Takahashi, Masato; Maeda, Hideaki

2009-03-01

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

Dynamic domains of amyloid fibrils can be site-specifically assigned with proton detected 3D NMR spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Falk, Alexander S.; Siemer, Ansgar B., E-mail: asiemer@usc.edu [Keck School of Medicine of USC, Department of Biochemistry and Molecular Medicine, Zilkha Neurogenetic Institute (United States)

2016-11-15

Several amyloid fibrils have cores framed by highly dynamic, intrinsically disordered, domains that can play important roles for function and toxicity. To study these domains in detail using solid-state NMR spectroscopy, site-specific resonance assignments are required. Although the rapid dynamics of these domains lead to considerable averaging of orientation-dependent NMR interactions and thereby line-narrowing, the proton linewidths observed in these samples is far larger than what is regularly observed in solution. Here, we show that it is nevertheless possible to record 3D HNCO, HNCA, and HNcoCA spectra on these intrinsically disordered domains and to obtain site-specific assignments.

Dynamic domains of amyloid fibrils can be site-specifically assigned with proton detected 3D NMR spectroscopy

International Nuclear Information System (INIS)

Falk, Alexander S.; Siemer, Ansgar B.

2016-01-01

Several amyloid fibrils have cores framed by highly dynamic, intrinsically disordered, domains that can play important roles for function and toxicity. To study these domains in detail using solid-state NMR spectroscopy, site-specific resonance assignments are required. Although the rapid dynamics of these domains lead to considerable averaging of orientation-dependent NMR interactions and thereby line-narrowing, the proton linewidths observed in these samples is far larger than what is regularly observed in solution. Here, we show that it is nevertheless possible to record 3D HNCO, HNCA, and HNcoCA spectra on these intrinsically disordered domains and to obtain site-specific assignments.

MetaboLab - advanced NMR data processing and analysis for metabolomics

Directory of Open Access Journals (Sweden)

Günther Ulrich L

2011-09-01

Full Text Available Abstract Background Despite wide-spread use of Nuclear Magnetic Resonance (NMR in metabolomics for the analysis of biological samples there is a lack of graphically driven, publicly available software to process large one and two-dimensional NMR data sets for statistical analysis. Results Here we present MetaboLab, a MATLAB based software package that facilitates NMR data processing by providing automated algorithms for processing series of spectra in a reproducible fashion. A graphical user interface provides easy access to all steps of data processing via a script builder to generate MATLAB scripts, providing an option to alter code manually. The analysis of two-dimensional spectra (1H,13C-HSQC spectra is facilitated by the use of a spectral library derived from publicly available databases which can be extended readily. The software allows to display specific metabolites in small regions of interest where signals can be picked. To facilitate the analysis of series of two-dimensional spectra, different spectra can be overlaid and assignments can be transferred between spectra. The software includes mechanisms to account for overlapping signals by highlighting neighboring and ambiguous assignments. Conclusions The MetaboLab software is an integrated software package for NMR data processing and analysis, closely linked to the previously developed NMRLab software. It includes tools for batch processing and gives access to a wealth of algorithms available in the MATLAB framework. Algorithms within MetaboLab help to optimize the flow of metabolomics data preparation for statistical analysis. The combination of an intuitive graphical user interface along with advanced data processing algorithms facilitates the use of MetaboLab in a broader metabolomics context.

Ferromagnetic correlations in Yb based heavy fermions probed by NMR relaxation: YbNi{sub 4}P{sub 2} vs. Yb(Rh,Ir){sub 2}Si{sub 2}

Energy Technology Data Exchange (ETDEWEB)

Baenitz, M.; Sarkar, R.; Khuntia, P.; Krellner, C.; Geibel, C.; Steglich, F. [Max - Planck Institute of Chemical Physics of Solids, 01187 Dresden, Germany (Germany)

2012-07-01

Intersite correlations in Ce-based heavy fermion systems close to the quantum critical point separating the magnetic ordered state from the paramagnetic Kondo lattice are in almost all cases predominantly antiferromagnetic (AFM) in nature. The NMR relaxation of these systems show an evolution from localized fluctuations with 1/T{sub 1} nearly constant above the Kondo temperature T{sub K}, to a linear in T Korringa- like behavior with a constant and enhanced (1/T{sub 1}T)- value below T{sub K}. We report on {sup 31}P-NMR results on the ferromagnetic (FM) quantum critical system YbNi{sub 4}P{sub 2} over a wide range in temperature (2-300 K) and field (0.2 - 9 T). Here, {sup 31}(1/T{sub 1}T)(T) does not show such a signature at T{sub K}, instead a continuous increase of (1/T{sub 1}T) down to lowest T is observed. A similar behavior has been reported for YbRh{sub 2}Si{sub 2}, which also exhibits strong FM correlations evidenced by {sup 29}Si - NMR and an enhanced Wilson ratio. Furthermore, in CeFePO, which is likely unique among Ce-based quantum critical system because of its strong FM correlations, (1/T{sub 1}T) also diverges continuously for T {yields}0. This suggests that the difference in the relaxation between most of the Ce systems and the Yb systems is predominantly related to a change from AFM to FM intersite correlations. NMR-results (shift, line width, T{sub 1}) are analyzed and discussed in different models (Korringa, Moriya).

3D Reconstruction of NMR Images by LabVIEW

Directory of Open Access Journals (Sweden)

Peter IZAK

2007-01-01

Full Text Available This paper introduces the experiment of 3D reconstruction NMR images via virtual instrumentation - LabVIEW. The main idea is based on marching cubes algorithm and image processing implemented by module of Vision assistant. The two dimensional images shot by the magnetic resonance device provide information about the surface properties of human body. There is implemented algorithm which can be used for 3D reconstruction of magnetic resonance images in biomedical application.

Comparative analysis of the surface exposed proteome of two canine osteosarcoma cell lines and normal canine osteoblasts.

Science.gov (United States)

Milovancev, Milan; Hilgart-Martiszus, Ian; McNamara, Michael J; Goodall, Cheri P; Seguin, Bernard; Bracha, Shay; Wickramasekara, Samanthi I

2013-06-13

Osteosarcoma (OSA) is the most common primary bone tumor of dogs and carries a poor prognosis despite aggressive treatment. An improved understanding of the biology of OSA is critically needed to allow for development of novel diagnostic, prognostic, and therapeutic tools. The surface-exposed proteome (SEP) of a cancerous cell includes a multifarious array of proteins critical to cellular processes such as proliferation, migration, adhesion, and inter-cellular communication. The specific aim of this study was to define a SEP profile of two validated canine OSA cell lines and a normal canine osteoblast cell line utilizing a biotinylation/streptavidin system to selectively label, purify, and identify surface-exposed proteins by mass spectrometry (MS) analysis. Additionally, we sought to validate a subset of our MS-based observations via quantitative real-time PCR, Western blot and semi-quantitative immunocytochemistry. Our hypothesis was that MS would detect differences in the SEP composition between the OSA and the normal osteoblast cells. Shotgun MS identified 133 putative surface proteins when output from all samples were combined, with good consistency between biological replicates. Eleven of the MS-detected proteins underwent analysis of gene expression by PCR, all of which were actively transcribed, but varied in expression level. Western blot of whole cell lysates from all three cell lines was effective for Thrombospondin-1, CYR61 and CD44, and indicated that all three proteins were present in each cell line. Semi-quantitative immunofluorescence indicated that CD44 was expressed at much higher levels on the surface of the OSA than the normal osteoblast cell lines. The results of the present study identified numerous differences, and similarities, in the SEP of canine OSA cell lines and normal canine osteoblasts. The PCR, Western blot, and immunocytochemistry results, for the subset of proteins evaluated, were generally supportive of the mass spectrometry data

Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

KAUST Repository

Bendjeriou-Sedjerari, Anissa

2016-08-11

Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

Tungsten(VI) Carbyne/Bis(carbene) Tautomerization Enabled by N-Donor SBA15 Surface Ligands: A Solid-State NMR and DFT Study

KAUST Repository

Bendjeriou-Sedjerari, Anissa; Sofack-Kreutzer, Julien; Minenkov, Yury; Abou-Hamad, Edy; Hamzaoui, Bilel; Werghi, Baraa; Anjum, Dalaver H.; Cavallo, Luigi; Huang, Kuo-Wei; Basset, Jean-Marie

2016-01-01

Designing supported well-defined bis(carbene) complexes remains a key challenge in heterogeneous catalysis. The reaction of W(CtBu)(CH(2)tBu)(3) with amine-modified mesoporous SBA15 silica, which has vicinal silanol/silylamine pairs [(SiOH)(SiNH2)], leads to [(SiNH2-)(SiO-)W(CHtBu)(CH(2)tBu)(2)] and [(SiNH2-)(SiO-)W(=CHtBu)(2)(CH(2)tBu). Variable temperature, H-1-H-1 2D double-quantum, H-1-C-13 HETCOR, and HETCOR with spin diffusion solid-state NMR spectroscopy demonstrate tautomerization between the alkyl alkylidyne and the bis(alkylidene) on the SBA15 surface. Such equilibrium is possible through the coordination of W to the surface [(Si-OH)(Si-NH2)] groups, which act as a [N,O] pincer ligand. DFT calculations provide a rationalization for the surface-complex tautomerization and support the experimental results. This direct observation of such a process shows the strong similarity between molecular mechanisms in homogeneous and heterogeneous catalysis. In propane metathesis (at 150 degrees C), the tungsten bis(carbene) tautomer is favorable, with a turnover number (TON) of 262. It is the highest TON among all the tungsten alkyl-supported catalysts.

Untangle soil-water-mucilage interactions: 1H NMR Relaxometry is lifting the veil

Science.gov (United States)

Brax, Mathilde; Buchmann, Christian; Schaumann, Gabriele Ellen

2017-04-01

Mucilage is mainly produced at the root tips and has a high water holding capacity derived from highly hydrophilic gel-forming substances. The objective of the MUCILAGE project is to understand the mechanistic role of mucilage for the regulation of water supply for plants. Our subproject investigates the chemical and physical properties of mucilage as pure gel and mixed with soil. 1H-NMR Relaxometry and PFG NMR represent non-intrusive powerful methods for soil scientific research by allowing quantification of the water distribution as well as monitoring of the water mobility in soil pores and gel phases.Relaxation of gel water differs from the one of pure water due to additional interactions with the gel matrix. Mucilage in soil leads to a hierarchical pore structure, consisting of the polymeric biohydrogel network surrounded by the surface of soil particles. The two types of relaxation rates 1/T1 and 1/T2 measured with 1H-NMR relaxometry refer to different relaxation mechanisms of water, while PFG-NMR measures the water self-diffusion coefficient. The objective of our study is to distinguish in situ water in gel from pore water in a simplified soil system, and to determine how the "gel effect" affects both relaxation rates and the water self-diffusion coefficient in porous systems. We demonstrate how the mucilage concentration and the soil solution alter the properties of water in the respective gel phases and pore systems in model soils. To distinguish gel-inherent processes from classical processes, we investigated the variations of the water mobility in pure chia mucilage under different conditions by using 1H-NMR relaxometry and PFG NMR. Using model soils, the signals coming from pore water and gel water were differentiated. We combined the equations describing 1H-NMR relaxation in porous systems and our experimental results, to explain how the presence of gel in soil affects 1H-NMR relaxation. Out of this knowledge we propose a method, which determines in

Rapid prediction of multi-dimensional NMR data sets

International Nuclear Information System (INIS)

Gradmann, Sabine; Ader, Christian; Heinrich, Ines; Nand, Deepak; Dittmann, Marc; Cukkemane, Abhishek; Dijk, Marc van; Bonvin, Alexandre M. J. J.; Engelhard, Martin; Baldus, Marc

2012-01-01

We present a computational environment for Fast Analysis of multidimensional NMR DAta Sets (FANDAS) that allows assembling multidimensional data sets from a variety of input parameters and facilitates comparing and modifying such “in silico” data sets during the various stages of the NMR data analysis. The input parameters can vary from (partial) NMR assignments directly obtained from experiments to values retrieved from in silico prediction programs. The resulting predicted data sets enable a rapid evaluation of sample labeling in light of spectral resolution and structural content, using standard NMR software such as Sparky. In addition, direct comparison to experimental data sets can be used to validate NMR assignments, distinguish different molecular components, refine structural models or other parameters derived from NMR data. The method is demonstrated in the context of solid-state NMR data obtained for the cyclic nucleotide binding domain of a bacterial cyclic nucleotide-gated channel and on membrane-embedded sensory rhodopsin II. FANDAS is freely available as web portal under WeNMR (http://www.wenmr.eu/services/FANDAShttp://www.wenmr.eu/services/FANDAS).

Rapid prediction of multi-dimensional NMR data sets

Energy Technology Data Exchange (ETDEWEB)

Gradmann, Sabine; Ader, Christian [Utrecht University, Faculty of Science, Bijvoet Center for Biomolecular Research (Netherlands); Heinrich, Ines [Max Planck Institute for Molecular Physiology, Department of Physical Biochemistry (Germany); Nand, Deepak [Utrecht University, Faculty of Science, Bijvoet Center for Biomolecular Research (Netherlands); Dittmann, Marc [Max Planck Institute for Molecular Physiology, Department of Physical Biochemistry (Germany); Cukkemane, Abhishek; Dijk, Marc van; Bonvin, Alexandre M. J. J. [Utrecht University, Faculty of Science, Bijvoet Center for Biomolecular Research (Netherlands); Engelhard, Martin [Max Planck Institute for Molecular Physiology, Department of Physical Biochemistry (Germany); Baldus, Marc, E-mail: m.baldus@uu.nl [Utrecht University, Faculty of Science, Bijvoet Center for Biomolecular Research (Netherlands)

2012-12-15

We present a computational environment for Fast Analysis of multidimensional NMR DAta Sets (FANDAS) that allows assembling multidimensional data sets from a variety of input parameters and facilitates comparing and modifying such 'in silico' data sets during the various stages of the NMR data analysis. The input parameters can vary from (partial) NMR assignments directly obtained from experiments to values retrieved from in silico prediction programs. The resulting predicted data sets enable a rapid evaluation of sample labeling in light of spectral resolution and structural content, using standard NMR software such as Sparky. In addition, direct comparison to experimental data sets can be used to validate NMR assignments, distinguish different molecular components, refine structural models or other parameters derived from NMR data. The method is demonstrated in the context of solid-state NMR data obtained for the cyclic nucleotide binding domain of a bacterial cyclic nucleotide-gated channel and on membrane-embedded sensory rhodopsin II. FANDAS is freely available as web portal under WeNMR (http://www.wenmr.eu/services/FANDAShttp://www.wenmr.eu/services/FANDAS).

Solution NMR Spectroscopy in Target-Based Drug Discovery.

Science.gov (United States)

Li, Yan; Kang, Congbao

2017-08-23

Solution NMR spectroscopy is a powerful tool to study protein structures and dynamics under physiological conditions. This technique is particularly useful in target-based drug discovery projects as it provides protein-ligand binding information in solution. Accumulated studies have shown that NMR will play more and more important roles in multiple steps of the drug discovery process. In a fragment-based drug discovery process, ligand-observed and protein-observed NMR spectroscopy can be applied to screen fragments with low binding affinities. The screened fragments can be further optimized into drug-like molecules. In combination with other biophysical techniques, NMR will guide structure-based drug discovery. In this review, we describe the possible roles of NMR spectroscopy in drug discovery. We also illustrate the challenges encountered in the drug discovery process. We include several examples demonstrating the roles of NMR in target-based drug discoveries such as hit identification, ranking ligand binding affinities, and mapping the ligand binding site. We also speculate the possible roles of NMR in target engagement based on recent processes in in-cell NMR spectroscopy.

Bayesian deconvolution and quantification of metabolites in complex 1D NMR spectra using BATMAN.

Science.gov (United States)

Hao, Jie; Liebeke, Manuel; Astle, William; De Iorio, Maria; Bundy, Jacob G; Ebbels, Timothy M D

2014-01-01

Data processing for 1D NMR spectra is a key bottleneck for metabolomic and other complex-mixture studies, particularly where quantitative data on individual metabolites are required. We present a protocol for automated metabolite deconvolution and quantification from complex NMR spectra by using the Bayesian automated metabolite analyzer for NMR (BATMAN) R package. BATMAN models resonances on the basis of a user-controllable set of templates, each of which specifies the chemical shifts, J-couplings and relative peak intensities for a single metabolite. Peaks are allowed to shift position slightly between spectra, and peak widths are allowed to vary by user-specified amounts. NMR signals not captured by the templates are modeled non-parametrically by using wavelets. The protocol covers setting up user template libraries, optimizing algorithmic input parameters, improving prior information on peak positions, quality control and evaluation of outputs. The outputs include relative concentration estimates for named metabolites together with associated Bayesian uncertainty estimates, as well as the fit of the remainder of the spectrum using wavelets. Graphical diagnostics allow the user to examine the quality of the fit for multiple spectra simultaneously. This approach offers a workflow to analyze large numbers of spectra and is expected to be useful in a wide range of metabolomics studies.

Fragment-Linking Approach Using (19)F NMR Spectroscopy To Obtain Highly Potent and Selective Inhibitors of β-Secretase.

Science.gov (United States)

Jordan, John B; Whittington, Douglas A; Bartberger, Michael D; Sickmier, E Allen; Chen, Kui; Cheng, Yuan; Judd, Ted

2016-04-28

Fragment-based drug discovery (FBDD) has become a widely used tool in small-molecule drug discovery efforts. One of the most commonly used biophysical methods in detecting weak binding of fragments is nuclear magnetic resonance (NMR) spectroscopy. In particular, FBDD performed with (19)F NMR-based methods has been shown to provide several advantages over (1)H NMR using traditional magnetization-transfer and/or two-dimensional methods. Here, we demonstrate the utility and power of (19)F-based fragment screening by detailing the identification of a second-site fragment through (19)F NMR screening that binds to a specific pocket of the aspartic acid protease, β-secretase (BACE-1). The identification of this second-site fragment allowed the undertaking of a fragment-linking approach, which ultimately yielded a molecule exhibiting a more than 360-fold increase in potency while maintaining reasonable ligand efficiency and gaining much improved selectivity over cathepsin-D (CatD). X-ray crystallographic studies of the molecules demonstrated that the linked fragments exhibited binding modes consistent with those predicted from the targeted screening approach, through-space NMR data, and molecular modeling.

Protein-Glycan Quinary Interactions in Crowding Environment Unveiled by NMR Spectroscopy.

Science.gov (United States)

Diniz, Ana; Dias, Jorge S; Jiménez-Barbero, Jesús; Marcelo, Filipa; Cabrita, Eurico J

2017-09-21

Protein-glycan interactions as modulators for quinary structures in crowding environments were explored. The interaction between human galectin 3 (Gal-3) and distinct macromolecular crowders, such as bovine and human serum albumin (BSA and HSA), Ficoll 70 and PEG3350, was scrutinized. The molecular recognition event of the specific ligand, lactose, by Gal-3 in crowding conditions was evaluated. Gal-3 interactions were monitored by NMR analysing chemical shift perturbation (CSP) and line broadening of 1 H 15 N-HSQC signals. The intensity of the Gal-3 1 H 15 N-HSQC signals decreased in the presence of all crowders, due to the increase in the solution viscosity and to the formation of large protein complexes. When glycosylated containing samples of BSA and HSA were used, signal broadening was more severe than that observed in the presence of the more viscous solutions of PEG3350 and Ficoll 70. However, for the samples containing glycoproteins, the signal intensity of 1 H 15 N-HSQC recovered upon addition of lactose. We show that serum proteins interact with Gal-3, through their α2,3-linked sialylgalactose moieties exposed at their surfaces, competing with lactose for the same binding site. The quinary interaction between Gal-3 and serum glycoproteins, could help to co-localize Gal-3 at the cell surface, and may play a role in adhesion and signalling functions of this protein. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

NMR imaging of osteoarticular pathology

International Nuclear Information System (INIS)

Frocrain, L.; Duvauferrier, R.; Gagey, N.

1987-01-01

NMR imaging is assuming an increasingly important role in the diagnosis of osteo-articular disorders. Semiological descriptions of the mean pathological disorders of the locomotor system are presented. Some investigation strategies are proposed to compare NMR imaging with other imaging techniques in various pathological states [fr

A Simple Approach for Obtaining High Resolution, High Sensitivity ¹H NMR Metabolite Spectra of Biofluids with Limited Mass Supply

Energy Technology Data Exchange (ETDEWEB)

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

2006-11-01

A simple approach is reported that yields high resolution, high sensitivity ¹H NMR spectra of biofluids with limited mass supply. This is achieved by spinning a capillary sample tube containing a biofluid at the magic angle at a frequency of about 80Hz. A 2D pulse sequence called ¹H PASS is then used to produce a high-resolution ¹H NMR spectrum that is free from magnetic susceptibility induced line broadening. With this new approach a high resolution ¹H NMR spectrum of biofluids with a volume less than 1.0 µl can be easily achieved at a magnetic field strength as low as 7.05T. Furthermore, the methodology facilitates easy sample handling, i.e., the samples can be directly collected into inexpensive and disposable capillary tubes at the site of collection and subsequently used for NMR measurements. In addition, slow magic angle spinning improves magnetic field shimming and is especially suitable for high throughput investigations. In this paper first results are shown obtained in a magnetic field of 7.05T on urine samples collected from mice using a modified commercial NMR probe.

Antiferromagnetic Ordering in Quasi-Triangular Localized Spin System, β'-Et2Me2P[Pd(dmit)2]2, Studied by 13C NMR

Science.gov (United States)

Otsuka, Kei; Iikubo, Hideaki; Kogure, Takayuki; Takano, Yoshiki; Hiraki, Ko-ichi; Takahashi, Toshihiro; Cui, Hengbo; Kato, Reizo

2014-05-01

We performed 13C NMR measurements of a selectively 13C isotope-labeled single-crystal sample of a frustrated spin system, β'-Et2Me2P[Pd(dmit)2]2. A long-range antiferromagnetic (AF) ordering below 17 K was confirmed by the observation of NMR spectrum broadening and well split resonance lines at lower temperatures. NMR spectra in the AF state can be well explained by a two sublattice model. From the analysis of the angular dependence of the NMR spectrum, we clarified the magnetic structure in the AF state, where the easy and hard axes are the crystallographic c*- and b-axes, respectively, and the effective localized moments are quite small, ˜0.28 μB/dimer. This suggests a strong quantum fluctuation effect due to magnetic frustrations in a quasi-triangular spin-1/2 system.

Study on the Effects of Oligo chitosan and Bioliquifert on Two Rice Mutants, NMR 151 and NMR 152

International Nuclear Information System (INIS)

Shakinah Salleh; Faiz Ahmad; Sobri Hussein

2016-01-01

Nuclear Malaysia has successfully developed two new rice mutants namely NMR 151 and NMR 152. In addition, Nuclear Malaysia has also successfully developed Oligo chitosan and liquid bio fertilizer (Bioliquifert). Oligo chitosan acts as elicitor that has been proven to be very effective in controlling disease infections and improving yield productivity. Bioliquifert on the other hand is a mixture of microbes containing major nutrient-providing microorganisms. The objective of this study is to observe the effects of Oligo chitosan and Bioliquifert on rice mutants, NMR 151 and NMR 152. The treatment was applied on 14 day old seedlings of MR 219, NMR 151 and NMR 152 sowed in 20 cm pots containing silty clay from the paddy soil of Tanjung Karang, Selangor. The seedlings were then placed in the greenhouse at Nuclear Malaysia until it reaches 110 days old. Study was conducted in a Complete Randomized Design (CRD) with 3 replications was used and each replication consisted of three plants. All treatments received compound and single dressing fertilizer as recommended by National Rice Production Package except for Treatment 2 and 3, in which Treatment 2 received Oligo chitosan and Bioliquifert while Treatment 3 only received Bioliquifert. Results on plant height, number of tiller and plant fresh weight are not significantly different for all cultivar except for seed dry weight of NMR 152 and MR 219. (author)

High-precision drop shape analysis (HPDSA) of quasistatic contact angles on silanized silicon wafers with different surface topographies during inclining-plate measurements: Influence of the surface roughness on the contact line dynamics

International Nuclear Information System (INIS)

Heib, F.; Hempelmann, R.; Munief, W.M.; Ingebrandt, S.; Fug, F.; Possart, W.; Groß, K.; Schmitt, M.

2015-01-01

Highlights: • Analysis of the triple line motion on surfaces with nanoscale surface topographies. • Analysis of the triple line motion is performed in sub-pixel resolution. • A special fitting and statistical approach for contact angle analysis is applied. • The analyses result set of contact angle data which is independent of “user-skills”. • Characteristically density distributions in dependence on the surface properties. - Abstract: Contact angles and wetting of solid surfaces are strongly influenced by the physical and chemical properties of the surfaces. These influence quantities are difficult to distinguish from each other if contact angle measurements are performed by measuring only the advancing θ a and the receding θ r contact angle. In this regard, time-dependent water contact angles are measured on two hydrophobic modified silicon wafers with different physical surface topographies. The first surface is nearly atomically flat while the second surface is patterned (alternating flat and nanoscale rough patterns) which is synthesized by a photolithography and etching procedure. The different surface topographies are characterized with atomic force microscopy (AFM), Fourier transform infrared reflection absorption spectroscopy (FTIRRAS) and Fourier transform infrared attenuated total reflection spectroscopy (FTIR-ATR). The resulting set of contact angle data obtained by the high-precision drop shape analysis approach is further analyzed by a Gompertzian fitting procedure and a statistical counting procedure in dependence on the triple line velocity. The Gompertzian fit is used to analyze overall properties of the surface and dependencies between the motion on the front and the back edge of the droplets. The statistical counting procedure results in the calculation of expectation values E(p) and standard deviations σ(p) for the inclination angle φ, contact angle θ, triple line velocity vel and the covered distance of the triple line dis

High-precision drop shape analysis (HPDSA) of quasistatic contact angles on silanized silicon wafers with different surface topographies during inclining-plate measurements: Influence of the surface roughness on the contact line dynamics

Energy Technology Data Exchange (ETDEWEB)

Heib, F., E-mail: f.heib@mx.uni-saarland.de [Department of Physical Chemistry, Saarland University, 66123 Saarbrücken (Germany); Hempelmann, R. [Department of Physical Chemistry, Saarland University, 66123 Saarbrücken (Germany); Munief, W.M.; Ingebrandt, S. [Department of Informatics and Microsystem Technology, University of Applied Sciences, Kaiserslautern, 66482 Zweibrücken (Germany); Fug, F.; Possart, W. [Department of Adhesion and Interphases in Polymers, Saarland University, 66123 Saarbrücken (Germany); Groß, K.; Schmitt, M. [Department of Physical Chemistry, Saarland University, 66123 Saarbrücken (Germany)

2015-07-01

Highlights: • Analysis of the triple line motion on surfaces with nanoscale surface topographies. • Analysis of the triple line motion is performed in sub-pixel resolution. • A special fitting and statistical approach for contact angle analysis is applied. • The analyses result set of contact angle data which is independent of “user-skills”. • Characteristically density distributions in dependence on the surface properties. - Abstract: Contact angles and wetting of solid surfaces are strongly influenced by the physical and chemical properties of the surfaces. These influence quantities are difficult to distinguish from each other if contact angle measurements are performed by measuring only the advancing θ{sub a} and the receding θ{sub r} contact angle. In this regard, time-dependent water contact angles are measured on two hydrophobic modified silicon wafers with different physical surface topographies. The first surface is nearly atomically flat while the second surface is patterned (alternating flat and nanoscale rough patterns) which is synthesized by a photolithography and etching procedure. The different surface topographies are characterized with atomic force microscopy (AFM), Fourier transform infrared reflection absorption spectroscopy (FTIRRAS) and Fourier transform infrared attenuated total reflection spectroscopy (FTIR-ATR). The resulting set of contact angle data obtained by the high-precision drop shape analysis approach is further analyzed by a Gompertzian fitting procedure and a statistical counting procedure in dependence on the triple line velocity. The Gompertzian fit is used to analyze overall properties of the surface and dependencies between the motion on the front and the back edge of the droplets. The statistical counting procedure results in the calculation of expectation values E(p) and standard deviations σ(p) for the inclination angle φ, contact angle θ, triple line velocity vel and the covered distance of the triple

NMR study of local diamagnetic properties of carbon structures with multiwalled nanotubes

International Nuclear Information System (INIS)

Nikolaev, E.G.; Omel'yanovsky, O.E.; Prudkovsky, V.S.; Sadakov, A.V.; Tsebro, V.I.

2009-01-01

The reasons for the high diamagnetic susceptibility of carbon columns, which are covered with a nanotube mesh, from the interior part of cathode deposits have been studied by means of NMR. A comparative study is made of the 13 C NMR spectra and the magnetic susceptibility of carbon columns before and after ultrasonic processing as well as of finely dispersed material, obtained as a result of such processing, enriched with multilayer nanotubes. The strong diamagnetism of the carbon columns is apparently associated with a quite dense conglomerate of graphite particles, nanotubes, and multilayer polyhedral particles present in their core and not with the surface mesh of multilayer nanotubes. To make a more accurate determination of the character of the anisotropy of the magnetic susceptibility of multilayer carbon nanotubes, the form of the 13 C NMR spectra of samples enriched with multilayer nanotubes, where the nanotubes are either not oriented or only partially oriented, is analyzed. It is shown that the diamagnetic susceptibility of multilayer carbon nanotubes is highest when the magnetic field is oriented perpendicular to their axis

NMR experiments on a three-dimensional vibrofluidized granular medium

Science.gov (United States)

Huan, Chao; Yang, Xiaoyu; Candela, D.; Mair, R. W.; Walsworth, R. L.

2004-04-01

A three-dimensional granular system fluidized by vertical container vibrations was studied using pulsed field gradient NMR coupled with one-dimensional magnetic resonance imaging. The system consisted of mustard seeds vibrated vertically at 50 Hz, and the number of layers Nl⩽4 was sufficiently low to achieve a nearly time-independent granular fluid. Using NMR, the vertical profiles of density and granular temperature were directly measured, along with the distributions of vertical and horizontal grain velocities. The velocity distributions showed modest deviations from Maxwell-Boltzmann statistics, except for the vertical velocity distribution near the sample bottom, which was highly skewed and non-Gaussian. Data taken for three values of Nl and two dimensionless accelerations Γ=15,18 were fitted to a hydrodynamic theory, which successfully models the density and temperature profiles away from the vibrating container bottom. A temperature inversion near the free upper surface is observed, in agreement with predictions based on the hydrodynamic parameter μ which is nonzero only in inelastic systems.

An Inversion Recovery NMR Kinetics Experiment

OpenAIRE

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

2011-01-01

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