NMR at earth's magnetic field using para-hydrogen induced polarization.

Science.gov (United States)

Hamans, Bob C; Andreychenko, Anna; Heerschap, Arend; Wijmenga, Sybren S; Tessari, Marco

2011-09-01

A method to achieve NMR of dilute samples in the earth's magnetic field by applying para-hydrogen induced polarization is presented. Maximum achievable polarization enhancements were calculated by numerically simulating the experiment and compared to the experimental results and to the thermal equilibrium in the earth's magnetic field. Simultaneous 19F and 1H NMR detection on a sub-milliliter sample of a fluorinated alkyne at millimolar concentration (∼10(18) nuclear spins) was realized with just one single scan. A highly resolved spectrum with a signal/noise ratio higher than 50:1 was obtained without using an auxiliary magnet or any form of radio frequency shielding. Copyright © 2011 Elsevier Inc. All rights reserved.

Nuclear magnetic resonance of laser-polarized noble gases in molecules, materials and organisms

Energy Technology Data Exchange (ETDEWEB)

Goodson, Boyd McLean [Univ. of California, Berkeley, CA (United States)

1999-12-01

Conventional nuclear magnetic resonance (NMR) spectroscopy and magnetic resonance imaging (MRI) are fundamentally challenged by the insensitivity that stems from the ordinarily low spin polarization achievable in even the strongest NMR magnets. However, by transferring angular momentum from laser light to electronic and nuclear spins, optical pumping methods can increase the nuclear spin polarization of noble gases by several orders of magnitude, thereby greatly enhancing their NMR sensitivity. This dissertation is primarily concerned with the principles and practice of optically pumped nuclear magnetic resonance (OPNMR). The enormous sensitivity enhancement afforded by optical pumping noble gases can be exploited to permit a variety of novel NMR experiments across many disciplines. Many such experiments are reviewed, including the void-space imaging of organisms and materials, NMR and MRI of living tissues, probing structure and dynamics of molecules in solution and on surfaces, and zero-field NMR and MRI.

Nuclear magnetic resonance of laser-polarized noble gases in molecules, materials and organisms

International Nuclear Information System (INIS)

Goodson, Boyd M.

1999-01-01

Conventional nuclear magnetic resonance (NMR) spectroscopy and magnetic resonance imaging (MRI) are fundamentally challenged by the insensitivity that stems from the ordinarily low spin polarization achievable in even the strongest NMR magnets. However, by transferring angular momentum from laser light to electronic and nuclear spins, optical pumping methods can increase the nuclear spin polarization of noble gases by several orders of magnitude, thereby greatly enhancing their NMR sensitivity. This dissertation is primarily concerned with the principles and practice of optically pumped nuclear magnetic resonance (OPNMR). The enormous sensitivity enhancement afforded by optical pumping noble gases can be exploited to permit a variety of novel NMR experiments across many disciplines. Many such experiments are reviewed, including the void-space imaging of organisms and materials, NMR and MRI of living tissues, probing structure and dynamics of molecules in solution and on surfaces, and zero-field NMR and MRI

Dynamic Nuclear Polarization and other magnetic ideas at EPFL.

Science.gov (United States)

Bornet, Aurélien; Milani, Jonas; Wang, Shutao; Mammoli, Daniele; Buratto, Roberto; Salvi, Nicola; Segaw, Takuya F; Vitzthum, Veronika; Miéville, Pascal; Chinthalapalli, Srinivas; Perez-Linde, Angel J; Carnevale, Diego; Jannin, Sami; Caporinia, Marc; Ulzega, Simone; Rey, Martial; Bodenhausen, Geoffrey

2012-01-01

Although nuclear magnetic resonance (NMR) can provide a wealth of information, it often suffers from a lack of sensitivity. Dynamic Nuclear Polarization (DNP) provides a way to increase the polarization and hence the signal intensities in NMR spectra by transferring the favourable electron spin polarization of paramagnetic centres to the surrounding nuclear spins through appropriate microwave irradiation. In our group at EPFL, two complementary DNP techniques are under investigation: the combination of DNP with magic angle spinning at temperatures near 100 K ('MAS-DNP'), and the combination of DNP at 1.2 K with rapid heating followed by the transfer of the sample to a high-resolution magnet ('dissolution DNP'). Recent applications of MAS-DNP to surfaces, as well as new developments of magnetization transfer of (1)H to (13)C at 1.2 K prior to dissolution will illustrate the work performed in our group. A second part of the paper will give an overview of some 'non-enhanced' activities of our laboratory in liquid- and solid-state NMR.

Study of xenon binding in cryptophane-A using laser-induced NMR polarization enhancement

International Nuclear Information System (INIS)

Luhmer, M.; Goodson, B.M.; Song, Y.Q.; Laws, D.D.; Kaiser, L.; Pines, A.; Lawrence Berkeley National Lab., CA

1999-01-01

Xenon is chemically inert, yet exhibits NMR parameters that are highly sensitive to its chemical environment. Considerable work has therefore capitalized on the utility of 129 Xe (I = 1/2) as a magnetic resonance probe of molecules, materials, and biological systems. In solution, spin-polarization transfer between laser-polarized xenon and the hydrogen nuclei of nearby molecules leads to signal enhancements in the resolved 1 H NMR spectrum, offering new opportunities for probing the chemical environment of xenon atoms. Following binding of laser-polarized xenon to molecules of cryptophane-A, selective enhancements of the 1 H NMR signals were observed. A theoretical framework for the interpretation of such experimental results is provided, and the spin polarization-induced nuclear Overhauser effects are shown to yield information about the molecular environment of xenon. The observed selective 1 H enhancements allowed xenon-proton internuclear distances to be estimated. These distances reveal structural characteristics of the complex, including the preferred molecular conformations adopted by cryptophane-A upon binding of xenon

High-Frequency Dynamic Nuclear Polarization in the Nuclear Rotating Frame

DEFF Research Database (Denmark)

Farrar, C. T.; Hall, D. A.; Gerfen, G. J.

2000-01-01

A proton dynamic nuclear polarization (DNP) NMR signal enhancement (ϵ) close to thermal equilibrium, ϵ = 0.89, has been obtained at high field (B0 = 5 T, νepr = 139.5 GHz) using 15 mM trityl radical in a 40:60 water/glycerol frozen solution at 11 K. The electron-nuclear polarization transfer...... is performed in the nuclear rotating frame with microwave irradiation during a nuclear spin-lock pulse. The growth of the signal enhancement is governed by the rotating frame nuclear spin–lattice relaxation time (T1ρ), which is four orders of magnitude shorter than the nuclear spin–lattice relaxation time (T1n......). Due to the rapid polarization transfer in the nuclear rotating frame the experiment can be recycled at a rate of 1/T1ρ and is not limited by the much slower lab frame nuclear spin–lattice relaxation rate (1/T1n). The increased repetition rate allowed in the nuclear rotating frame provides an effective...

Nuclear magnetic resonance in pulse radiolysis. Chemically induced dynamic nuclear polarization

International Nuclear Information System (INIS)

Trifunac, A.D.; Johnson, K.W.; Lowers, R.H.

1976-01-01

Nuclear magnetic resonance and chemically induced dynamic nuclear polarization (CIDNP) were applied to the study of pulse radiolysis. Samples were irradiated with a 3-MeV electron beam from the Argonne Van de Graaff accelerator in an EPR magnet (approximately 4000 G) which had axial holes for beam access. A fast flow system transferred the irradiated solution to the rotating 5-mm NMR sample tube. The NMR spectra of mixtures of sodium acetate and methanol were presented to demonstrate the features of the CIDNP in pulse radiolysis

Ultra-Low Field SQUID-NMR using LN2 Cooled Cu Polarizing Field coil

Science.gov (United States)

Demachi, K.; Kawagoe, S.; Ariyoshi, S.; Tanaka, S.

2017-07-01

We are developing an Ultra-Low Field (ULF) Magnetic Resonance Imaging (MRI) system using a High-Temperature Superconductor superconducting quantum interference device (HTS rf-SQUID) for food inspection. The advantages of the ULF-NMR (Nuclear Magnetic Resonance) / MRI as compared with a conventional high field MRI are that they are compact and of low cost. In this study, we developed a ULF SQUID-NMR system using a polarizing coil to measure fat of which relaxation time T1 is shorter. The handmade polarizing coil was cooled by liquid nitrogen to reduce the resistance and accordingly increase the allowable current. The measured decay time of the polarizing field was 40 ms. The measurement system consisted of the liquid nitrogen cooled polarizing coil, a SQUID, a Cu wound flux transformer, a measurement field coil for the field of 47 μT, and an AC pulse coil for a 90°pulse field. The NMR measurements were performed in a magnetically shielded room to reduce the environmental magnetic field. The size of the sample was ϕ35 mm × L80 mm. After applying a polarizing field and a 90°pulse, an NMR signal was detected by the SQUID through the flux transformer. As a result, the NMR spectra of fat samples were obtained at 2.0 kHz corresponding to the measurement field Bm of 47 μT. The T1 relaxation time of the mineral oil measured in Bm was 45 ms. These results suggested that the ULF-NMR/MRI system has potential for food inspection.

Dynamic nuclear-polarization studies of paramagnetic species in solution

International Nuclear Information System (INIS)

Glad, W.E.

1982-07-01

Dynamic Nuclear Polarization (DNP) was used to measure the electron spin lattice relaxation times, T 1 , of transition metal ions in aqueous solution. Saturation which is induced in the electron spin system is transferred to the solvent proton spins by dipole-dipole interactions. The change in the polarization of the proton spins is much larger than it is in the electron spins. The change in proton polarization is easily measured by proton Nuclear Magnetic Resonance (NMR). In one experimental arrangement the sample solution was continuously flowed through a microwave cavity to the NMR coil. The NMR was observed with a continuous wave NMR spectrometer. In a second arrangement the whole sample tube was moved from within the microwave cavity to the NMR coil in less than 40 ms by a blast of compressed air. The NMR was then observed with a pulse-Fourier-transform spectrometer. With the second arrangement a mean-square microwave magnetic field at the sample of more than 10 G 2 is obtainable with 14 W of microwave power. Measurements of DNP at 9 GHz were made on aqueous solutions of VO 2+ , Mn 2+ , Cr(CN) 6 3- , Cu 2+ and Cu(ethylenediamine) 2 (H 2 0) 2 2+ ions from 3 to 60 0 C. It was also possible to observe DNP on resolved proton resonances from mixed water-acetonitrile solutions of VO 2+ and Cr(CN) 6 3- ions

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

Science.gov (United States)

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

2013-01-01

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

Low-Temperature Dynamic Nuclear Polarization at 9.4 Tesla With a 30 Milliwatt Microwave Source

Science.gov (United States)

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

2010-01-01

Dynamic nuclear polarization (DNP) can provide large signal enhancements in nuclear magnetic resonance (NMR) by transfer of polarization from electron spins to nuclear spins. We discuss several aspects of DNP experiments at 9.4 Tesla (400 MHz resonant frequency for 1H, 264 GHz for electron spins in organic radicals) in the 7–80 K temperature range, using a 30 mW, frequency-tunable microwave source and a quasi-optical microwave bridge for polarization control and low-loss microwave transmission. In experiments on frozen glycerol/water doped with nitroxide radicals, DNP signal enhancements up to a factor of 80 are observed (relative to 1H NMR signals with thermal equilibrium spin polarization). The largest sensitivity enhancements are observed with a new triradical dopant, DOTOPA-TEMPO. Field modulation with a 10 G root-mean-squared amplitude during DNP increases the nuclear spin polarizations by up to 135%. Dependencies of 1H NMR signal amplitudes, nuclear spin relaxation times, and DNP build-up times on the dopant and its concentration, temperature, microwave power, and modulation frequency are reported and discussed. The benefits of low-temperature DNP can be dramatic: the 1H spin polarization is increased approximately 1000-fold at 7 K with DNP, relative to thermal polarization at 80 K. PMID:20392658

NMR parallel Q-meter with double-balanced-mixer detection for polarized target experiments

International Nuclear Information System (INIS)

Boissevain, J.; Tippens, W.B.

1983-01-01

A constant-voltage, parallel-tuned nuclear magnetic resonance (NMR) circuit, patterned after a Liverpool design, has been developed for polarized target experiments. Measuring the admittance of the resonance circuit allows advantageous use of double-balanced mixer detection. The resonant circuit is tolerant of stray capacitance between the NMR coil and the target cavity, thus easing target-cell-design constraints. The reference leg of the circuit includes a voltage-controlled attenuator and phase shifter for ease of tuning. The NMR output features a flat background and has good linearity and stability

Low-temperature dynamic nuclear polarization at 9.4 T with a 30 mW microwave source.

Science.gov (United States)

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

2010-06-01

Dynamic nuclear polarization (DNP) can provide large signal enhancements in nuclear magnetic resonance (NMR) by transfer of polarization from electron spins to nuclear spins. We discuss several aspects of DNP experiments at 9.4 T (400 MHz resonant frequency for (1)H, 264 GHz for electron spins in organic radicals) in the 7-80K temperature range, using a 30 mW, frequency-tunable microwave source and a quasi-optical microwave bridge for polarization control and low-loss microwave transmission. In experiments on frozen glycerol/water doped with nitroxide radicals, DNP signal enhancements up to a factor of 80 are observed (relative to (1)H NMR signals with thermal equilibrium spin polarization). The largest sensitivity enhancements are observed with a new triradical dopant, DOTOPA-TEMPO. Field modulation with a 10 G root-mean-squared amplitude during DNP increases the nuclear spin polarizations by up to 135%. Dependencies of (1)H NMR signal amplitudes, nuclear spin relaxation times, and DNP build-up times on the dopant and its concentration, temperature, microwave power, and modulation frequency are reported and discussed. The benefits of low-temperature DNP can be dramatic: the (1)H spin polarization is increased approximately 1000-fold at 7 K with DNP, relative to thermal polarization at 80K. (c) 2010 Elsevier Inc. All rights reserved.

Cluster formation restricts dynamic nuclear polarization of xenon in solid mixtures

DEFF Research Database (Denmark)

Kuzma, N. N.; Pourfathi, M.; Kara, H.

2012-01-01

During dynamic nuclear polarization (DNP) at 1.5 K and 5 T, Xe-129 nuclear magnetic resonance (NMR) spectra of a homogeneous xenon/1-propanol/trityl-radical solid mixture exhibit a single peak, broadened by H-1 neighbors. A second peak appears upon annealing for several hours at 125 K. Its...

NMR study of hyper-polarized {sup 129}Xe and applications to liquid-phase NMR experiments; Etude de la resonance magnetique nucleaire du Xenon{sup 129} hyperpolarise et applications en RMN des liquides

Energy Technology Data Exchange (ETDEWEB)

Marion, D

2008-07-15

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)

Sub-minute kinetics of human red cell fumarase: 1 H spin-echo NMR spectroscopy and 13 C rapid-dissolution dynamic nuclear polarization.

Science.gov (United States)

Shishmarev, Dmitry; Wright, Alan J; Rodrigues, Tiago B; Pileio, Giuseppe; Stevanato, Gabriele; Brindle, Kevin M; Kuchel, Philip W

2018-03-01

Fumarate is an important probe of metabolism in hyperpolarized magnetic resonance imaging and spectroscopy. It is used to detect the release of fumarase in cancer tissues, which is associated with necrosis and drug treatment. Nevertheless, there are limited reports describing the detailed kinetic studies of this enzyme in various cells and tissues. Thus, we aimed to evaluate the sub-minute kinetics of human red blood cell fumarase using nuclear magnetic resonance (NMR) spectroscopy, and to provide a quantitative description of the enzyme that is relevant to the use of fumarate as a probe of cell rupture. The fumarase reaction was studied using time courses of 1 H spin-echo and 13 C-NMR spectra. 1 H-NMR experiments showed that the fumarase reaction in hemolysates is sufficiently rapid to make its kinetics amenable to study in a period of approximately 3 min, a timescale characteristic of hyperpolarized 13 C-NMR spectroscopy. The rapid-dissolution dynamic nuclear polarization (RD-DNP) technique was used to hyperpolarize [1,4- 13 C]fumarate, which was injected into concentrated hemolysates. The kinetic data were analyzed using recently developed FmR α analysis and modeling of the enzymatic reaction using Michaelis-Menten equations. In RD-DNP experiments, the decline in the 13 C-NMR signal from fumarate, and the concurrent rise and fall of that from malate, were captured with high spectral resolution and signal-to-noise ratio, which allowed the robust quantification of fumarase kinetics. The kinetic parameters obtained indicate the potential contribution of hemolysis to the overall rate of the fumarase reaction when 13 C-NMR RD-DNP is used to detect necrosis in animal models of implanted tumors. The analytical procedures developed will be applicable to studies of other rapid enzymatic reactions using conventional and hyperpolarized substrate NMR spectroscopy. Copyright © 2018 John Wiley & Sons, Ltd.

Stable isotope-resolved analysis with quantitative dissolution dynamic nuclear polarization

DEFF Research Database (Denmark)

Lerche, Mathilde Hauge; Yigit, Demet; Frahm, Anne Birk

2018-01-01

Metabolite profiles and their isotopomer distributions can be studied non-invasively in complex mixtures with NMR. The advent of dissolution Dynamic Nuclear Polarization (dDNP) and isotope enrichment add sensitivity and resolution to such met-abolic studies. Metabolic pathways and networks can be...

Frozen Acrylamide Gels as Dynamic Nuclear Polarization Matrices.

KAUST Repository

Viger-Gravel, Jasmine; Berruyer, Pierrick; Gajan, David; Basset, Jean-Marie; Lesage, Anne; Tordo, Paul; Ouari, Olivier; Emsley, Lyndon

2017-01-01

We show that aqueous acrylamide gels can be used to provide dynamic nuclear polarization (DNP) NMR signal enhancements of around 200 at 9.4 T and 100 K. The enhancements are shown to increase with cross linker concentration and low concentrations of the AMUPol biradical. We show that this DNP matrix can be used in situations where conventional incipient wetness methods fail, such as to obtain DNP surface enhanced NMR spectra from inorganic nanoparticles. In particular, we obtain 113Cd spectra from CdTe-COOH NPs in minutes. The spectra clearly indicate a highly-disordered cadmium rich surface.

Frozen Acrylamide Gels as Dynamic Nuclear Polarization Matrices.

KAUST Repository

Viger-Gravel, Jasmine

2017-05-24

We show that aqueous acrylamide gels can be used to provide dynamic nuclear polarization (DNP) NMR signal enhancements of around 200 at 9.4 T and 100 K. The enhancements are shown to increase with cross linker concentration and low concentrations of the AMUPol biradical. We show that this DNP matrix can be used in situations where conventional incipient wetness methods fail, such as to obtain DNP surface enhanced NMR spectra from inorganic nanoparticles. In particular, we obtain 113Cd spectra from CdTe-COOH NPs in minutes. The spectra clearly indicate a highly-disordered cadmium rich surface.

NMR-Based Identification of Metabolites in Polar and Non-Polar Extracts of Avian Liver.

Science.gov (United States)

Fathi, Fariba; Brun, Antonio; Rott, Katherine H; Falco Cobra, Paulo; Tonelli, Marco; Eghbalnia, Hamid R; Caviedes-Vidal, Enrique; Karasov, William H; Markley, John L

2017-11-16

Metabolites present in liver provide important clues regarding the physiological state of an organism. The aim of this work was to evaluate a protocol for high-throughput NMR-based analysis of polar and non-polar metabolites from a small quantity of liver tissue. We extracted the tissue with a methanol/chloroform/water mixture and isolated the polar metabolites from the methanol/water layer and the non-polar metabolites from the chloroform layer. Following drying, we re-solubilized the fractions for analysis with a 600 MHz NMR spectrometer equipped with a 1.7 mm cryogenic probe. In order to evaluate the feasibility of this protocol for metabolomics studies, we analyzed the metabolic profile of livers from house sparrow ( Passer domesticus ) nestlings raised on two different diets: livers from 10 nestlings raised on a high protein diet (HP) for 4 d and livers from 12 nestlings raised on the HP diet for 3 d and then switched to a high carbohydrate diet (HC) for 1 d. The protocol enabled the detection of 52 polar and nine non-polar metabolites in ¹H NMR spectra of the extracts. We analyzed the lipophilic metabolites by one-way ANOVA to assess statistically significant concentration differences between the two groups. The results of our studies demonstrate that the protocol described here can be exploited for high-throughput screening of small quantities of liver tissue (approx. 100 mg wet mass) obtainable from small animals.

Structure of Lipid Nanoparticles Containing siRNA or mRNA by Dynamic Nuclear Polarization-Enhanced NMR Spectroscopy.

Science.gov (United States)

Viger-Gravel, Jasmine; Schantz, Anna; Pinon, Arthur C; Rossini, Aaron J; Schantz, Staffan; Emsley, Lyndon

2018-02-22

Here, we show how dynamic nuclear polarization (DNP) NMR spectroscopy experiments permit the atomic level structural characterization of loaded and empty lipid nanoparticles (LNPs). The LNPs used here were synthesized by the microfluidic mixing technique and are composed of ionizable cationic lipid (DLin-MC3-DMA), a phospholipid (distearoylphosphatidylcholine, DSPC), cholesterol, and poly(ethylene glycol) (PEG) (dimyristoyl phosphatidyl ethanolamine (DMPE)-PEG 2000), as well as encapsulated cargoes that are either phosphorothioated siRNA (50 or 100%) or mRNA. We show that LNPs form physically stable complexes with bioactive drug siRNA for a period of 94 days. Relayed DNP experiments are performed to study 1 H- 1 H spin diffusion and to determine the spatial location of the various components of the LNP by studying the average enhancement factors as a function of polarization time. We observe a striking feature of LNPs in the presence and in the absence of encapsulating siRNA or mRNA by comparing our experimental results to numerical spin-diffusion modeling. We observe that LNPs form a layered structure, and we detect that DSPC and DMPE-PEG 2000 lipids form a surface rich layer in the presence (or absence) of the cargoes and that the cholesterol and ionizable cationic lipid are embedded in the core. Furthermore, relayed DNP 31 P solid-state NMR experiments allow the location of the cargo encapsulated in the LNPs to be determined. On the basis of the results, we propose a new structural model for the LNPs that features a homogeneous core with a tendency for layering of DSPC and DMPE-PEG at the surface.

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

Science.gov (United States)

Thurber, Kent; Tycko, Robert

2016-03-01

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

Recursive polarization of nuclear spins in diamond at arbitrary magnetic fields

International Nuclear Information System (INIS)

Pagliero, Daniela; Laraoui, Abdelghani; Henshaw, Jacob D.; Meriles, Carlos A.

2014-01-01

We introduce an alternate route to dynamically polarize the nuclear spin host of nitrogen-vacancy (NV) centers in diamond. Our approach articulates optical, microwave, and radio-frequency pulses to recursively transfer spin polarization from the NV electronic spin. Using two complementary variants of the same underlying principle, we demonstrate nitrogen nuclear spin initialization approaching 80% at room temperature both in ensemble and single NV centers. Unlike existing schemes, our approach does not rely on level anti-crossings and is thus applicable at arbitrary magnetic fields. This versatility should prove useful in applications ranging from nanoscale metrology to sensitivity-enhanced NMR

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.

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

Optically enhanced nuclear cross polarization in acridine-doped fluorene

Energy Technology Data Exchange (ETDEWEB)

Oshiro, C.M.

1982-06-01

The objective of this work has been to create large polarizations of the dilute /sup 13/C nuclei in the solid state. The idea was to create /sup 1/H polarizations larger than Boltzmann and to use the proton enhanced nuclear induction spectroscopy cross polarization technique to then transfer this large polarization to the /sup 13/C spin system. Optical Nuclear Polarization (ONP) of acridine-doped fluorene single crystals was studied. In addition, ONP of powdered samples of the acridine-doped fluorene was studied. In general, many compounds do not crystallize easily or do not form large crystals suitable for NMR experiments. Powdered, amorphous and randomly dispersed samples are generally far more readily available than single crystals. One objective of this work has been to (first) create large /sup 1/H polarizations. Although large optical proton polarizations in single crystals have been reported previously, optically generated polarizations in powdered samples have not been reported. For these reasons, ONP studies of powdered samples of the acridine-doped fluorene were also undertaken. Using ONP in combination with the proton enhanced nuclear induction spectroscopy experiment, large /sup 13/C polarizations have been created in fluorene single crystals. These large /sup 13/C polarizations have permitted the determination of the seven incongruent chemical shielding tensors of the fluorene molecule. Part 2 of this thesis describes the proton enhanced nuclear induction spectroscopy experiment. Part 3 describes the ONP experiment. Part 4 is a description of the experimental set-up. Part 5 describes the data analysis for the determination of the chemical shielding tensors. Part 6 presents the results of the ONP experiments performed in this work and the chemical shielding tensors determined.

Optically enhanced nuclear cross polarization in acridine-doped fluorene

International Nuclear Information System (INIS)

Oshiro, C.M.

1982-06-01

The objective of this work has been to create large polarizations of the dilute 13 C nuclei in the solid state. The idea was to create 1 H polarizations larger than Boltzmann and to use the proton enhanced nuclear induction spectroscopy cross polarization technique to then transfer this large polarization to the 13 C spin system. Optical Nuclear Polarization (ONP) of acridine-doped fluorene single crystals was studied. In addition, ONP of powdered samples of the acridine-doped fluorene was studied. In general, many compounds do not crystallize easily or do not form large crystals suitable for NMR experiments. Powdered, amorphous and randomly dispersed samples are generally far more readily available than single crystals. One objective of this work has been to (first) create large 1 H polarizations. Although large optical proton polarizations in single crystals have been reported previously, optically generated polarizations in powdered samples have not been reported. For these reasons, ONP studies of powdered samples of the acridine-doped fluorene were also undertaken. Using ONP in combination with the proton enhanced nuclear induction spectroscopy experiment, large 13 C polarizations have been created in fluorene single crystals. These large 13 C polarizations have permitted the determination of the seven incongruent chemical shielding tensors of the fluorene molecule. Part 2 of this thesis describes the proton enhanced nuclear induction spectroscopy experiment. Part 3 describes the ONP experiment. Part 4 is a description of the experimental set-up. Part 5 describes the data analysis for the determination of the chemical shielding tensors. Part 6 presents the results of the ONP experiments performed in this work and the chemical shielding tensors determined

Solid state nuclear magnetic resonance studies of cross polarization from quadrupolar nuclei

Energy Technology Data Exchange (ETDEWEB)

De Paul, Susan M. [Univ. of California, Berkeley, CA (United States)

1997-08-01

The development of solid-state Nuclear Magnetic Resonance (NMR) has, to a large extent, focused on using spin-1/2 nuclei as probes to investigate molecular structure and dynamics. For such nuclei, the technique of cross polarization is well-established as a method for sensitivity enhancement. However, over two-thirds of the nuclei in the periodic table have a spin-quantum number greater than one-half and are known as quadrupolar nuclei. Such nuclei are fundamental constituents of many inorganic materials including minerals, zeolites, glasses, and gels. It is, therefore, of interest to explore the extent to which polarization can be transferred from quadrupolar nuclei. In this dissertation, solid-state NMR experiments involving cross polarization from quadrupolar nuclei to spin-1/2 nuclei under magic-angle spinning (MAS) conditions are investigated in detail.

Prospects for sub-micron solid state nuclear magnetic resonance imaging with low-temperature dynamic nuclear polarization.

Science.gov (United States)

Thurber, Kent R; Tycko, Robert

2010-06-14

We evaluate the feasibility of (1)H nuclear magnetic resonance (NMR) imaging with sub-micron voxel dimensions using a combination of low temperatures and dynamic nuclear polarization (DNP). Experiments are performed on nitroxide-doped glycerol-water at 9.4 T and temperatures below 40 K, using a 30 mW tunable microwave source for DNP. With DNP at 7 K, a 0.5 microL sample yields a (1)H NMR signal-to-noise ratio of 770 in two scans with pulsed spin-lock detection and after 80 db signal attenuation. With reasonable extrapolations, we infer that (1)H NMR signals from 1 microm(3) voxel volumes should be readily detectable, and voxels as small as 0.03 microm(3) may eventually be detectable. Through homonuclear decoupling with a frequency-switched Lee-Goldburg spin echo technique, we obtain 830 Hz (1)H NMR linewidths at low temperatures, implying that pulsed field gradients equal to 0.4 G/d or less would be required during spatial encoding dimensions of an imaging sequence, where d is the resolution in each dimension.

Resonance-inclined optical nuclear spin polarization of liquids in diamond structures

Science.gov (United States)

Chen, Q.; Schwarz, I.; Jelezko, F.; Retzker, A.; Plenio, M. B.

2016-02-01

Dynamic nuclear polarization (DNP) of molecules in a solution at room temperature has the potential to revolutionize nuclear magnetic resonance spectroscopy and imaging. The prevalent methods for achieving DNP in solutions are typically most effective in the regime of small interaction correlation times between the electron and nuclear spins, limiting the size of accessible molecules. To solve this limitation, we design a mechanism for DNP in the liquid phase that is applicable for large interaction correlation times. Importantly, while this mechanism makes use of a resonance condition similar to solid-state DNP, the polarization transfer is robust to a relatively large detuning from the resonance due to molecular motion. We combine this scheme with optically polarized nitrogen-vacancy (NV) center spins in nanodiamonds to design a setup that employs optical pumping and is therefore not limited by room temperature electron thermal polarization. We illustrate numerically the effectiveness of the model in a flow cell containing nanodiamonds immobilized in a hydrogel, polarizing flowing water molecules 4700-fold above thermal polarization in a magnetic field of 0.35 T, in volumes detectable by current NMR scanners.

Photochemically induced dynamic nuclear polarization NMR study of yeast and horse muscle phosphoglycerate kinase

International Nuclear Information System (INIS)

Scheffler, J.E.; Cohn, M.

1986-01-01

A photochemically induced dynamic nuclear polarization (photo-CIDNP) study of yeast and horse muscle phosphoglycerate kinase with flavin dyes was undertaken to identify the histidine, tryptophan, and tyrosine resonances in the aromatic region of the simplified 1 H NMR spectra of these enzymes and to investigate the effect of substrates on the resonances observable by CIDNP. Identification of the CIDNP-enhanced resonances with respect to the type of amino acid residue has been achieved since only tyrosine yields emission peaks and the dye 8-aminoriboflavin enhances tryptophan but not histidine. By use of the known amino acid sequences and structures derived from X-ray crystallographic studies of the enzymes from the two species, assignment of the specific residues in the protein sequences giving rise to the CIDNP spectra was partially achieved. In addition, flavin dye accessibility was used to probe any changes in enzyme structure induced by substrate binding. The accessibility of a tyrosine to photoexcited flavin is reduced in the presence of MgATP. Since the tyrosine residues are located some distance from the MgATP binding site of the catalytic center, it is proposed either that this change is due to a distant conformational change or that a second metal-ATP site inferred from other studies lies close to one of the tyrosines. Horse muscle phosphoglycerate kinase exhibits seven resonances by CIDNP NMR. The addition of 3-phosphoglycerate and MgATP results in the appearance of two additional resonances in the CIDNP spectrum due to a histidine residue that is inaccessible to flavin in both the enzyme alone and its binary complex with 3-phosphoglycerate. The CIDNP spectra are consistent with the suggestions that binding of 3-phosphoglycerate alone is insufficient to effect domain movement and that binding of both substrates are required for conversion of the horse muscle enzyme to its catalytically active form

Dynamic nuclear polarization of nucleic acid with endogenously bound manganese

International Nuclear Information System (INIS)

Wenk, Patricia; Kaushik, Monu; Richter, Diane; Vogel, Marc; Suess, Beatrix; Corzilius, Björn

2015-01-01

We report the direct dynamic nuclear polarization (DNP) of 13 C nuclei of a uniformly [ 13 C, 15 N]-labeled, paramagnetic full-length hammerhead ribozyme (HHRz) complex with Mn 2+ where the enhanced polarization is fully provided by the endogenously bound metal ion and no exogenous polarizing agent is added. A 13 C enhancement factor of ε = 8 was observed by intra-complex DNP at 9.4 T. In contrast, “conventional” indirect and direct DNP experiments were performed using AMUPol as polarizing agent where we obtained a 1 H enhancement factor of ε ≈ 250. Comparison with the diamagnetic (Mg 2+ ) HHRz complex shows that the presence of Mn 2+ only marginally influences the (DNP-enhanced) NMR properties of the RNA. Furthermore two-dimensional correlation spectra ( 15 N– 13 C and 13 C– 13 C) reveal structural inhomogeneity in the frozen, amorphous state indicating the coexistence of several conformational states. These demonstrations of intra-complex DNP using an endogenous metal ion as well as DNP-enhanced MAS NMR of RNA in general yield important information for the development of new methods in structural biology

NMR at earth's magnetic field using para-hydrogen induced polarization

NARCIS (Netherlands)

Hamans, B.C.; Andreychenko, A.; Heerschap, A.; Wijmenga, S.S.; Tessari, M.

2011-01-01

A method to achieve NMR of dilute samples in the earth's magnetic field by applying para-hydrogen induced polarization is presented. Maximum achievable polarization enhancements were calculated by numerically simulating the experiment and compared to the experimental results and to the thermal

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-12-21

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

Observation of strongly forbidden solid effect dynamic nuclear polarization transitions via electron-electron double resonance detected NMR

Energy Technology Data Exchange (ETDEWEB)

Smith, Albert A.; Corzilius, Björn; Haze, Olesya; Swager, Timothy M.; Griffin, Robert G., E-mail: rgg@mit.edu [Department of Chemistry and Francis Bitter Magnet Laboratory, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States)

2013-12-07

We present electron paramagnetic resonance experiments for which solid effect dynamic nuclear polarization transitions were observed indirectly via polarization loss on the electron. This use of indirect observation allows characterization of the dynamic nuclear polarization (DNP) process close to the electron. Frequency profiles of the electron-detected solid effect obtained using trityl radical showed intense saturation of the electron at the usual solid effect condition, which involves a single electron and nucleus. However, higher order solid effect transitions involving two, three, or four nuclei were also observed with surprising intensity, although these transitions did not lead to bulk nuclear polarization—suggesting that higher order transitions are important primarily in the transfer of polarization to nuclei nearby the electron. Similar results were obtained for the SA-BDPA radical where strong electron-nuclear couplings produced splittings in the spectrum of the indirectly observed solid effect conditions. Observation of high order solid effect transitions supports recent studies of the solid effect, and suggests that a multi-spin solid effect mechanism may play a major role in polarization transfer via DNP.

Dynamic nuclear polarization of nucleic acid with endogenously bound manganese

Energy Technology Data Exchange (ETDEWEB)

Wenk, Patricia [University of Tübingen, Werner Siemens Imaging Center and Department of Preclinical Imaging and Radiopharmacy (Germany); Kaushik, Monu; Richter, Diane [Goethe University, Institute of Physical und Theoretical Chemistry, Institute of Biophysical Chemistry und Center for Biomolecular Magnetic Resonance (BMRZ) (Germany); Vogel, Marc; Suess, Beatrix [Technical University Darmstadt, Department of Biology (Germany); Corzilius, Björn, E-mail: corzilius@em.uni-frankfurt.de [Goethe University, Institute of Physical und Theoretical Chemistry, Institute of Biophysical Chemistry und Center for Biomolecular Magnetic Resonance (BMRZ) (Germany)

2015-09-15

We report the direct dynamic nuclear polarization (DNP) of {sup 13}C nuclei of a uniformly [{sup 13}C,{sup 15}N]-labeled, paramagnetic full-length hammerhead ribozyme (HHRz) complex with Mn{sup 2+} where the enhanced polarization is fully provided by the endogenously bound metal ion and no exogenous polarizing agent is added. A {sup 13}C enhancement factor of ε = 8 was observed by intra-complex DNP at 9.4 T. In contrast, “conventional” indirect and direct DNP experiments were performed using AMUPol as polarizing agent where we obtained a {sup 1}H enhancement factor of ε ≈ 250. Comparison with the diamagnetic (Mg{sup 2+}) HHRz complex shows that the presence of Mn{sup 2+} only marginally influences the (DNP-enhanced) NMR properties of the RNA. Furthermore two-dimensional correlation spectra ({sup 15}N–{sup 13}C and {sup 13}C–{sup 13}C) reveal structural inhomogeneity in the frozen, amorphous state indicating the coexistence of several conformational states. These demonstrations of intra-complex DNP using an endogenous metal ion as well as DNP-enhanced MAS NMR of RNA in general yield important information for the development of new methods in structural biology.

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)

A fragment separator at LBL for beta-NMR experiment

International Nuclear Information System (INIS)

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

1992-03-01

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

Bis-gadolinium complexes for solid effect and cross effect dynamic nuclear polarization

Energy Technology Data Exchange (ETDEWEB)

Kaushik, Monu; Corzilius, Bjoern [Goethe-Universitaet Frankfurt am Main, Institut fuer Physikalische und Theoretische Chemie, Institut fuer Biophysikalische Chemie und Biomolekulares Magnetresonanzzentrum (BMRZ) (Germany); Qi, Mian; Godt, Adelheid [Fakultaet fuer Chemie und Centrum fuer Molekulare Materialien (CM2), Universitaet Bielefeld (Germany)

2017-04-03

High-spin complexes act as polarizing agents (PAs) for dynamic nuclear polarization (DNP) in solid-state NMR spectroscopy and feature promising aspects towards biomolecular DNP. We present a study on bis(Gd-chelate)s which enable cross effect (CE) DNP owing to spatial confinement of two dipolar-coupled electron spins. Their well-defined Gd..Gd distances in the range of 1.2-3.4 nm allowed us to elucidate the Gd..Gd distance dependence of the DNP mechanism and NMR signal enhancement. We found that Gd..Gd distances above 2.1 nm result in solid effect DNP while distances between 1.2 and 2.1 nm enable CE for {sup 1}H, {sup 13}C, and {sup 15}N nuclear spins. We compare 263 GHz electron paramagnetic resonance (EPR) spectra with the obtained DNP field profiles and discuss possible CE matching conditions within the high-spin system and the influence of dipolar broadening of the EPR signal. Our findings foster the understanding of the CE mechanism and the design of high-spin PAs for specific applications of DNP. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

Enhancement of molecular NMR signal induced by polarization transfer from laser-polarized 129Xe

International Nuclear Information System (INIS)

Sun Xianping

2001-01-01

There is a large non-equilibrium nuclear polarization and a longer relaxation time in the laser-polarized 129 Xe produced by means of optical pumping and spin exchange. The characteristics of the laser-polarized 129 Xe permit the transfer of the polarization to enhance the atomic nuclear spin in liquid, solid and surface of solid molecules. Therefore, the sensitivity in nuclear magnetic resonance measurements for the molecules is enhanced and applications in the investigations of materials and surface sciences are expanded. The progress in the investigations of materials and surface sciences are expanded. The progress in the investigations of the polarization transfer between laser-polarized 129 Xe and the atomic nuclei in the molecules, the relative physics and the measurement of some parameters are introduced

Basis for calculating cross sections for nuclear magnetic resonance spin-modulated polarized neutron scattering.

Science.gov (United States)

Kotlarchyk, Michael; Thurston, George M

2016-12-28

In this work we study the potential for utilizing the scattering of polarized neutrons from nuclei whose spin has been modulated using nuclear magnetic resonance (NMR). From first principles, we present an in-depth development of the differential scattering cross sections that would arise in such measurements from a hypothetical target system containing nuclei with non-zero spins. In particular, we investigate the modulation of the polarized scattering cross sections following the application of radio frequency pulses that impart initial transverse rotations to selected sets of spin-1/2 nuclei. The long-term aim is to provide a foundational treatment of the scattering cross section associated with enhancing scattering signals from selected nuclei using NMR techniques, thus employing minimal chemical or isotopic alterations, so as to advance the knowledge of macromolecular or liquid structure.

A technique for measurement of vector and tensor polarization in solid spin one polarized targets

International Nuclear Information System (INIS)

Kielhorn, W.F.

1991-06-01

Vector and tensor polarizations are explicitly defined and used to characterize the polarization states of spin one polarized targets, and a technique for extracting these polarizations from nuclear magnetic resonance (NMR) data is developed. This technique is independent of assumptions about spin temperature, but assumes the target's crystal structure induces a quadrupole interaction with the spin one particles. Analysis of the NMR signals involves a computer curve fitting algorithm implemented with a fast Fourier transform method which speeds and simplifies curve fitting algorithms used previously. For accurate curve fitting, the NMR electronic circuit must be modeled by the fitting algorithm. Details of a circuit, its model, and data collected from this circuit are given for a solid deuterated ammonia target. 37 refs., 19 figs., 3 tabs

System for measuring the proton polarization in a polarized target

International Nuclear Information System (INIS)

Karnaukhov, I.M.; Lukhanin, A.A.; Telegin, Yu.N.; Trotsenko, V.I.; Chechetenko, V.F.

1984-01-01

The system for measuring the proton polarization in a polarized target representing the high-sensitivity nuclear magnetic resonance (NMR) is described Q-meter with series connection and a circuit for measuring system resonance characteristic is used for NMR-absorption signal recording. Measuring coil is produced of a strip conductor in order to obtain uniform system sensitivity to polarization state in all target volume and improve signal-to-noise ratio. Polarization measuring system operates ion-line with the M-6000 computer. The total measuring error for the value of free proton polarization in target taking into account the error caused by local depolarization of working substance under irradiation by high-intense photon beam is <= 6%. Long-term application of the described system for measuring the proton polarization in the LUEh-20000 accelerator target used in the pion photoproduction experiments has demonstrated its high reliability

Overhauser shift and dynamic nuclear polarization on carbon fibers

Science.gov (United States)

Herb, Konstantin; Denninger, Gert

2018-06-01

We report on the first experimental magnetic resonance determination of the coupling between electrons and nuclear spins (1H, 13C) in carbon fibers. Our results strongly support the assumption that the electronic spins are delocalized on graphene like structures in the fiber. The coupling between these electrons and the nuclei of the lattice results in dynamic nuclear polarization of the nuclei (DNP), enabling very sensitive NMR experiments on these nuclear spins. For possible applications of graphene in spintronics devices the coupling between nuclei and electrons is essential. We were able to determine the interactions down to 30 × 10-9(30 ppb) . We were even able to detect the coupling of the electrons to 13C (in natural abundance). These experiments open the way for a range of new double resonance investigations with possible applications in the field of material science.

A technique for measurement of vector and tensor polarization in solid spin one polarized targets

Energy Technology Data Exchange (ETDEWEB)

Kielhorn, W.F.

1991-06-01

Vector and tensor polarizations are explicitly defined and used to characterize the polarization states of spin one polarized targets, and a technique for extracting these polarizations from nuclear magnetic resonance (NMR) data is developed. This technique is independent of assumptions about spin temperature, but assumes the target's crystal structure induces a quadrupole interaction with the spin one particles. Analysis of the NMR signals involves a computer curve fitting algorithm implemented with a fast Fourier transform method which speeds and simplifies curve fitting algorithms used previously. For accurate curve fitting, the NMR electronic circuit must be modeled by the fitting algorithm. Details of a circuit, its model, and data collected from this circuit are given for a solid deuterated ammonia target. 37 refs., 19 figs., 3 tabs.

Verdazyl-ribose: A new radical for solid-state dynamic nuclear polarization at high magnetic field

Science.gov (United States)

Thurber, Kent R.; Le, Thanh-Ngoc; Changcoco, Victor; Brook, David J. R.

2018-04-01

Solid-state dynamic nuclear polarization (DNP) using the cross-effect relies on radical pairs whose electron spin resonance (ESR) frequencies differ by the nuclear magnetic resonance (NMR) frequency. We measure the DNP provided by a new water-soluble verdazyl radical, verdazyl-ribose, under both magic-angle spinning (MAS) and static sample conditions at 9.4 T, and compare it to a nitroxide radical, 4-hydroxy-TEMPO. We find that verdazyl-ribose is an effective radical for cross-effect DNP, with the best relative results for a non-spinning sample. Under non-spinning conditions, verdazyl-ribose provides roughly 2× larger 13C cross-polarized (CP) NMR signal than the nitroxide, with similar polarization buildup times, at both 29 K and 76 K. With MAS at 7 kHz and 1.5 W microwave power, the verdazyl-ribose does not provide as much DNP as the nitroxide, with the verdazyl providing less NMR signal and a longer polarization buildup time. When the microwave power is decreased to 30 mW with 5 kHz MAS, the two types of radical are comparable, with the verdazyl-doped sample having a larger NMR signal which compensates for its longer polarization buildup time. We also present electron spin relaxation measurements at Q-band (1.2 T) and ESR lineshapes at 1.2 and 9.4 T. Most notably, the verdazyl radical has a longer T1e than the nitroxide (9.9 ms and 1.3 ms, respectively, at 50 K and 1.2 T). The verdazyl electron spin lineshape is significantly affected by the hyperfine coupling to four 14N nuclei, even at 9.4 T. We also describe 3000-spin calculations to illustrate the DNP potential of possible radical pairs: verdazyl-verdazyl, verdazyl-nitroxide, or nitroxide-nitroxide pairs. These calculations suggest that the verdazyl radical at 9.4 T has a narrower linewidth than optimal for cross-effect DNP using verdazyl-verdazyl pairs. Because of the hyperfine coupling contribution to the electron spin linewidth, this implies that DNP using the verdazyl radical would improve at lower

Verdazyl-ribose: A new radical for solid-state dynamic nuclear polarization at high magnetic field.

Science.gov (United States)

Thurber, Kent R; Le, Thanh-Ngoc; Changcoco, Victor; Brook, David J R

2018-04-01

Solid-state dynamic nuclear polarization (DNP) using the cross-effect relies on radical pairs whose electron spin resonance (ESR) frequencies differ by the nuclear magnetic resonance (NMR) frequency. We measure the DNP provided by a new water-soluble verdazyl radical, verdazyl-ribose, under both magic-angle spinning (MAS) and static sample conditions at 9.4 T, and compare it to a nitroxide radical, 4-hydroxy-TEMPO. We find that verdazyl-ribose is an effective radical for cross-effect DNP, with the best relative results for a non-spinning sample. Under non-spinning conditions, verdazyl-ribose provides roughly 2× larger 13 C cross-polarized (CP) NMR signal than the nitroxide, with similar polarization buildup times, at both 29 K and 76 K. With MAS at 7 kHz and 1.5 W microwave power, the verdazyl-ribose does not provide as much DNP as the nitroxide, with the verdazyl providing less NMR signal and a longer polarization buildup time. When the microwave power is decreased to 30 mW with 5 kHz MAS, the two types of radical are comparable, with the verdazyl-doped sample having a larger NMR signal which compensates for its longer polarization buildup time. We also present electron spin relaxation measurements at Q-band (1.2 T) and ESR lineshapes at 1.2 and 9.4 T. Most notably, the verdazyl radical has a longer T 1e than the nitroxide (9.9 ms and 1.3 ms, respectively, at 50 K and 1.2 T). The verdazyl electron spin lineshape is significantly affected by the hyperfine coupling to four 14 N nuclei, even at 9.4 T. We also describe 3000-spin calculations to illustrate the DNP potential of possible radical pairs: verdazyl-verdazyl, verdazyl-nitroxide, or nitroxide-nitroxide pairs. These calculations suggest that the verdazyl radical at 9.4 T has a narrower linewidth than optimal for cross-effect DNP using verdazyl-verdazyl pairs. Because of the hyperfine coupling contribution to the electron spin linewidth, this implies that DNP using the verdazyl

NMR detection of short-lived β-emitter {sup 12}N implanted in water

Energy Technology Data Exchange (ETDEWEB)

Sugihara, T., E-mail: sugihara@vg.phys.sci.osaka-u.ac.jp; Mihara, M.; Shimaya, J.; Matsuta, K.; Fukuda, M.; Ohno, J.; Tanaka, M.; Yamaoka, S.; Watanabe, K.; Iwakiri, S.; Yanagihara, R.; Tanaka, Y.; Du, H.; Onishi, K.; Kambayashi, S.; Minamisono, T. [Osaka University, Department of Physics (Japan); Nishimura, D. [Tokyo University of Science, Department of Physics (Japan); Izumikawa, T. [Niigata University, Radioisotope Center (Japan); Ozawa, A. [University of Tsukuba, Department of Physics (Japan); Ishibashi, Y. [RIKEN Nishina Center for Accelerator-Based Science (Japan); and others

2017-11-15

The beta-detected nuclear magnetic resonance (β-NMR) in liquid H{sub 2}O has been observed for the first time using a short-lived β-ray emitter {sup 12}N (I{sup π} = 1{sup +},T{sub 1/2}=11 ms). A nuclear spin polarized {sup 12}N beam with an energy of about 20 MeV/nucleon was implanted into an enclosed water sample. About 50 % of implanted {sup 12}N ions maintained nuclear polarization and exhibited a β-NMR spectrum. The chemical shift of {sup 12}N in H{sub 2}O relative to {sup 12}N in Pt was deduced to be −(3.6±0.5) × 10{sup 2} ppm.

Determination of the composition of a mixture of polar substances by NMR; Determinacao da composicao de uma mistura de substancias polares por espectrometria de ressonancia magnetica nuclear

Energy Technology Data Exchange (ETDEWEB)

Teixeira, Antonio C.F.; Silva, Antonio J.R. da [Universidade Federal, Rio de Janeiro (Brazil). Nucleo de Pesquisas de Produtos Naturais

1994-12-31

This work describes the process of analysis of a mixture of polar compounds obtained from the extract of Phyllanthus tennellus, a plant known in Brazil as `quebra-pedra`, which is extensively used in Brazilian popular medicine. The methodology, which includes the use of chromatography and NMR, is described. The proposed composition of the mixture is presented. A discussion is presented concerning one component which could not be identified

Polarized nuclear target based on parahydrogen induced polarization

OpenAIRE

Budker, D.; Ledbetter, M. P.; Appelt, S.; Bouchard, L. S.; Wojtsekhowski, B.

2012-01-01

We discuss a novel concept of a polarized nuclear target for accelerator fixed-target scattering experiments, which is based on parahydrogen induced polarization (PHIP). One may be able to reach a 33% free-proton polarization in the ethane molecule. The potential advantages of such a target include operation at zero magnetic field, fast ($\\sim$100 Hz) polarization reversal, and operation with large intensity of an electron beam.

Dynamic Nuclear Polarization enhanced NMR at 187 GHz/284 MHz using an Extended Interaction Klystron amplifier.

Science.gov (United States)

Kemp, Thomas F; Dannatt, Hugh R W; Barrow, Nathan S; Watts, Anthony; Brown, Steven P; Newton, Mark E; Dupree, Ray

2016-04-01

A Dynamic Nuclear Polarisation (DNP) enhanced solid-state Magic Angle Spinning (MAS) NMR spectrometer which uses a 187 GHz (corresponding to (1)H NMR frequency of 284 MHz) Extended Interaction Klystron (EIK) amplifier as the microwave source is briefly described. Its performance is demonstrated for a biomolecule (bacteriorhodopsin), a pharmaceutical, and surface functionalised silica. The EIK is very compact and easily incorporated into an existing spectrometer. The bandwidth of the amplifier is sufficient that it obviates the need for a sweepable magnetic field, once set, for all commonly used radicals. The variable power (CW or pulsed) output from the EIK is transmitted to the DNP-NMR probe using a quasi-optic system with a high power isolator and a corrugated waveguide which feeds the microwaves into the DNP-NMR probe. Curved mirrors inside the probe project the microwaves down the axis of the MAS rotor, giving a very efficient system such that maximum DNP enhancement is achieved with less than 3 W output from the microwave source. The DNP-NMR probe operates with a sample temperature down to 90K whilst spinning at 8 kHz. Significant enhancements, in excess of 100 for bacteriorhodopsin in purple membrane (bR in PM), are shown along with spectra which are enhanced by ≈25 with respect to room temperature, for both the pharmaceutical furosemide and surface functionalised silica. These enhancements allow hitherto prohibitively time consuming experiments to be undertaken. The power at which the DNP enhancement in bR in PM saturates does not change significantly between 90K and 170 K even though the enhancement drops by a factor of ≈11. As the DNP build up time decreases by a factor 3 over this temperature range, the reduction in T1n is presumably a significant contribution to the drop in enhancement. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

Dynamic nuclear polarization using frequency modulation at 3.34 T.

Science.gov (United States)

Hovav, Y; Feintuch, A; Vega, S; Goldfarb, D

2014-01-01

During dynamic nuclear polarization (DNP) experiments polarization is transferred from unpaired electrons to their neighboring nuclear spins, resulting in dramatic enhancement of the NMR signals. While in most cases this is achieved by continuous wave (cw) irradiation applied to samples in fixed external magnetic fields, here we show that DNP enhancement of static samples can improve by modulating the microwave (MW) frequency at a constant field of 3.34 T. The efficiency of triangular shaped modulation is explored by monitoring the (1)H signal enhancement in frozen solutions containing different TEMPOL radical concentrations at different temperatures. The optimal modulation parameters are examined experimentally and under the most favorable conditions a threefold enhancement is obtained with respect to constant frequency DNP in samples with low radical concentrations. The results are interpreted using numerical simulations on small spin systems. In particular, it is shown experimentally and explained theoretically that: (i) The optimal modulation frequency is higher than the electron spin-lattice relaxation rate. (ii) The optimal modulation amplitude must be smaller than the nuclear Larmor frequency and the EPR line-width, as expected. (iii) The MW frequencies corresponding to the enhancement maxima and minima are shifted away from one another when using frequency modulation, relative to the constant frequency experiments. Copyright © 2013 Elsevier Inc. All rights reserved.

Magnetic moment of $^{17}$Ne using beta -NMR and tilted foil polarization

CERN Document Server

Baby, L T; Hass, M; Haas, H; Weissman, L; Brown, B A

2004-01-01

We report on the measurement of the magnetic moment of the ground state of /sup 17/Ne. Radioactive /sup 17/Ne nuclei were delivered from the high resolution mass separator at ISOLDE onto a high voltage platform at -200 kV and were polarized using the tilted foil polarization method. The polarized nuclei were implanted into a Pt stopper situated in a liquid-helium cooled beta -NMR apparatus and the asymmetry destruction of the ensuing beta rays was monitored as a function of the rf frequency applied to the polarized nuclei. The measured value of mu = 0.74 +or- 0.03 affirms the nu p/sub 1/2//sup - / nature of the ground state of /sup 17/Ne and is compared to shell model calculations. (10 refs).

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

Science.gov (United States)

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

2017-10-01

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

Polarized targets at triangle universities nuclear laboratory

Energy Technology Data Exchange (ETDEWEB)

Seely, M.L. [North Carolina State Univ., Raleigh, NC (United States); Gould, C.R. [North Carolina State Univ., Raleigh, NC (United States); Haase, D.G. [North Carolina State Univ., Raleigh, NC (United States); Huffman, P.R. [Triangle Universities Nuclear Laboratory, Durham, NC 27708 (United States); Keith, C.D. [North Carolina State Univ., Raleigh, NC (United States); Roberson, N.R. [Triangle Universities Nuclear Laboratory, Durham, NC 27708 (United States); Tornow, W. [Triangle Universities Nuclear Laboratory, Durham, NC 27708 (United States); Wilburn, W.S. [Triangle Universities Nuclear Laboratory, Durham, NC 27708 (United States)

1995-03-01

A summary of the polarized and aligned nuclear targets which have been constructed and used at the Triangle Universities Nuclear Laboratory is given. Statically polarized targets, typically operating at a temperature of 12 mK and a magnetic field of 7 T, have provided significant nuclear polarization in {sup 1}H, {sup 3}He, {sup 27}Al, {sup 93}Nb and {sup 165}Ho. A rotating, aligned {sup 165}Ho target is also in use. A {sup 3}He melting curve thermometer has been developed for use in statically polarized targets. A dynamically polarized proton target is under construction. ((orig.))

Nuclear physics with polarized particles

CERN Document Server

Paetz gen Schieck, Hans

2012-01-01

The measurement of spin-polarization observables in reactions of nuclei and particles is of great utility and advantage when the effects of single-spin sub-states are to be investigated. Indeed, the unpolarized differential cross-section encompasses the averaging over the spin states of the particles, and thus loses details of the interaction process. This introductory text combines, in a single volume, course-based lecture notes on spin physics and on polarized-ion sources with the aim of providing a concise yet self-contained starting point for newcomers to the field, as well as for lecturers in search of suitable material for their courses and seminars. A significant part of the book is devoted to introducing the formal theory-a description of polarization and of nuclear reactions with polarized particles. The remainder of the text describes the physical basis of methods and devices necessary to perform experiments with polarized particles and to measure polarization and polarization effects in nuclear rea...

A pulse programmable parahydrogen polarizer using a tunable electromagnet and dual channel NMR spectrometer

Science.gov (United States)

Coffey, Aaron M.; Shchepin, Roman V.; Feng, Bibo; Colon, Raul D.; Wilkens, Ken; Waddell, Kevin W.; Chekmenev, Eduard Y.

2017-11-01

Applications of parahydrogen induced polarization (PHIP) often warrant conversion of the chemically-synthesized singlet-state spin order into net heteronuclear magnetization. In order to obtain optimal yields from the overall hyperpolarization process, catalytic hydrogenation must be tightly synchronized to subsequent radiofrequency (RF) transformations of spin order. Commercial NMR consoles are designed to synchronize applied waves on multiple channels and consequently are well-suited as controllers for these types of hyperpolarization experiments that require tight coordination of RF and non-RF events. Described here is a PHIP instrument interfaced to a portable NMR console operating with a static field electromagnet in the milliTesla regime. In addition to providing comprehensive control over chemistry and RF events, this setup condenses the PHIP protocol into a pulse-program that in turn can be readily shared in the manner of traditional pulse sequences. In this device, a TTL multiplexer was constructed to convert spectrometer TTL outputs into 24 VDC signals. These signals then activated solenoid valves to control chemical shuttling and reactivity in PHIP experiments. Consolidating these steps in a pulse-programming environment speeded calibration and improved quality assurance by enabling the B0/B1 fields to be tuned based on the direct acquisition of thermally polarized and hyperpolarized NMR signals. Performance was tested on the parahydrogen addition product of 2-hydroxyethyl propionate-1-13C-d3, where the 13C polarization was estimated to be P13C = 20 ± 2.5% corresponding to 13C signal enhancement approximately 25 million-fold at 9.1 mT or approximately 77,000-fold 13C enhancement at 3 T with respect to thermally induced polarization at room temperature.

The Bochum Polarized Target

International Nuclear Information System (INIS)

Reicherz, G.; Goertz, S.; Harmsen, J.; Heckmann, J.; Meier, A.; Meyer, W.; Radtke, E.

2001-01-01

The Bochum 'Polarized Target' group develops the target material 6 LiD for the COMPASS experiment at CERN. Several different materials like alcohols, alcanes and ammonia are under investigation. Solid State Targets are polarized in magnetic fields higher than B=2.5T and at temperatures below T=1K. For the Dynamic Nuclear Polarization process, paramagnetic centers are induced chemically or by irradiation with ionizing beams. The radical density is a critical factor for optimization of polarization and relaxation times at adequate magnetic fields and temperatures. In a high sensitive EPR--apparatus, an evaporator and a dilution cryostat with a continuous wave NMR--system, the materials are investigated and optimized. To improve the polarization measurement, the Liverpool NMR-box is modified by exchanging the fixed capacitor for a varicap diode which not only makes the tuning very easy but also provides a continuously tuned circuit. The dependence of the signal area upon the circuit current is measured and it is shown that it follows a linear function

Nuclear polarization in muonic 208Pb

International Nuclear Information System (INIS)

Haga, Akihiro; Tanaka, Yasutoshi; Horikawa, Yataro

2002-01-01

We calculate nuclear-polarization energy shifts in muonic 208 Pb. We employ a relativistic field-theoretical calculation and evaluate the ladder, cross, and seagull terms of the two-photon exchange diagrams in both the Feynman and Coulomb gauges. Gauge independence is very well satisfied with the calculated nuclear-polarization energies. Using these results, we analyze fine-structure splitting energies of muonic 208 Pb because of the presence of the persisting discrepancies between experiment and calculation. The present nuclear-polarization energies explain about half of the anomaly in the Δ2p fine-structure splitting energy, and only one-fourth of the anomaly in the Δ3p fine-structure splitting energy

On the large COMPASS polarized deuteron target

CERN Document Server

Finger, M; Baum, G; Doshita, N; Finger, M Jr; Gautheron, F; Goertz, St; Hasegawa, T; Heckmann, J; Hess, Ch; Horikawa, N; Ishimoto, S; Iwata, T; Kisselev, Y; Koivuniemi, J; Kondo, K; Le Goff, J-M; Magnon, A; Marchand, C; Matsuda, T; Meyer, W; Reicherz, G; Srnka, A

2006-01-01

The spin structure of the nucleons is investigated in deep inelastic scattering of a polarized muon beam and a polarized nucleon target in the COMPASS experiment at CERN since 2001. To achieve high luminosities a large solid polarized target is used. The COMPASS polarized target consists of a high cooling power $^{3}$He/$^{4}$He dilution refrigerator capable to maintain working temperature of the target material at about 50mK, a superconducting solenoid and dipole magnet system for longitudinal and transversal magnetic field on the target material, respectively, target cells containing polarizable material, microwave cavities and high power microwave radiation systems for dynamic nuclear polarization and the nuclear magnetic resonance system for nuclear spin polarization measurements. During 2001–2004 experiments superconducting magnet system with opening angle $\\pm$69 mrad, polarized target holder with two target cells and corresponding microwave and NMR systems have been used. For the data taking from 200...

Solid state nuclear magnetic resonance: investigating the spins of nuclear related materials

International Nuclear Information System (INIS)

Charpentier, Th.

2007-10-01

The author reviews his successive research works: his research thesis work on the Multiple Quantum Magic Angle Spinning (MQMAS) which is a quadric-polar nucleus multi-quanta correlation spectroscopy method, the modelling of NMR spectra of disordered materials, the application to materials of interest for the nuclear industry (notably the glasses used for nuclear waste containment). He presents the various research projects in which he is involved: storing glasses, nuclear magnetic resonance in paramagnetism, solid hydrogen storing matrices, methodological and instrument developments in high magnetic field and high resolution solid NMR, long range distance measurement by solid state Tritium NMR (observing the structure and dynamics of biological complex systems at work)

Methodological developments of low field MRI: Elasto-graphy, MRI-ultrasound interaction and dynamic nuclear polarization

International Nuclear Information System (INIS)

Madelin, Guillaume

2005-01-01

This thesis deals with two aspects of low field (0.2 T) Magnetic Resonance Imaging (MRI): the research of new contrasts due to the interaction between Nuclear Magnetic Resonance (NMR) and acoustics (elasto-graphy, spin-phonon interaction) and enhancement of the signal-to-noise ratio by Dynamic Nuclear Polarization (DNP). Magnetic Resonance Elasto-graphy (MRE) allows to assess some viscoelastic properties of tissues by visualization of the propagation of low frequency acoustic strain waves. A review on MRE is given, as well as a study on local measurement of the acoustic absorption coefficient. The next part is dedicated to MRI-ultrasound interaction. First, the ultrasonic transducer was calibrated for power and acoustic field using the comparison of two methods: the radiation force method (balance method) and laser interferometry. Then, we tried to modify the T1 contrast of tissues by spin-phonon interaction due to the application of ultrasound at the resonance frequency at 0.2 T, which is about 8.25 MHz. No modification of T1 contrast has been obtained, but the acoustic streaming phenomenon has been observed in liquids. MRI visualization of this streaming could make possible to calibrate transducers as well as to assess some mechanical properties of viscous fluids. The goal of the last part was to set up DNP experiments at 0.2 T in order to enhance the NMR signal. This double resonance method is based on the polarization transfer of unpaired electrons of free radicals to the surrounding protons of water. This transfer occurs by cross relaxation during the saturation of an electronic transition using Electronic Paramagnetic Resonance (EPR). Two EPR cavities operating at 5.43 GHz have been tested on oxo-TEMPO free radicals (nitroxide). An enhancement of the NMR signal by a factor 30 was obtained during these preliminary experiments. (author)

Communication: Permanent dipoles contribute to electric polarization in chiral NMR spectra

International Nuclear Information System (INIS)

Buckingham, A. David

2014-01-01

Nuclear magnetic resonance spectroscopy is blind to chirality because the spectra of a molecule and its mirror image are identical unless the environment is chiral. However, precessing nuclear magnetic moments in chiral molecules in a strong magnetic field induce an electric polarization through the nuclear magnetic shielding polarizability. This effect is equal and opposite for a molecule and its mirror image but is small and has not yet been observed. It is shown that the permanent electric dipole moment of a chiral molecule is partially oriented through the antisymmetric part of the nuclear magnetic shielding tensor, causing the electric dipole to precess with the nuclear magnetic moment and producing a much larger temperature-dependent electric polarization with better prospects of detection

Frequency-agile gyrotron for electron decoupling and pulsed dynamic nuclear polarization

Science.gov (United States)

Scott, Faith J.; Saliba, Edward P.; Albert, Brice J.; Alaniva, Nicholas; Sesti, Erika L.; Gao, Chukun; Golota, Natalie C.; Choi, Eric J.; Jagtap, Anil P.; Wittmann, Johannes J.; Eckardt, Michael; Harneit, Wolfgang; Corzilius, Björn; Th. Sigurdsson, Snorri; Barnes, Alexander B.

2018-04-01

We describe a frequency-agile gyrotron which can generate frequency-chirped microwave pulses. An arbitrary waveform generator (AWG) within the NMR spectrometer controls the microwave frequency, enabling synchronized pulsed control of both electron and nuclear spins. We demonstrate that the acceleration of emitted electrons, and thus the microwave frequency, can be quickly changed by varying the anode voltage. This strategy results in much faster frequency response than can be achieved by changing the potential of the electron emitter, and does not require a custom triode electron gun. The gyrotron frequency can be swept with a rate of 20 MHz/μs over a 670 MHz bandwidth in a static magnetic field. We have already implemented time-domain electron decoupling with dynamic nuclear polarization (DNP) magic angle spinning (MAS) with this device. In this contribution, we show frequency-swept DNP enhancement profiles recorded without changing the NMR magnet or probe. The profile of endofullerenes exhibits a DNP profile with a <10 MHz linewidth, indicating that the device also has sufficient frequency stability, and therefore phase stability, to implement pulsed DNP mechanisms such as the frequency-swept solid effect. We describe schematics of the mechanical and vacuum construction of the device which includes a novel flanged sapphire window assembly. Finally, we discuss how commercially available continuous-wave gyrotrons can potentially be converted into similar frequency-agile high-power microwave sources.

Nuclear polarization in hydrogenlike 82208Pb81+

International Nuclear Information System (INIS)

Haga, Akihiro; Tanaka, Yasutoshi; Horikawa, Yataro

2002-01-01

We calculate nuclear-polarization energy shifts for the hydrogenlike 82 208 Pb 81+ . The retarded transverse part as well as the longitudinal part is taken into account as the electromagnetic interaction between an electron and the nucleus. With a finite charge distribution for the nuclear ground state and the random-phase approximation to describe the nuclear excitations, we obtain nuclear-polarization energy of the 1s 1/2 state as -38.2 (-37.0) meV in the Feynman (Coulomb) gauge. For the 2s 1/2 , 2p 1/2 , and 2p 3/2 states, they are -6.7 (-6.4), -0.2 (-0.2), and +0.0 (+0.0) meV, respectively. The transverse contribution is small in comparison with the longitudinal nuclear-polarization correction. It is about 12% both for the 1s 1/2 and 2s 1/2 states. The seagull term in the two-photon exchange diagrams is also shown to be quite important to obtain the gauge-invariant nuclear-polarization energies

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

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...

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.

Studies of metal-biomolecule systems in liquids with beta-detected NMR

CERN Document Server

Walczak, Michal

2017-01-01

My internship took place within a small research team funded via the European Research Council (ERC Starting Grant: Beta-Drop NMR) at ISOLDE. It was devoted to laser spin-polarization and beta-detected NMR techniques and their future applications in chemistry and biology. I was involved in the design and tests of the beta-NMR spectrometer which will be used in the upcoming experiments. In this way I have been exposed to many topics in physics (atomic and nuclear physics), experimental techniques (vacuum technology, lasers, beta detectors, electronics, DAQ software), as well as chemistry and biology (NMR on metal ions, metal ion binding to biomolecules, quantum chemistry calculations).

Versatile Ion-polarized Techniques On-line (VITO) experiment at ISOLDE-CERN

Czech Academy of Sciences Publication Activity Database

Stachura, M.; Gottberg, A.; Johnston, K.; Bissell, M. L.; Ruiz, R. F. G.; Correia, J. M.; Costa, A. R. G.; Dehn, M.; Deicher, M.; Fenta, A.; Hemmingsen, L.; Molholt, T. E.; Munch, M.; Neyens, G.; Pallada, S.; Silva, M. R.; Zákoucký, Dalibor

2016-01-01

Roč. 376, JUN (2016), s. 369-373 ISSN 0168-583X Institutional support: RVO:61389005 Keywords : laser-induced nuclear polarization * beta-NMR spectroscopy * beta-Asymmetry * PAC spectroscopy * radioisotopes Subject RIV: BG - Nuclear, Atomic and Molecular Physics, Colliders Impact factor: 1.109, year: 2016

Robust techniques for polarization and detection of nuclear spin ensembles

Science.gov (United States)

Scheuer, Jochen; Schwartz, Ilai; Müller, Samuel; Chen, Qiong; Dhand, Ish; Plenio, Martin B.; Naydenov, Boris; Jelezko, Fedor

2017-11-01

Highly sensitive nuclear spin detection is crucial in many scientific areas including nuclear magnetic resonance spectroscopy, magnetic resonance imaging (MRI), and quantum computing. The tiny thermal nuclear spin polarization represents a major obstacle towards this goal which may be overcome by dynamic nuclear spin polarization (DNP) methods. The latter often rely on the transfer of the thermally polarized electron spins to nearby nuclear spins, which is limited by the Boltzmann distribution of the former. Here we utilize microwave dressed states to transfer the high (>92 % ) nonequilibrium electron spin polarization of a single nitrogen-vacancy center (NV) induced by short laser pulses to the surrounding 13C carbon nuclear spins. The NV is repeatedly repolarized optically, thus providing an effectively infinite polarization reservoir. A saturation of the polarization of the nearby nuclear spins is achieved, which is confirmed by the decay of the polarization transfer signal and shows an excellent agreement with theoretical simulations. Hereby we introduce the polarization readout by polarization inversion method as a quantitative magnetization measure of the nuclear spin bath, which allows us to observe by ensemble averaging macroscopically hidden polarization dynamics like Landau-Zener-Stückelberg oscillations. Moreover, we show that using the integrated solid effect both for single- and double-quantum transitions nuclear spin polarization can be achieved even when the static magnetic field is not aligned along the NV's crystal axis. This opens a path for the application of our DNP technique to spins in and outside of nanodiamonds, enabling their application as MRI tracers. Furthermore, the methods reported here can be applied to other solid state systems where a central electron spin is coupled to a nuclear spin bath, e.g., phosphor donors in silicon and color centers in silicon carbide.

System for measuring of proton polarization in polarized target

International Nuclear Information System (INIS)

Derkach, A.Ya.; Lukhanin, A.A.; Karnaukhov, I.M.; Kuz'menko, V.S.; Telegin, Yu.N.; Trotsenko, V.I.; Chechetenko, V.F.

1981-01-01

Measurement system of proton polarization in the target, which uses the method of nuclear magnetic resonance is described. To record the signal of NMR-absorption a parallel Q-meter of voltage with analogous subtraction of resonance characteristics of measurement circuit is used. To obtain gradual sensitivity of the system to polarization state in the whole volume of the target the measurement coils is made of tape conductor. The analysis and mathematical modelling of Q-meter are carried out. Corrections for nonlinearity and dispersion are calculated. Key diagrams of the main electron blocks of Q-meter are presented. The system described operates on line with the M6000 computer. Total error of measurement of polarization value of free protons in the target does not exceed 6% [ru

Polarization transfer from polarized nuclear spin to μ- spin in muonic atom

International Nuclear Information System (INIS)

Kuno, Yoshitaka; Nagamine, Kanetada; Yamazaki, Toshimitsu.

1987-02-01

A theoretical study of polarization transfer from an initially-polarized nuclear spin to a μ - spin in a muonic atom is given. The switching of the hyperfine interaction at excited muonic states as well as at the ground 1s state is taken into account. The upper state of hyperfine doublet at the muonic 1s state is considered to proceed down to the lower state. It is found that as the hyperfine interaction becomes effective at higher excited muonic orbitals, a less extent of polarization is transferred from the nuclear spin to the μ - spin. The theoretical values obtained are compared with the recent experiment of μ - repolarization in a polarized 209 Bi target. (author)

Dynamic nuclear polarization of irradiated target materials

International Nuclear Information System (INIS)

Seely, M.L.

1982-01-01

Polarized nucleon targets used in high energy physics experiments usually employ the method of dynamic nuclear polarization (DNP) to polarize the protons or deuterons in an alcohol. DNP requires the presence of paramagnetic centers, which are customarily provided by a chemical dopant. These chemically doped targets have a relatively low polarizable nucleon content and suffer from loss of polarization when subjected to high doses of ionizing radiation. If the paramagnetic centers formed when the target is irradiated can be used in the DNP process, it becomes possible to produce targets using materials which have a relatively high polarizable nucleon content, but which are not easily doped by chemical means. Furthermore, the polarization of such targets may be much more radiation resistant. Dynamic nuclear polarization in ammonia, deuterated ammonia, ammonium hydroxide, methylamine, borane ammonia, butonal, ethane and lithium borohydride has been studied. These studies were conducted at the Stanford Linear Accelerator Center using the Yale-SLAC polarized target system. Results indicate that the use of ammonia and deuterated ammonia as polarized target materials would make significant increases in polarized target performance possible

solvent effect on 14n nmr shielding of glycine, serine, leucine

African Journals Online (AJOL)

a

constants favor the more polar tautomers. Ab initio calculation of nuclear magnetic shielding has become an indispensable aid in the investigation of molecular structure and accurate assignment of NMR spectra of compounds. The solvation effect is taken into account via the self-consistent reaction field (SCRF) method.

Nuclear magnetic resonance apparatus having semitoroidal RF coil for use in topical NMR and NMR imaging

International Nuclear Information System (INIS)

Fukushima, E.; Assink, R.A.; Roeder, S.B.W.; Gibson, A.A.V.

1984-01-01

An improved nuclear magnetic resonance (NMR) apparatus for use in topical magnetic resonance (TMR) spectroscopy and other remote sensing NMR applications includes a semitoroidal radio frequency (rf) coil. The semitoroidal rf coil produces an effective alternating magnetic field at a distance from the poles of the coil, to enable NMR measurements to be taken from selected regions inside an object, particularly human and other living subjects. The semitoroidal rf coil is relatively insensitive to magnetic interference from metallic objects located behind the coil, thereby rendering the coil particularly suited for use in both conventional and superconducting NMR magnets. The semitoroidal NMR coil can be constructed so that it emits little or no excess rf electric field associated with the rf magnetic field, thus avoiding adverse effects due to dielectric heating of the sample or to any other electric field interactions. The coil may be combined with a like orthogonal coil and suitably driven to provide a circularly polarised field; or it may be used in conjunction with a concentrically nested smaller semitoroidal coil to move the maximum field further from the coil assembly. (author)

Development and performance of a 129-GHz dynamic nuclear polarizer in an ultra-wide bore superconducting magnet.

Science.gov (United States)

Lumata, Lloyd L; Martin, Richard; Jindal, Ashish K; Kovacs, Zoltan; Conradi, Mark S; Merritt, Matthew E

2015-04-01

We sought to build a dynamic nuclear polarization system for operation at 4.6 T (129 GHz) and evaluate its efficiency in terms of (13)C polarization levels using free radicals that span a range of ESR linewidths. A liquid helium cryostat was placed in a 4.6 T superconducting magnet with a 150-mm warm bore diameter. A 129-GHz microwave source was used to irradiate (13)C enriched samples. Temperatures close to 1 K were achieved using a vacuum pump with a 453-m(3)/h roots blower. A hyperpolarized (13)C nuclear magnetic resonance (NMR) signal was detected using a saddle coil and a Varian VNMRS console operating at 49.208 MHz. Samples doped with free radicals BDPA (1,3-bisdiphenylene-2-phenylallyl), trityl OX063 (tris{8-carboxyl-2,2,6,6-benzo(1,2-d:4,5-d)-bis(1,3)dithiole-4-yl}methyl sodium salt), galvinoxyl ((2,6-di-tert-butyl-α-(3,5-di-tert-butyl-4-oxo-2,5-cyclohexadien-1-ylidene)-p-tolyloxy), 2,2-diphenylpicrylhydrazyl (DPPH) and 4-oxo-TEMPO (4-Oxo-2,2,6,6-tetramethyl-1-piperidinyloxy) were assayed. Microwave dynamic nuclear polarization (DNP) spectra and solid-state (13)C polarization levels for these samples were determined. (13)C polarization levels close to 50 % were achieved for [1-(13)C]pyruvic acid at 1.15 K using the narrow electron spin resonance (ESR) linewidth free radicals trityl OX063 and BDPA, while 10-20 % (13)C polarizations were achieved using galvinoxyl, DPPH and 4-oxo-TEMPO. At this field strength free radicals with smaller ESR linewidths are still superior for DNP of (13)C as opposed to those with linewidths that exceed that of the (1)H Larmor frequency.

Probing membrane protein structure using water polarization transfer solid-state NMR.

Science.gov (United States)

Williams, Jonathan K; Hong, Mei

2014-10-01

Water plays an essential role in the structure and function of proteins, lipid membranes and other biological macromolecules. Solid-state NMR heteronuclear-detected (1)H polarization transfer from water to biomolecules is a versatile approach for studying water-protein, water-membrane, and water-carbohydrate interactions in biology. We review radiofrequency pulse sequences for measuring water polarization transfer to biomolecules, the mechanisms of polarization transfer, and the application of this method to various biological systems. Three polarization transfer mechanisms, chemical exchange, spin diffusion and NOE, manifest themselves at different temperatures, magic-angle-spinning frequencies, and pulse irradiations. Chemical exchange is ubiquitous in all systems examined so far, and spin diffusion plays the key role in polarization transfer within the macromolecule. Tightly bound water molecules with long residence times are rare in proteins at ambient temperature. The water polarization-transfer technique has been used to study the hydration of microcrystalline proteins, lipid membranes, and plant cell wall polysaccharides, and to derive atomic-resolution details of the kinetics and mechanism of ion conduction in channels and pumps. Using this approach, we have measured the water polarization transfer to the transmembrane domain of the influenza M2 protein to obtain information on the structure of this tetrameric proton channel. At short mixing times, the polarization transfer rates are site-specific and depend on the pH, labile protons, sidechain conformation, as well as the radial position of the residues in this four-helix bundle. Despite the multiple dependences, the initial transfer rates reflect the periodic nature of the residue positions from the water-filled pore, thus this technique provides a way of gleaning secondary structure information, helix tilt angle, and the oligomeric structure of membrane proteins. Copyright © 2014 Elsevier Inc. All

Core Technology Development of Nuclear spin polarization

International Nuclear Information System (INIS)

Yoo, Byung Duk; Gwon, Sung Ok; Kwon, Duck Hee; Lee, Sung Man

2009-12-01

In order to study nuclear spin polarization, we need several core technologies such as laser beam source to polarize the nuclear spin, low pressured helium cell development whose surface is essential to maintain polarization otherwise most of the polarized helium relaxed in short time, development of uniform magnetic field system which is essential for reducing relaxation, efficient vacuum system, development of polarization measuring system, and development of pressure raising system about 1000 times. The purpose of this study is to develop resonable power of laser system, that is at least 5 watt, 1083 nm, 4GHz tuneable. But the limitation of this research fund enforce to develop amplifying system into 5 watt with 1 watt system utilizing laser-diod which is already we have in stock. We succeeded in getting excellent specification of fiber laser system with power of 5 watts, 2 GHz linewidth, more than 80 GHz tuneable

On the thermal properties of polarized nuclear matter

International Nuclear Information System (INIS)

Hassan, M.Y.M.; Montasser, S.S.; Ramadan, S.

1979-08-01

The thermal properties of polarized nuclear matter are calculated using Skyrme III interaction modified by Dabrowski for polarized nuclear matter. The temperature dependence of the volume, isospin, spin and spin isospin pressure and energies are determined. The temperature, isospin, spin and spin isospin dependence of the equilibrium Fermi momentum is also discussed. (author)

Local field in LiD polarized target material

CERN Document Server

Kisselev, Yu V; Baum, G; Berglund, P; Doshita, N; Gautheron, F; Görtz, S; Horikawa, N; Koivuniemi, J H; Kondo, K; Magnon, A; Meyer, Werner T; Reicherz, G

2004-01-01

We have experimentally studied the first and the second moments of D, **6Li and **7Li (I greater than 1/2) NMR lines in a granulated LiD- target material as a function of nuclear polarizations and the data has been compared with a theory elaborated by Abragam, Roinel and Bouffard for monocrystalline samples. The experiments were carried out in the large COMPASS twin-target at CERN. The static local magnetic field of the polarized nuclei was measured by frequency shift between the NMR-signals in the two oppositely polarized cells and lead to the first moment, whereas the investigation of the second moment was done through Gaussian approximation. The average field magnitude in granulated material was estimated 20% larger than the value given by the calculations for monocrystalline samples of cylindrical shape. The second moment shows a qualitative agreement with the theory but it is slightly larger at the negative than at the positive polarization. In a polarized mode, the moments depend on the saturated microw...

NMR clinical imaging and spectroscopy: Its impact on nuclear medicine

International Nuclear Information System (INIS)

1990-01-01

This is a collection of four papers describing aspects of past and future use of nuclear magnetic resonance as a clinical diagnostic tool. The four papers are entitled (1) What Does NMR Offer that Nuclear Medicine Does Not? by Jerry W. Froelich, (2) Oncological Imaging: Now, Future and Impact Jerry W. Froelich, (3) Magnetic Resonance Spectroscopy/Spectroscopic Imaging and Nuclear Medicine: Past, Present and Future by H. Cecil Charles, and (4) MR Cardiology: Now, Future and Impact by Robert J. Herfkens

Hyperpolarized 129Xe as an NMR probe for functional studies

International Nuclear Information System (INIS)

Wolber, J.

2000-01-01

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

Dynamical nuclear polarization using multi-colour control of color centers in diamond

Energy Technology Data Exchange (ETDEWEB)

Yang, Pengcheng [Huazhong University of Science and Technology, School of Physics, Wuhan (China); Huazhong University of Science and Technology, Center for Quantum Optical Science, Wuhan (China); Plenio, Martin B. [Universitaet Ulm, Institut fuer Theoretische Physik, Ulm (Germany); Universitaet Ulm, Center for Integrated Quantum Science and Technology, Ulm (Germany); Cai, Jianming [Huazhong University of Science and Technology, School of Physics, Wuhan (China); Huazhong University of Science and Technology, Center for Quantum Optical Science, Wuhan (China); Universitaet Ulm, Institut fuer Theoretische Physik, Ulm (Germany); Universitaet Ulm, Center for Integrated Quantum Science and Technology, Ulm (Germany)

2016-12-15

Dynamical nuclear polarization (DNP) transfers the polarization of electron spins at cryogenic temperatures to achieve strong nuclear polarization for applications in nuclear magnetic resonance. Recently introduced approaches employ optical pumping of nitrogen-vacancy (NV) centers in diamond to achieve DNP even at ambient temperatures. In such schemes microwave radiation is used to establish a Hartmann-Hahn condition between the NV electron spin and proximal nuclear spins to facilitate polarization transfer. For a single monochromatic microwave driving field, the Hartmann-Hahn condition cannot be satisfied for an ensemble of NV centers due to inhomogeneous broadening and reduces significantly the overall efficiency of dynamical nuclear polarization using an ensemble of NV centers. Here, we adopt generalized Hartmann-Hahn type dynamical nuclear polarization schemes by applying microwave driving fields with (multiple) time-modulated frequencies. We show that it is possible to enhance the effective coupling between an ensemble of NV center spins with inhomogeneous broadening and nuclear spins, thereby improving significantly the overall efficiency of dynamical nuclear polarization. This approach can also be used to achieve dynamical nuclear polarization of an ensemble of nuclei with a distribution of Larmor frequencies, which would be helpful in magnetic resonance spectroscopy using a single NV spin sensor. (orig.)

Modeling alignment enhancement for solid polarized targets

Energy Technology Data Exchange (ETDEWEB)

Keller, D. [University of Virginia, Charlottesville, VA (United States)

2017-07-15

A model of dynamic orientation using optimized radiofrequency (RF) irradiation produced perpendicular to the holding field is developed for the spin-1 system required for tensor-polarized fixed-target experiments. The derivation applies to RF produced close to the Larmor frequency of the nucleus and requires the electron spin-resonance linewidth to be much smaller than the nuclear magnetic resonance frequency. The rate equations are solved numerically to study a semi-saturated steady-state resulting from the two sources of irradiation: microwave from the DNP process and the additional RF used to manipulate the tensor polarization. The steady-state condition and continuous-wave NMR lineshape are found that optimize the spin-1 alignment in the polycrystalline materials used as solid polarized targets in charged-beam nuclear and particle physics experiments. (orig.)

Discovery of Intermediates of lacZ β-Galactosidase Catalyzed Hydrolysis Using dDNP NMR

DEFF Research Database (Denmark)

Kjeldsen, Christian; Ardenkjær-Larsen, Jan Henrik; Duus, Jens Ø.

2018-01-01

Using dissolution dynamic nuclear polarization, the sensitivity of single scan solution state 13C NMR can be improved up to 4 orders of magnitude. In this study, the enzyme lacZ β-galactosidase from Escherichia coli was subjected to hyperpolarized substrate, and previously unknown reaction...

Discovery of Intermediates of lacZ beta-Galactosidase Catalyzed Hydrolysis Using dDNP NMR

DEFF Research Database (Denmark)

Kjeldsen, Christian; Ardenkjær-Larsen, Jan Henrik; Duus, Jens Øllgaard

2018-01-01

Using dissolution dynamic nuclear polarization, the sensitivity of single scan solution state C-13 NMR can be improved up to 4 orders of magnitude. In this study, the enzyme lacZ beta-galactosidase from Escherichia coli was subjected to hyperpolarized substrate, and previously unknown reaction...

Report of the workshop on nuclear polarization phenomena

International Nuclear Information System (INIS)

1985-01-01

The third work shop on the study of the nuclear polarization was held in December 1984 at RCNP (Research Center for Nuclear Physics). Osaka University, in advance of the comming international conference. About 80 researchers gathered and discussed both theoretical and experimental aspects of nuclear polarization phenomena. Forty eight papers were presented at the work shop and they are collected in this report. Although almost all of them are written in Japanese, the abstracts are prepared in English. (Aoki, K.)

Integrated Geophysical Measurements for Bioremediation Monitoring: Combining Spectral Induced Polarization, Nuclear Magnetic Resonance and Magnetic Methods

Energy Technology Data Exchange (ETDEWEB)

Keating, Kristina [Rutgers Univ., Newark, NJ (United States). Dept. of Earth and Environmental Sciences; Slater, Lee [Rutgers Univ., Newark, NJ (United States). Dept. of Earth and Environmental Sciences; Ntarlagiannis, Dimitris [Rutgers Univ., Newark, NJ (United States). Dept. of Earth and Environmental Sciences; Williams, Kenneth H. [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Earth Sciences Division

2015-02-24

This documents contains the final report for the project "Integrated Geophysical Measurements for Bioremediation Monitoring: Combining Spectral Induced Polarization, Nuclear Magnetic Resonance and Magnetic Methods" (DE-SC0007049) Executive Summary: Our research aimed to develop borehole measurement techniques capable of monitoring subsurface processes, such as changes in pore geometry and iron/sulfur geochemistry, associated with remediation of heavy metals and radionuclides. Previous work has demonstrated that geophysical method spectral induced polarization (SIP) can be used to assess subsurface contaminant remediation; however, SIP signals can be generated from multiple sources limiting their interpretation value. Integrating multiple geophysical methods, such as nuclear magnetic resonance (NMR) and magnetic susceptibility (MS), with SIP, could reduce the ambiguity of interpretation that might result from a single method. Our research efforts entails combining measurements from these methods, each sensitive to different mineral forms and/or mineral-fluid interfaces, providing better constraints on changes in subsurface biogeochemical processes and pore geometries significantly improving our understanding of processes impacting contaminant remediation. The Rifle Integrated Field Research Challenge (IFRC) site was used as a test location for our measurements. The Rifle IFRC site is located at a former uranium ore-processing facility in Rifle, Colorado. Leachate from spent mill tailings has resulted in residual uranium contamination of both groundwater and sediments within the local aquifer. Studies at the site include an ongoing acetate amendment strategy, native microbial populations are stimulated by introduction of carbon intended to alter redox conditions and immobilize uranium. To test the geophysical methods in the field, NMR and MS logging measurements were collected before, during, and after acetate amendment. Next, laboratory NMR, MS, and SIP measurements

Many-body kinetics of dynamic nuclear polarization by the cross effect

Science.gov (United States)

Karabanov, A.; Wiśniewski, D.; Raimondi, F.; Lesanovsky, I.; Köckenberger, W.

2018-03-01

Dynamic nuclear polarization (DNP) is an out-of-equilibrium method for generating nonthermal spin polarization which provides large signal enhancements in modern diagnostic methods based on nuclear magnetic resonance. A particular instance is cross-effect DNP, which involves the interaction of two coupled electrons with the nuclear spin ensemble. Here we develop a theory for this important DNP mechanism and show that the nonequilibrium nuclear polarization buildup is effectively driven by three-body incoherent Markovian dissipative processes involving simultaneous state changes of two electrons and one nucleus. We identify different parameter regimes for effective polarization transfer and discuss under which conditions the polarization dynamics can be simulated by classical kinetic Monte Carlo methods. Our theoretical approach allows simulations of the polarization dynamics on an individual spin level for ensembles consisting of hundreds of nuclear spins. The insight obtained by these simulations can be used to find optimal experimental conditions for cross-effect DNP and to design tailored radical systems that provide optimal DNP efficiency.

System of measurement of proton polarization in a polarized target

Energy Technology Data Exchange (ETDEWEB)

Karnaukov, I.M.; Chechetenko, V.F.; Lukhanin, A.A.; Telegin, Y.N.; Trotsenko, V.I.

1985-05-01

This paper describes a nuclear magnetic resonance spectrometer with high sensitivity. The signal of NMR absorption is recorded by a Q-meter with a series circuit and a circuit for compensation of the resonance characteristic of the measuring circuit. In order to ensure uniform sensitivity of the system to the state of polarization throughout the volume of the target and to enhance the S/N ration the measuring coil is made of a flat conductor. The polarization-measuring system works on-line with an M-6000 computer. The total error of measurement of the polarization of free protons in a target with allowance for the error due to local depolarization of free protons in a target with allowance for the error due to local depolarization of the working substance under irradiation with an intense photon beam is less than or equal to 6%.

Nonlinear Magnetic Phenomena in Highly Polarized Target Materials

CERN Document Server

Kiselev, Yu F

2007-01-01

The report introduces and surveys nonlinear magnetic phenomena which have been observed at high nuclear polarizations in polarized targets of the SMC and of the COMPASS collaborations at CERN. Some of these phenomena, namely the frequency modulation eect and the distortion of the NMR line shape, promote the development of the polarized target technique. Others, as the spin-spin cross-relaxation between spin subsystems can be used for the development of quantum statistical physics. New findings bear on an electromagnetic noise and the spectrally resolved radiation from LiD with negatively polarized nuclei detected by low temperature bolometers. These nonlinear phenomena need to be taken into account for achieving the ultimate polarizations.

Nuclear magnetic resonance (NMR) imaging in the diagnosis of liver disease. Differential diagnosis of hepatic tumors and correlation between NMR imaging and histological findings

Energy Technology Data Exchange (ETDEWEB)

Ebara, Masaaki; Oto, Masao; Sugiura, Nobuyuki; Kimura, Kunio; Okuda, Kunio; Hirooka, Noboru; Ikehira, Hiroo; Fukuda, Nobuo; Tateno, Yukio

1984-06-01

Characteristics of nuclear magnetic resonance (NMR) images for various liver diseases were examined using a 0.1 T resistive NMR imaging unit on 26 patients with liver disease and 10 normal volunteers. Hepatic tumors, including small hepatocellular carcinoma 1.5 cm in diameter, were detected on NMR imaging. Ring sign characteristic of nodular type hepatocellular carcinoma was shown on NMR-CT in 60 % of patients. T/sub 1/ values allowed differential diagnosis of hepatic tumors. There was close correlation between NMR images and histopathological findings. The T/sub 1/ in the liver and spleen was more prolonged in patients with liver cirrhosis than in normal volunteers, with significant differences. (Namekawa, K.).

The origin of the mid-infrared nuclear polarization of active galactic nuclei

Science.gov (United States)

Lopez-Rodriguez, E.; Alonso-Herrero, A.; Diaz-Santos, T.; Gonzalez-Martin, O.; Ichikawa, K.; Levenson, N. A.; Martinez-Paredes, M.; Nikutta, R.; Packham, C.; Perlman, E.; Almeida, C. Ramos; Rodriguez-Espinosa, J. M.; Telesco, C. M.

2018-05-01

We combine new (NGC 1275, NGC 4151, and NGC 5506) and previously published (Cygnus A, Mrk 231, and NGC 1068) sub-arcsecond resolution mid-infrared (MIR; 8-13 μm) imaging- and spectro-polarimetric observations of six Seyfert galaxies using CanariCam on the 10.4-m Gran Telescopio CANARIAS. These observations reveal a diverse set of physical processes responsible for the nuclear polarization, and permit characterization of the origin of the MIR nuclear polarimetric signature of active galactic nuclei (AGN). For all radio quiet objects, we found that the nuclear polarization is low (sensitivity to detect such extended emission (i.e., NGC 1068 and NGC 4151). We suggest that the higher degree of polarization previously found in lower resolution data arises only on the larger-than-nuclear scales. Only the radio-loud Cygnus A exhibits significant nuclear polarization (˜11 per cent), attributable to synchrotron emission from the pc-scale jet close to the core. We present polarization models that suggest that the MIR nuclear polarization for highly obscured objects arises from a self-absorbed MIR polarized clumpy torus and/or dichroism from the host galaxy, while for unabsorbed cores, MIR polarization arises from dust scattering in the torus and/or surrounding nuclear dust.

Hyperpolarized NMR Probes for Biological Assays

Directory of Open Access Journals (Sweden)

Sebastian Meier

2014-01-01

Full Text Available During the last decade, the development of nuclear spin polarization enhanced (hyperpolarized molecular probes has opened up new opportunities for studying the inner workings of living cells in real time. The hyperpolarized probes are produced ex situ, introduced into biological systems and detected with high sensitivity and contrast against background signals using high resolution NMR spectroscopy. A variety of natural, derivatized and designed hyperpolarized probes has emerged for diverse biological studies including assays of intracellular reaction progression, pathway kinetics, probe uptake and export, pH, redox state, reactive oxygen species, ion concentrations, drug efficacy or oncogenic signaling. These probes are readily used directly under natural conditions in biofluids and are often directly developed and optimized for cellular assays, thus leaving little doubt about their specificity and utility under biologically relevant conditions. Hyperpolarized molecular probes for biological NMR spectroscopy enable the unbiased detection of complex processes by virtue of the high spectral resolution, structural specificity and quantifiability of NMR signals. Here, we provide a survey of strategies used for the selection, design and use of hyperpolarized NMR probes in biological assays, and describe current limitations and developments.

Order and chaos in the nonlinear response of driven nuclear spin systems

Energy Technology Data Exchange (ETDEWEB)

Brun, E; Derighetti, B; Holzner, R; Ravani, M [Zurich Univ. (Switzerland). Inst. fuer Physik

1984-01-01

The authors report on observations of ordered and chaotic behavior of a nonlinear system of strongly polarized nuclear spins inside the tuning coil of an NMR detector. The combined system: spins plus LC-circuit, may act as a nonlinear bistable absorber or a spin-flip laser, depending on the sign of the nuclear spin polarization. For the NMR laser experimental evidence is presented for limit-cycle behavior, sequences of bifurcations which lead to chaos, intermittency, multistability, and pronounced hysteresis effects. The experimental facts are compared with computer solutions of appropriate Bloch equations for the macroscopic order parameters.

The electron-spin--nuclear-spin interaction studied by polarized neutron scattering.

Science.gov (United States)

Stuhrmann, Heinrich B

2007-11-01

Dynamic nuclear spin polarization (DNP) is mediated by the dipolar interaction of paramagnetic centres with nuclear spins. This process is most likely to occur near paramagnetic centres at an angle close to 45 degrees with respect to the direction of the external magnetic field. The resulting distribution of polarized nuclear spins leads to an anisotropy of the polarized neutron scattering pattern, even with randomly oriented radical molecules. The corresponding cross section of polarized coherent neutron scattering in terms of a multipole expansion is derived for radical molecules in solution. An application using data of time-resolved polarized neutron scattering from an organic chromium(V) molecule is tested.

Measuring absolute spin polarization in dissolution-DNP by Spin PolarimetrY Magnetic Resonance (SPY-MR).

OpenAIRE

Vuichoud , Basile; Milani , Jonas; Chappuis , Quentin; Bornet , Aurélien; Bodenhausen , Geoffrey; Jannin , Sami

2015-01-01

Dynamic nuclear polarization at 1.2 K and 6.7 T allows one to achieve spin temperatures on the order of a few millikelvin, so that the high-temperature approximation (Delta E < kT) is violated for the nuclear Zeeman interaction Delta E = gamma B(0)h/(2 pi) of most isotopes. Provided that, after rapid dissolution and transfer to an NMR or MRI system, the hyperpolarized molecules contain at least two nuclear spins I and S with a scalar coupling J(IS), the polarization of spin I (short for 'inve...

Nuclear physics with polarized heavy ions

International Nuclear Information System (INIS)

Fick, D.; Grawert, G.; Turkiewicz, I.M.

1992-01-01

Polarized heavy ion beams ( 6 Li, 7 Li, 23 Na) have been in use as tools for the investigation of nuclear scattering and nuclear reactions for almost two decades. This review attempts to survey the research activities in this field with reference to nuclear structure, nuclear dynamics and reaction mechanisms. Besides reviewing the results from full quantum mechanical coupled channels analyses of data, special attention is paid to handwaving arguments and semiclassical pictures as a complementary way of obtaining a better understanding of the relevant physics. (orig.)

Level crossing analysis of chemically induced dynamic nuclear polarization: Towards a common description of liquid-state and solid-state cases

Energy Technology Data Exchange (ETDEWEB)

Sosnovsky, Denis V.; Ivanov, Konstantin L., E-mail: ivanov@tomo.nsc.ru [International Tomography Centre of SB RAS, Institutskaya 3a, 630090, Novosibirsk (Russian Federation); Novosibirsk State University, Pirogova 2, 630090, Novosibirsk (Russian Federation); Jeschke, Gunnar [Institut für Physikalische Chemie, ETH Zürich, Vladimir-Prelog-Weg 2, CH-8093 Zürich (Switzerland); Matysik, Jörg [Institut für Analytische Chemie, Universität Leipzig, Linnéstr. 3, D-04103 Leipzig (Germany); Vieth, Hans-Martin [International Tomography Centre of SB RAS, Institutskaya 3a, 630090, Novosibirsk (Russian Federation); Institut für Experimentalphysik, Freie Universität Berlin, Arnimallee 14, D-14195 Berlin (Germany)

2016-04-14

Chemically Induced Dynamic Nuclear Polarization (CIDNP) is an efficient method of creating non-equilibrium polarization of nuclear spins by using chemical reactions, which have radical pairs as intermediates. The CIDNP effect originates from (i) electron spin-selective recombination of radical pairs and (ii) the dependence of the inter-system crossing rate in radical pairs on the state of magnetic nuclei. The CIDNP effect can be investigated by using Nuclear Magnetic Resonance (NMR) methods. The gain from CIDNP is then two-fold: it allows one to obtain considerable amplification of NMR signals; in addition, it provides a very useful tool for investigating elusive radicals and radical pairs. While the mechanisms of the CIDNP effect in liquids are well established and understood, detailed analysis of solid-state CIDNP mechanisms still remains challenging; likewise a common theoretical frame for the description of CIDNP in both solids and liquids is missing. Difficulties in understanding the spin dynamics that lead to the CIDNP effect in the solid-state case are caused by the anisotropy of spin interactions, which increase the complexity of spin evolution. In this work, we propose to analyze CIDNP in terms of level crossing phenomena, namely, to attribute features in the CIDNP magnetic field dependence to Level Crossings (LCs) and Level Anti-Crossings (LACs) in a radical pair. This approach allows one to describe liquid-state CIDNP; the same holds for the solid-state case where anisotropic interactions play a significant role in CIDNP formation. In solids, features arise predominantly from LACs, since in most cases anisotropic couplings result in perturbations, which turn LCs into LACs. We have interpreted the CIDNP mechanisms in terms of the LC/LAC concept. This consideration allows one to find analytical expressions for a wide magnetic field range, where several different mechanisms are operative; furthermore, the LAC description gives a way to determine CIDNP sign

Development and applications of NMR [nuclear magnetic resonance] in low fields and zero field

International Nuclear Information System (INIS)

Bielecki, A.

1987-05-01

This dissertation is about nuclear magnetic resonance (NMR) spectroscopy in the absence of applied magnetic fields. NMR is usually done in large magnetic fields, often as large as can be practically attained. The motivation for going the opposite way, toward zero field, is that for certain types of materials, particularly powdered or polycrystalline solids, the NMR spectra in zero field are easier to interpret than those obtained in high field. 92 refs., 60 figs., 1 tab

Self-Sustaining Dynamical Nuclear Polarization Oscillations in Quantum Dots

DEFF Research Database (Denmark)

Rudner, Mark Spencer; Levitov, Leonid

2013-01-01

Early experiments on spin-blockaded double quantum dots revealed robust, large-amplitude current oscillations in the presence of a static (dc) source-drain bias. Despite experimental evidence implicating dynamical nuclear polarization, the mechanism has remained a mystery. Here we introduce......) and nuclear spin diffusion, which governs dynamics of the spatial profile of nuclear polarization. The proposed framework naturally explains the differences in phenomenology between vertical and lateral quantum dot structures as well as the extremely long oscillation periods....

Monitoring microbial growth and activity using spectral induced polarization and low-field nuclear magnetic resonance

Science.gov (United States)

Zhang, Chi; Keating, Kristina; Revil, Andre

2015-04-01

Microbes and microbial activities in the Earth's subsurface play a significant role in shaping subsurface environments and are involved in environmental applications such as remediation of contaminants in groundwater and oil fields biodegradation. Stimulated microbial growth in such applications could cause wide variety of changes of physical/chemical properties in the subsurface. It is critical to monitor and determine the fate and transportation of microorganisms in the subsurface during such applications. Recent geophysical studies demonstrate the potential of two innovative techniques, spectral induced polarization (SIP) and low-field nuclear magnetic resonance (NMR), for monitoring microbial growth and activities in porous media. The SIP measures complex dielectric properties of porous media at low frequencies of exciting electric field, and NMR studies the porous structure of geologic media and characterizes fluids subsurface. In this laboratory study, we examined both SIP and NMR responses from bacterial growth suspension as well as suspension mixed with silica sands. We focus on the direct contribution of microbes to the SIP and NMR signals in the absence of biofilm formation or biomineralization. We used Zymomonas mobilis and Shewanella oneidensis (MR-1) for SIP and NMR measurements, respectively. The SIP measurements were collected over the frequency range of 0.1 - 1 kHz on Z. mobilis growth suspension and suspension saturated sands at different cell densities. SIP data show two distinct peaks in imaginary conductivity spectra, and both imaginary and real conductivities increased as microbial density increased. NMR data were collected using both CPMG pulse sequence and D-T2 mapping to determine the T2-distribution and diffusion properties on S. oneidensis suspension, pellets (live and dead), and suspension mixed with silica sands. NMR data show a decrease in the T2-distribution in S. oneidensis suspension saturated sands as microbial density increase. A

8. Nuclear magnetic resonance users meeting; 1. Luso-Brazilian NMR meeting. Abstracts

International Nuclear Information System (INIS)

2001-01-01

The NMR Users Meeting is held every year in Brazil and its eighth edition took place from May 7 - 11, 2001 together with the first Luso-Brazilian Meeting on Nuclear Magnetic Resonance. The extended abstracts book comprise: ten major conferences, four plenary lectures delivered by enterprise representatives (three from USA and one from Germany), six talks about the state-of-the-art of NMR methods (especially bi and tri-dimensional new techniques) and summaries of results from one hundred and twenty four research works. Among these research results which have been discussed, one hundred and sixteen were presented as congress panels/posters and eight as oral communications. The major topics of the scientific and technological research works are thus distributed: 63% in chemical sciences (mainly structural elucidation and stereochemistry of organic compounds and dynamical studies of chemical reactions), 19% in materials science (including petroleum), 8% in applied life sciences (agricultural and food sciences, biological sciences and medicine), 8% about theoretical aspects related to nuclear magnetic resonance and 2% regarding improvements in NMR instrumental techniques

ULF-NMR system using HTS-SQUID and permanent magnet

Energy Technology Data Exchange (ETDEWEB)

Fukumoto, Shohei, E-mail: hatukade@ens.tut.ac.jp [Toyohashi University of Technology, 1-1 Hibarigaoka, Tempaku-cho, Toyohashi, Aichi 441-8580 (Japan); Tsunaki, Shingo; Chigasaki, Takumi; Hatsukade, Yoshimi; Tanaka, Saburo [Toyohashi University of Technology, 1-1 Hibarigaoka, Tempaku-cho, Toyohashi, Aichi 441-8580 (Japan)

2013-01-15

Highlights: ► A permanent magnet was introduced into a ULF SQUID-NMR system for polarization. ► An instrument to transfer a sample in the magnet to under a SQUID was implemented. ► An AC pulse coil was also introduced to apply a π/2 pulse to obtain an NMR signal. ► A {sup 1}H NMR signal was measured while applying a static field of 45 μT. ► The signal to noise ratio of the {sup 1}H NMR signal was about 100. -- Abstract: We have constructed an ultra-low field (ULF) nuclear magnetic resonance (NMR)/magnetic resonance imaging (MRI) system using an HTS-rf-SQUID and room-temperature electromagnets in a magnetically shielded room (MSR). In this study, in order to improve the signal to noise ratio (S/N) of the system, we introduced a permanent magnet instead of the electromagnet for pre-polarizing the sample to enhance the pre-polarizing field (B{sub p}). The cylindrical permanent magnet of 270 mT was used to magnetize a water sample for several seconds outside the MSR and about 1.5 m away from the SQUID. We constructed an instrument to transfer the magnetized sample from the permanent magnet to under the SQUID in 0.5 s. Since the non-adiabatic condition cannot be kept in such sample transfer scheme, an AC pulse coil to apply an AC pulse field B{sub AC} to rotate the magnetization moments for π/2 was introduced to measure a free induction decay (FID) signal from the sample. By this system, we obtained an NMR signal from the water sample of 10 ml while applying a static field of 45 μT and π/2 pulse after the transfer. The S/N of the NMR spectrum was about 100 by a single shot, which was 10 times larger than that obtained with the electromagnet of 32 mT. In addition, we demonstrated the measurements of the longitudinal relaxation time (T{sub 1}) and the spin echo signal of the water sample by the system.

Optical pumping and xenon NMR

International Nuclear Information System (INIS)

Raftery, M.D.

1991-11-01

Nuclear Magnetic Resonance (NMR) spectroscopy of xenon has become an important tool for investigating a wide variety of materials, especially those with high surface area. The sensitivity of its chemical shift to environment, and its chemical inertness and adsorption properties make xenon a particularly useful NMR probe. This work discusses the application of optical pumping to enhance the sensitivity of xenon NMR experiments, thereby allowing them to be used in the study of systems with lower surface area. A novel method of optically-pumping 129 Xe in low magnetic field below an NMR spectrometer and subsequent transfer of the gas to high magnetic field is described. NMR studies of the highly polarized gas adsorbed onto powdered samples with low to moderate surface areas are now possible. For instance, NMR studies of optically-pumped xenon adsorbed onto polyacrylic acid show that xenon has a large interaction with the surface. By modeling the low temperature data in terms of a sticking probability and the gas phase xenon-xenon interaction, the diffusion coefficient for xenon at the surface of the polymer is determined. The sensitivity enhancement afforded by optical pumping also allows the NMR observation of xenon thin films frozen onto the inner surfaces of different sample cells. The geometry of the thin films results in interesting line shapes that are due to the bulk magnetic susceptibility of xenon. Experiments are also described that combine optical pumping with optical detection for high sensitivity in low magnetic field to observe the quadrupoler evolution of 131 Xe spins at the surface of the pumping cells. In cells with macroscopic asymmetry, a residual quadrupolar interaction causes a splitting in the 131 Xe NMR frequencies in bare Pyrex glass cells and cells with added hydrogen

NMR analog of Bell's inequalities violation test

International Nuclear Information System (INIS)

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

2008-01-01

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

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

Spin polarized states in strongly asymmetric nuclear matter

International Nuclear Information System (INIS)

Isayev, A.A.; Yang, J.

2004-01-01

The possibility of appearance of spin polarized states in strongly asymmetric nuclear matter is analyzed within the framework of a Fermi liquid theory with the Skyrme effective interaction. The zero temperature dependence of the neutron and proton spin polarization parameters as functions of density is found for SLy4 and SLy5 effective forces. It is shown that at some critical density strongly asymmetric nuclear matter undergoes a phase transition to the state with the oppositely directed spins of neutrons and protons while the state with the same direction of spins does not appear. In comparison with neutron matter, even small admixture of protons strongly decreases the threshold density of spin instability. It is clarified that protons become totally polarized within a very narrow density domain while the density profile of the neutron spin polarization parameter is characterized by the appearance of long tails near the transition density

UTOPIA NMR: activating unexploited magnetization using interleaved low-gamma detection

Energy Technology Data Exchange (ETDEWEB)

Viegas, Aldino; Viennet, Thibault [Heinrich-Heine-University, Institute of Physical Biology (Germany); Yu, Tsyr-Yan [Academia Sinica, Institute of Atomic and Molecular Sciences (China); Schumann, Frank [Bruker BioSpin GmbH (Switzerland); Bermel, Wolfgang [Bruker BioSpin GmbH (Germany); Wagner, Gerhard [Harvard Medical School, Department of Biological Chemistry and Molecular Pharmacology (United States); Etzkorn, Manuel, E-mail: manuel.etzkorn@hhu.de [Heinrich-Heine-University, Institute of Physical Biology (Germany)

2016-01-15

A growing number of nuclear magnetic resonance (NMR) spectroscopic studies are impaired by the limited information content provided by the standard set of experiments conventionally recorded. This is particularly true for studies of challenging biological systems including large, unstructured, membrane-embedded and/or paramagnetic proteins. Here we introduce the concept of unified time-optimized interleaved acquisition NMR (UTOPIA-NMR) for the unified acquisition of standard high-γ (e.g. {sup 1}H) and low-γ (e.g. {sup 13}C) detected experiments using a single receiver. Our aim is to activate the high level of polarization and information content distributed on low-γ nuclei without disturbing conventional magnetization transfer pathways. We show that using UTOPIA-NMR we are able to recover nearly all of the normally non-used magnetization without disturbing the standard experiments. In other words, additional spectra, that can significantly increase the NMR insights, are obtained for free. While we anticipate a broad range of possible applications we demonstrate for the soluble protein Bcl-x{sub L} (ca. 21 kDa) and for OmpX in nanodiscs (ca. 160 kDa) that UTOPIA-NMR is particularly useful for challenging protein systems including perdeuterated (membrane) proteins.

UTOPIA NMR: activating unexploited magnetization using interleaved low-gamma detection

International Nuclear Information System (INIS)

Viegas, Aldino; Viennet, Thibault; Yu, Tsyr-Yan; Schumann, Frank; Bermel, Wolfgang; Wagner, Gerhard; Etzkorn, Manuel

2016-01-01

A growing number of nuclear magnetic resonance (NMR) spectroscopic studies are impaired by the limited information content provided by the standard set of experiments conventionally recorded. This is particularly true for studies of challenging biological systems including large, unstructured, membrane-embedded and/or paramagnetic proteins. Here we introduce the concept of unified time-optimized interleaved acquisition NMR (UTOPIA-NMR) for the unified acquisition of standard high-γ (e.g. 1 H) and low-γ (e.g. 13 C) detected experiments using a single receiver. Our aim is to activate the high level of polarization and information content distributed on low-γ nuclei without disturbing conventional magnetization transfer pathways. We show that using UTOPIA-NMR we are able to recover nearly all of the normally non-used magnetization without disturbing the standard experiments. In other words, additional spectra, that can significantly increase the NMR insights, are obtained for free. While we anticipate a broad range of possible applications we demonstrate for the soluble protein Bcl-x L (ca. 21 kDa) and for OmpX in nanodiscs (ca. 160 kDa) that UTOPIA-NMR is particularly useful for challenging protein systems including perdeuterated (membrane) proteins

UTOPIA NMR: activating unexploited magnetization using interleaved low-gamma detection.

Science.gov (United States)

Viegas, Aldino; Viennet, Thibault; Yu, Tsyr-Yan; Schumann, Frank; Bermel, Wolfgang; Wagner, Gerhard; Etzkorn, Manuel

2016-01-01

A growing number of nuclear magnetic resonance (NMR) spectroscopic studies are impaired by the limited information content provided by the standard set of experiments conventionally recorded. This is particularly true for studies of challenging biological systems including large, unstructured, membrane-embedded and/or paramagnetic proteins. Here we introduce the concept of unified time-optimized interleaved acquisition NMR (UTOPIA-NMR) for the unified acquisition of standard high-γ (e.g. (1)H) and low-γ (e.g. (13)C) detected experiments using a single receiver. Our aim is to activate the high level of polarization and information content distributed on low-γ nuclei without disturbing conventional magnetization transfer pathways. We show that using UTOPIA-NMR we are able to recover nearly all of the normally non-used magnetization without disturbing the standard experiments. In other words, additional spectra, that can significantly increase the NMR insights, are obtained for free. While we anticipate a broad range of possible applications we demonstrate for the soluble protein Bcl-xL (ca. 21 kDa) and for OmpX in nanodiscs (ca. 160 kDa) that UTOPIA-NMR is particularly useful for challenging protein systems including perdeuterated (membrane) proteins.

$\\beta$-NMR of copper isotopes in ionic liquids

CERN Multimedia

We propose to test the feasibility of spin-polarization and $\\beta$-NMR studies on several short-lived copper isotopes, $^{58}$ Cu, $^{74}$Cu and $^{75}$Cu in crystals and liquids. The motivation is given by biological studies of Cu with $\\beta$-NMR in liquid samples, since Cu is present in a large number of enzymes involved in electron transfer and activation of oxygen. The technique is based on spin-polarization via optical pumping in the new VITO beamline. We will use the existing lasers, NMR magnet and NMR chambers and we will prepare a new optical pumping system. The studies will be devoted to tests of achieved $\\beta$-asymmetry in solid hosts, the behaviour of asymmetry when increasing vacuum, and finally NMR scans in ionic liquids. The achieved spin polarization will be also relevant for the plans to measure with high precision the magnetic moments of neutron-rich Cu isotopes.

Nuclear magnetic resonance (NMR) imaging of Arnold-Chiari type I malformation with hydromyelia

International Nuclear Information System (INIS)

DeLaPaz, R.L.; Brady, T.J.; Buonanno, F.S.; New, P.F.; Kistler, J.P.; McGinnis, B.D.; Pykett, I.L.; Taveras, J.M.

1983-01-01

Saturation recovery nuclear magnetic resonance (NMR) images and metrizamide computed tomography (CT) scans were obtained in an adult patient with a clinical history suggestive of syringomyelia. Both NMR and CT studies showed low lying cerebellar tonsils. The CT study demonstrated central cavitation of the spinal cord from the midthoracic to midcervical levels but could not exclude an intramedullary soft tissue mass at the cervico-medullary junction. The NMR images in transverse, coronal, and sagittal planes demonstrated extension of an enlarged central spinal cord cerebrospinal fluid space to the cervico-medullary junction. This was felt to be strong evidence for exclusion of an intramedullary soft tissue mass and in favor of a diagnosis of Arnold-Chiari Type I malformation with hydromyelia. The noninvasive nature of spinal cord and cervico-medullary junction evaluation with NMR is emphasized

Solid and liquid 129Xe NMR signals enhanced by spin-exchange optical pumping under flow

International Nuclear Information System (INIS)

Zhou Xin; Luo Jun; Sun Xianping; Zeng Xizhi; Liu Maili; Liu Wuyang

2002-01-01

Laser-polarized 129 Xe gas was produced by spin-exchange with Cs atom optically pumped with diode laser array in a low field under flow. The nuclear spin polarizations of the solid and liquid 129 Xe frozen from the laser-polarized 129 Xe gas were 2.16% and 1.45% respectively in the SY-80M NMR spectrometer, which corresponded to the enhancements of 6000 and 5000 compared to those without optical pumping under the same conditions. It could provide the base and possibility for quantum computers using laser-enhanced solid and liquid 129 Xe. Polarization loss of transport and state change was also discussed

The polarized double cell target of the SMC

International Nuclear Information System (INIS)

Adams, D.; Adeva, B.; Arik, E.; Arvidson, A.; Badelek, B.; Ballintijn, M.K.; Bardin, G.; Baum, G.; Berglund, P.; Betev, L.; Bird, I.G.; Birsa, R.; Bjoerkholm, P.; Bonner, B.E.; Botton, N. de; Boutemeur, M.; Bradamante, F.; Bravar, A.; Bressan, A.; Bueltmann, S.; Burtin, E.; Cavata, C.; Crabb, D.; Cranshaw, J.; Cuhadar, T.; Torre, S. Dalla; Dantzig, R. van; Derro, B.; Deshpande, A.; Dhawan, S.; Dulya, C.; Dyring, A.; Eichblatt, S.; Faivre, J.C.; Fasching, D.; Feinstein, F.; Fernandez, C.; Forthmann, S.; Frois, B.; Gallas, A.; Garzon, J.A.; Gaussiran, T.; Gilly, H.; Giorgi, M.; Goeler, E. von; Goertz, S.; Gracia, G.; Groot, N. de; Perdekamp, M. Grosse; Guelmez, E.; Haft, K.; Harrach, D. von; Hasegawa, T.; Hautle, P.; Hayashi, N.; Heusch, C.A.; Horikawa, N.; Hughes, V.W.; Igo, G.; Ishimoto, S.; Iwata, T.; Kabuss, E.M.; Kageya, T.; Karev, A.; Kessler, H.J.; Ketel, T.J.; Kiryluk, J.; Kishi, A.; Kisselev, Yu.; Klostermann, L.; Kraemer, D.; Krivokhijine, V.; Kroeger, W.; Kurek, K.; Kyynaeraeinen, J.; Lamanna, M.; Landgraf, U.; Layda, T.; Le Goff, J.M.; Lehar, F.; Lesquen, A. de; Lichtenstadt, J.; Lindqvist, T.; Litmaath, M.; Lowe, M.; Magnon, A.; Mallot, G.K.; Marie, F.; Martin, A.; Martino, J.; Matsuda, T.; Mayes, B.; McCarthy, J.S.; Medved, K.; Meyer, W.; Middelkoop, G. van; Miller, D.; Miyachi, Y.; Mori, K.; Moromisato, J.; Nassalski, J.; Naumann, L.; Neganov, B.; Niinikoski, T.O.; Oberski, J.E.J.; Ogawa, A.; Ozben, C.; Parks, D.P.; Pereira, H.; Penzo, A.; Perrot-Kunne, F.; Peshekhonov, D.; Piegaia, R.; Pinsky, L.; Platchkov, S.; Plo, M.; Pose, D.; Postma, H.; Pretz, J.; Pussieux, T.; Pyrlik, J.; Raedel, G.; Reyhancan, I.; Reicherz, G.; Rieubland, J.M.; Rijllart, A.; Roberts, J.B.; Rock, S.; Rodriguez, M.; Rondio, E.; Rosado, A.; Roscherr, B.; Sabo, I.; Saborido, J.; Sandacz, A.; Savin, I.; Schiavon, P.; Schiller, A.; Schueler, K.P.; Segel, R.; Seitz, R.; Semertzidis, Y.; Sever, F.; Shanahan, P.; Sichtermann, E.P.; Simeoni, F.; Smirnov, G.I.; Staude, A.; Steinmetz, A.; Stiegler, U.; Stuhrmann, H.; Szleper, M.; Teichert, K.M.; Tessarotto, F.; Thers, D.; Tlaczala, W.; Trentalange, S.; Tripet, A.; Unel, G.; Velasco, M.; Vogt, J.; Voss, R.; Weinstein, R.; Whitten, C.; Windmolders, R.; Willumeit, R.; Wislicki, W.; Witzmann, A.; Zanetti, A.M.; Zaremba, K.; Zhao, J.

1999-01-01

The polarized target of the Spin Muon Collaboration at CERN was used for deep inelastic muon scattering experiments during 1993-1996 with a polarized muon beam to investigate the spin structure of the nucleon. Most of the experiments were carried out with longitudinal target polarization and 190 GeV muons, and some were done with transverse polarization and 100 GeV muons. Protons as well as deuterons were polarized by dynamic nuclear polarization (DNP) in three kinds of solid materials -- butanol, ammonia, and deuterated butanol -- with maximum degrees of polarization of 94%, 91% and 60%, respectively. Considerable attention was paid to the accuracies of the NMR polarization measurements and their analyses, the accuracies achieved were between 2.0% and 3.2%. The SMC target system with two cells of opposite polarizations, each cell 65 cm long and 5 cm in diameter, constitutes the largest polarized target system ever built and facilitates accurate spin asymmetry measurements. The design considerations, construction and performance of the target are reviewed

The polarized double cell target of the SMC

CERN Document Server

Adams, D; Adeva, B; Arik, E; Arvidson, A; Badelek, B; Ballintijn, M K; Bardin, G; Baum, G; Berglund, P; Betev, L; Bird, I G; Birsa, R; Björkholm, P; Bonner, B E; De Botton, N R; Boutemeur, M; Bradamante, Franco; Bravar, A; Bressan, A; Bültmann, S; Burtin, E; Cavata, C; Crabb, D; Cranshaw, J; Çuhadar-Dönszelmann, T; Dalla Torre, S; Van Dantzig, R; Derro, B R; Deshpande, A A; Dhawan, S K; Dulya, C M; Dyring, A; Eichblatt, S; Faivre, Jean-Claude; Fasching, D; Feinstein, F; Fernández, C; Forthmann, S; Frois, Bernard; Gallas, A; Garzón, J A; Gaussiran, T; Gilly, H; Giorgi, M A; von Goeler, E; Görtz, S; Gracia, G; De Groot, N; Grosse-Perdekamp, M; Gülmez, E; Haft, K; Von Harrach, D; Hasegawa, T; Hautle, P; Hayashi, N; Heusch, C A; Horikawa, N; Hughes, V W; Igo, G; Ishimoto, S; Iwata, T; Kabuss, E M; Kageya, T; Karev, A G; Kessler, H J; Ketel, T; Kiryluk, J; Kishi, A; Kiselev, Yu F; Klostermann, L; Krämer, Dietrich; Krivokhizhin, V G; Kröger, W; Kurek, K; Kyynäräinen, J; Lamanna, M; Landgraf, U; Layda, T; Le Goff, J M; Lehár, F; de Lesquen, A; Lichtenstadt, J; Lindqvist, T; Litmaath, M; Loewe, M; Magnon, A; Mallot, G K; Marie, F; Martin, A; Martino, J; Matsuda, T; Mayes, B W; McCarthy, J S; Medved, K S; Meyer, W T; Van Middelkoop, G; Miller, D; Miyachi, Y; Mori, K; Moromisato, J H; Nassalski, J P; Naumann, Lutz; Neganov, B S; Niinikoski, T O; Oberski, J; Ogawa, A; Ozben, C; Parks, D P; Pereira, H; Penzo, Aldo L; Perrot-Kunne, F; Peshekhonov, V D; Piegaia, R; Pinsky, L; Platchkov, S K; Pló, M; Pose, D; Postma, H; Pretz, J; Pussieux, T; Pyrlik, J; Rädel, G; Reyhancan, I; Reicherz, G; Rijllart, A; Roberts, J B; Rock, S E; Rodríguez, M; Rondio, Ewa; Rosado, A; Roscherr, B; Sabo, I; Saborido, J; Sandacz, A; Savin, I A; Schiavon, R P; Schiller, A; Schüler, K P; Segel, R E; Seitz, R; Semertzidis, Y K; Sever, F; Shanahan, P; Sichtermann, E P; Simeoni, F; Smirnov, G I; Staude, A; Steinmetz, A; Stiegler, U; Stuhrmann, H B; Szleper, M; Teichert, K M; Tessarotto, F; Thers, D; Tlaczala, W; Trentalange, S; Tripet, A; Ünel, G; Velasco, M; Vogt, J; Voss, Rüdiger; Weinstein, R; Whitten, C; Windmolders, R; Willumeit, R; Wislicki, W; Witzmann, A; Zanetti, A M; Zaremba, K; Zhao, J

1999-01-01

The polarized target of the Spin Muon Collaboration at CERN was used for deep inelastic muon scattering experiments during 1993 to 1996 with a polarized muon beam to investigate the spin structure of the nucleon. Most of the experiments were carried out with longitudinal target polarization and 190 GeV muons, and some were done with transverse polarization and 100 GeV muons. Protons as well as deuterons were polarized by dynamic nuclear polarization (DNP) in three kinds of solid materials $-$ butanol, ammonia, and deuterated butanol, with maximum degrees of polarization of 94, 91, and 60 \\%, respectively. Considerable attention was paid to the accuracies of the NMR polarization measurements and their analyses. The achieved accuracies were between 2.0 and 3.2 \\%. The SMC target system with two cells of opposite polarizations, each cell 65 cm long and 5 cm in diameter, constitutes the largest polarized target system ever built and facilitates accurate spin asymmetry measurements. The design considerations, the ...

Principles of nuclear magnetic resonance (NMR) - current state of the art

International Nuclear Information System (INIS)

Lerski, R.A.

1985-01-01

Nuclear magnetic resonance (NMR) imaging has progressed rapidly from laboratory curiosity to commercial exploitation and clinical application in the space of only three years. The physical principles underlying the technique are described and the equipment requirements outlined. The question of optimal magnetic field strength is discussed. (author)

Oocyte Polarization Is Coupled to the Chromosomal Bouquet, a Conserved Polarized Nuclear Configuration in Meiosis.

Directory of Open Access Journals (Sweden)

Yaniv M Elkouby

2016-01-01

Full Text Available The source of symmetry breaking in vertebrate oocytes is unknown. Animal-vegetal oocyte polarity is established by the Balbiani body (Bb, a conserved structure found in all animals examined that contains an aggregate of specific mRNAs, proteins, and organelles. The Bb specifies the oocyte vegetal pole, which is key to forming the embryonic body axes as well as the germline in most vertebrates. How Bb formation is regulated and how its asymmetric position is established are unknown. Using quantitative image analysis, we trace oocyte symmetry breaking in zebrafish to a nuclear asymmetry at the onset of meiosis called the chromosomal bouquet. The bouquet is a universal feature of meiosis where all telomeres cluster to one pole on the nuclear envelope, facilitating chromosomal pairing and meiotic recombination. We show that Bb precursor components first localize with the centrosome to the cytoplasm adjacent to the telomere cluster of the bouquet. They then aggregate around the centrosome in a specialized nuclear cleft that we identified, assembling the early Bb. We show that the bouquet nuclear events and the cytoplasmic Bb precursor localization are mechanistically coordinated by microtubules. Thus the animal-vegetal axis of the oocyte is aligned to the nuclear axis of the bouquet. We further show that the symmetry breaking events lay upstream to the only known regulator of Bb formation, the Bucky ball protein. Our findings link two universal features of oogenesis, the Bb and the chromosomal bouquet, to oocyte polarization. We propose that a meiotic-vegetal center couples meiosis and oocyte patterning. Our findings reveal a novel mode of cellular polarization in meiotic cells whereby cellular and nuclear polarity are aligned. We further reveal that in zygotene nests, intercellular cytoplasmic bridges remain between oocytes and that the position of the cytoplasmic bridge coincides with the location of the centrosome meiotic-vegetal organizing center

From single-site tantalum complexes to nanoparticles of TaxNy and TaOxNy supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy

KAUST Repository

Mohandas, Janet Chakkamadathil

2017-06-08

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of TaxNy and TaOxNy with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe5 (Me = methyl) and dimeric Ta-2(OMe)(10) with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of H-1, C-13, Si-29, and N-15 at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O-2 insertion into Ta-CH3 species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta-2(OMe)(10) on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H2O2 serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as TaxNy/TaOxNy.

Nuclear Fusion with Polarized Nucleons & PolFusion

CERN Document Server

Engels, Ralf; Büscher, Markus; Vasilyev, Alexander

2016-01-01

This book offers a detailed examination of the latest work on the potential of polarized fuel to realize the vision of energy production by nuclear fusion. It brings together contributions from nuclear physicists and fusion physicists with the aims of fostering exchange of information between the two communities, describing the current status in the field, and examining new ideas and projects under development. It is evident that polarized fuel can offer huge improvements for the first generation of fusion reactors and open new technological possibilities for future generations, including neutron lean reactors, which could be the most popular and sustainable energy production option to avoid environmental problems. Nevertheless, many questions must be resolved before polarized fuel can be used for energy production in the different reactor types. Readers will find this book to be a stimulating source of information on the key issues. It is based on contributions from leading scientists delivered at the meetin...

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

Structure and dynamics of paramagnetic transients by pulsed EPR and NMR detection of nuclear resonance

International Nuclear Information System (INIS)

Trifunac, A.D.

1981-01-01

Structure and dynamics of transient radicals in pulse radiolysis can be studied by time resolved EPR and NMR techniques. EPR study of kinetics and relaxation is illustrated. The NMR detection of nuclear resonance in transient radicals is a new method which allows the study of hyperfine coupling, population dynamics, radical kinetics, and reaction mechanism. 9 figures

Parahydrogen-enhanced zero-field nuclear magnetic resonance

Science.gov (United States)

Theis, T.; Ganssle, P.; Kervern, G.; Knappe, S.; Kitching, J.; Ledbetter, M. P.; Budker, D.; Pines, A.

2011-07-01

Nuclear magnetic resonance, conventionally detected in magnetic fields of several tesla, is a powerful analytical tool for the determination of molecular identity, structure and function. With the advent of prepolarization methods and detection schemes using atomic magnetometers or superconducting quantum interference devices, interest in NMR in fields comparable to the Earth's magnetic field and below (down to zero field) has been revived. Despite the use of superconducting quantum interference devices or atomic magnetometers, low-field NMR typically suffers from low sensitivity compared with conventional high-field NMR. Here we demonstrate direct detection of zero-field NMR signals generated through parahydrogen-induced polarization, enabling high-resolution NMR without the use of any magnets. The sensitivity is sufficient to observe spectra exhibiting 13C-1H scalar nuclear spin-spin couplings (known as J couplings) in compounds with 13C in natural abundance, without the need for signal averaging. The resulting spectra show distinct features that aid chemical fingerprinting.

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

Development of Laser-Polarized Noble Gas Magnetic Resonance Imaging (MRI) Technology

Science.gov (United States)

Walsworth, Ronald L.

2004-01-01

We are developing technology for laser-polarized noble gas nuclear magnetic resonance (NMR), with the aim of enabling it as a novel biomedical imaging tool for ground-based and eventually space-based application. This emerging multidisciplinary technology enables high-resolution gas-space magnetic resonance imaging (MRI)-e.g., of lung ventilation, perfusion, and gas-exchange. In addition, laser-polarized noble gases (3He and 1BXe) do not require a large magnetic field for sensitive NMR detection, opening the door to practical MRI with novel, open-access magnet designs at very low magnetic fields (and hence in confined spaces). We are pursuing two specific aims in this technology development program. The first aim is to develop an open-access, low-field (less than 0.01 T) instrument for MRI studies of human gas inhalation as a function of subject orientation, and the second aim is to develop functional imaging of the lung using laser-polarized He-3 and Xe-129.

Nuclear spin polarized H and D by means of spin-exchange optical pumping

Science.gov (United States)

Stenger, Jörn; Grosshauser, Carsten; Kilian, Wolfgang; Nagengast, Wolfgang; Ranzenberger, Bernd; Rith, Klaus; Schmidt, Frank

1998-01-01

Optically pumped spin-exchange sources for polarized hydrogen and deuterium atoms have been demonstrated to yield high atomic flow and high electron spin polarization. For maximum nuclear polarization the source has to be operated in spin temperature equilibrium, which has already been demonstrated for hydrogen. In spin temperature equilibrium the nuclear spin polarization PI equals the electron spin polarization PS for hydrogen and is even larger than PS for deuterium. We discuss the general properties of spin temperature equilibrium for a sample of deuterium atoms. One result are the equations PI=4PS/(3+PS2) and Pzz=PSṡPI, where Pzz is the nuclear tensor polarization. Furthermore we demonstrate that the deuterium atoms from our source are in spin temperature equilibrium within the experimental accuracy.

Simulation and Automation of Microwave Frequency Control in Dynamic Nuclear Polarization for Solid Polarized Targets

Science.gov (United States)

Perera, Gonaduwage; Johnson, Ian; Keller, Dustin

2017-09-01

Dynamic Nuclear Polarization (DNP) is used in most of the solid polarized target scattering experiments. Those target materials must be irradiated using microwaves at a frequency determined by the difference in the nuclear Larmor and electron paramagnetic resonance (EPR) frequencies. But the resonance frequency changes with time as a result of radiation damage. Hence the microwave frequency should be adjusted accordingly. Manually adjusting the frequency can be difficult, and improper adjustments negatively impact the polarization. In order to overcome these difficulties, two controllers were developed which automate the process of seeking and maintaining the optimal frequency: one being a standalone controller for a traditional DC motor and the other a LabVIEW VI for a stepper motor configuration. Further a Monte-Carlo simulation was developed which can accurately model the polarization over time as a function of microwave frequency. In this talk, analysis of the simulated data and recent improvements to the automated system will be presented. DOE.

Multiaxial Polarity Determines Individual Cellular and Nuclear Chirality.

Science.gov (United States)

Raymond, Michael J; Ray, Poulomi; Kaur, Gurleen; Fredericks, Michael; Singh, Ajay V; Wan, Leo Q

2017-02-01

Intrinsic cell chirality has been implicated in the left-right (LR) asymmetry of embryonic development. Impaired cell chirality could lead to severe birth defects in laterality. Previously, we detected cell chirality with an in vitro micropatterning system. Here, we demonstrate for the first time that chirality can be quantified as the coordination of multiaxial polarization of individual cells and nuclei. Using an object labeling, connected component based method, we characterized cell chirality based on cell and nuclear shape polarization and nuclear positioning of each cell in multicellular patterns of epithelial cells. We found that the cells adopted a LR bias the boundaries by positioning the sharp end towards the leading edge and leaving the nucleus at the rear. This behavior is consistent with the directional migration observed previously on the boundary of micropatterns. Although the nucleus is chirally aligned, it is not strongly biased towards or away from the boundary. As the result of the rear positioning of nuclei, the nuclear positioning has an opposite chirality to that of cell alignment. Overall, our results have revealed deep insights of chiral morphogenesis as the coordination of multiaxial polarization at the cellular and subcellular levels.

Boundary between the thermal and statistical polarization regimes in a nuclear spin ensemble

International Nuclear Information System (INIS)

Herzog, B. E.; Cadeddu, D.; Xue, F.; Peddibhotla, P.; Poggio, M.

2014-01-01

As the number of spins in an ensemble is reduced, the statistical fluctuations in its polarization eventually exceed the mean thermal polarization. This transition has now been surpassed in a number of recent nuclear magnetic resonance experiments, which achieve nanometer-scale detection volumes. Here, we measure nanometer-scale ensembles of nuclear spins in a KPF 6 sample using magnetic resonance force microscopy. In particular, we investigate the transition between regimes dominated by thermal and statistical nuclear polarization. The ratio between the two types of polarization provides a measure of the number of spins in the detected ensemble.

The 40th anniversary of the discovery of NMR-chemical shift and nuclear spin-spin coupling

International Nuclear Information System (INIS)

Zhu Zhenghe; Gou Qingquan

1989-01-01

After the discovery of NMR Phenomenon in the physics laboratories of E.M.Purcell at Harvard and F.Bloch at Stanford in 1946, W.G.Proctor and F.C.Yu made the successful discovery of NMR-chemical shift and nuclear spin-spin coupling at Stanford in 1950, Which brought NMR spectroscopy from the physics laboratory to the laboratories of many different fields. This is worth memorizing. Retrospecting the past 40 years, it is sure that chemical shift theory will be much more prosperous prospects

Integrated microchip incorporating atomic magnetometer and microfluidic channel for NMR and MRI

Science.gov (United States)

Ledbetter, Micah P [Oakland, CA; Savukov, Igor M [Los Alamos, NM; Budker, Dmitry [El Cerrito, CA; Shah, Vishal K [Plainsboro, NJ; Knappe, Svenja [Boulder, CO; Kitching, John [Boulder, CO; Michalak, David J [Berkeley, CA; Xu, Shoujun [Houston, TX; Pines, Alexander [Berkeley, CA

2011-08-09

An integral microfluidic device includes an alkali vapor cell and microfluidic channel, which can be used to detect magnetism for nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI). Small magnetic fields in the vicinity of the vapor cell can be measured by optically polarizing and probing the spin precession in the small magnetic field. This can then be used to detect the magnetic field of in encoded analyte in the adjacent microfluidic channel. The magnetism in the microfluidic channel can be modulated by applying an appropriate series of radio or audio frequency pulses upstream from the microfluidic chip (the remote detection modality) to yield a sensitive means of detecting NMR and MRI.

Nuclear spin polarization of targets

International Nuclear Information System (INIS)

Happer, W.

1990-01-01

Lasers can be used to produce milligrams to grams of noble gas nuclei with spin polarizations in excess of 50%. These quantities are sufficient to be very useful targets in nuclear physics experiments. Alkali-metal atoms are used to capture the angular momentum of circularly polarized laser photons, and the alkali-metal atoms transfer their angular momentum to noble gas atoms in binary or three-body collisions. Non-radiative collisions between the excited alkali atoms and molecular quenching gases are essential to avoid radiation trapping. The spin exchange can involve gas-phase van der Waals molecules, consisting of a noble gas atom and an alkali metal atom. Surface chemistry is also of great importance in determining the wall-induced relaxation rates of the noble gases

Novel nuclear magnetic resonance techniques for studying biological molecules

International Nuclear Information System (INIS)

Laws, David D.

2000-01-01

Over the fifty-five year history of Nuclear Magnetic Resonance (NMR), considerable progress has been made in the development of techniques for studying the structure, function, and dynamics of biological molecules. The majority of this research has involved the development of multi-dimensional NMR experiments for studying molecules in solution, although in recent years a number of groups have begun to explore NMR methods for studying biological systems in the solid-state. Despite this new effort, a need still exists for the development of techniques that improve sensitivity, maximize information, and take advantage of all the NMR interactions available in biological molecules. In this dissertation, a variety of novel NMR techniques for studying biomolecules are discussed. A method for determining backbone (φ/ψ) dihedral angles by comparing experimentally determined 13 C a , chemical-shift anisotropies with theoretical calculations is presented, along with a brief description of the theory behind chemical-shift computation in proteins and peptides. The utility of the Spin-Polarization Induced Nuclear Overhauser Effect (SPINOE) to selectively enhance NMR signals in solution is examined in a variety of systems, as are methods for extracting structural information from cross-relaxation rates that can be measured in SPINOE experiments. Techniques for the production of supercritical and liquid laser-polarized xenon are discussed, as well as the prospects for using optically pumped xenon as a polarizing solvent. In addition, a detailed study of the structure of PrP 89-143 is presented. PrP 89-143 is a 54 residue fragment of the prion proteins which, upon mutation and aggregation, can induce prion diseases in transgenic mice. Whereas the structure of the wild-type PrP 89-143 is a generally unstructured mixture of α-helical and β-sheet conformers in the solid state, the aggregates formed from the PrP 89-143 mutants appear to be mostly β-sheet.

Laser-driven nuclear-polarized hydrogen internal gas target

International Nuclear Information System (INIS)

Seely, J.; Crawford, C.; Clasie, B.; Xu, W.; Dutta, D.; Gao, H.

2006-01-01

We report the performance of a laser-driven polarized internal hydrogen gas target (LDT) in a configuration similar to that used in scattering experiments. This target used the technique of spin-exchange optical pumping to produce nuclear spin polarized hydrogen gas that was fed into a cylindrical storage (target) cell. We present in this paper the performance of the target, methods that were tried to improve the figure-of-merit (FOM) of the target, and a Monte Carlo simulation of spin-exchange optical pumping. The dimensions of the apparatus were optimized using the simulation and the experimental results were in good agreement with the results from the simulation. The best experimental result achieved was at a hydrogen flow rate of 1.1x10 18 atoms/s, where the sample beam exiting the storage cell had 58.2% degree of dissociation and 50.5% polarization. Based on this measurement, the atomic fraction in the storage cell was 49.6% and the density averaged nuclear polarization was 25.0%. This represents the highest FOM for hydrogen from an LDT and is higher than the best FOM reported by atomic beam sources that used storage cells

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

Rheo-NMR: nuclear magnetic resonance and the rheology of complex fluids

International Nuclear Information System (INIS)

Callaghan, Paul T.

1999-01-01

The application of nuclear magnetic resonance methods to the study of complex fluids under shearing and extensional flows is reviewed. Both NMR velocimetry and spectroscopy approaches are discussed while specific systems studied include polymer melts, rigid rod and random coil polymers in solution, lyotropic and thermotropic liquid crystals and liquid crystalline polymers, and wormlike micelles. Reference is made to food systems. (author)

Theory of coherent dynamic nuclear polarization in quantum dots

DEFF Research Database (Denmark)

Neder, Izhar; Rudner, Mark Spencer; Halperin, Bertrand

2014-01-01

We consider the production of dynamic nuclear spin polarization (DNP) in a two-electron double quantum dot, in which the electronic levels are repeatedly swept through a singlet-triplet avoided crossing. Our analysis helps to elucidate the intriguing interplay between electron-nuclear hyperfine...

NMR magnetic field controller for pulsed nuclear magnetic resonance experiments

International Nuclear Information System (INIS)

Scheler, G.; Anacker, M.

1975-01-01

A nuclear magnetic resonance controller for magnetic fields, which can also be used for pulsed NMR investigations, is described. A longtime stability of 10 -7 is achieved. The control signal is generated by a modified time sharing circuit with resonance at the first side band of the 2 H signal. An exact calibration of the magnetic field is achieved by the variation of the H 1 - or of the time-sharing frequency. (author)

Nuclear spin polarized alkali beams (Li and Na): Production and acceleration

International Nuclear Information System (INIS)

Jaensch, H.; Becker, K.; Blatt, K.; Leucker, H.; Fick, D.

1987-01-01

Recent improvements of the Heidelberg source for polarized heavy ions (PSI) are described. By means of optical pumping in combination with the existing multipole separation magnet the beam figure of merit (polarization 2 x intensity) was doubled. 7 Li and 23 Na atomic beams can now be produced in pure hyperfine magnetic substates. Fast switching of the polarization is achieved by an adiabatic medium field transition. The hyperfine magnetic substate population is determined by laser-induced fluorescence spectroscopy. In routine operation atomic beams with nuclear polarization p α ≥0.85 (α=z, zz) are obtained. The acceleration of polarized 23 Na - ions by a 12 MV tandem accelerator introduces a new problem: the energy at the terminal stripper foil is not sufficient to produce a usable yield of naked ions. For partially stripped ions hyperfine interaction of the remaining electrons with the nuclear spin reduces the nuclear polarization. Using in addition the Heidelberg postaccelerator 23 Na 9+ beams of energies between 49 and 184 MeV were obtained with an alignment on target of P zz ≅0.45. 7 Li beams have also been accelerated up to 45 MeV with an alignment of P zz =0.69. (orig.)

Nuclear polarization study: new frontiers for tests of QED in heavy highly charged ions.

Science.gov (United States)

Volotka, Andrey V; Plunien, Günter

2014-07-11

A systematic investigation of the nuclear polarization effects in one- and few-electron heavy ions is presented. The nuclear polarization corrections in the zeroth and first orders in 1/Z are evaluated to the binding energies, the hyperfine splitting, and the bound-electron g factor. It is shown that the nuclear polarization contributions can be substantially canceled simultaneously with the rigid nuclear corrections. This allows for new prospects for probing the QED effects in a strong electromagnetic field and the determination of fundamental constants.

12. Nuclear magnetic resonance users meeting; 3. Iberoamerican NMR meeting. Extended abstracts book

Energy Technology Data Exchange (ETDEWEB)

NONE

2009-07-01

The NMR Users Meeting is held every year in Brazil and its twelfth edition took place from May 4 - 8, 2009 together with the third Iberoamerican NMR Meeting. The extended abstracts book comprise: five plenary lectures, six major conferences, three mini-conferences and summaries of results from one hundred and two research works. Among these research results which have been discussed, ninety three were presented as congress panels/posters and nine as oral communications. The major topics of the scientific and technological research works are thus distributed: 65% in chemical sciences (mainly structural elucidation and stereochemistry of organic compounds and dynamical studies of chemical reactions), 16% in applied life sciences (agricultural and food sciences, biological sciences and medicine), 11% in materials science (including petroleum and alternative fuels), and 8% regarding theoretical aspects related to nuclear magnetic resonance or improvements in NMR instrumental techniques.

Nuclear magnetic resonance (NMR) tomography

International Nuclear Information System (INIS)

Skalpe, I.O.

1984-01-01

A brief survey of the working principle of the NMR technique in diagnostical medicine is given. Its clinical usefulness for locating tumors, diagnosing various other diseases, such as some mental illnesses and multiple sclerosis, and its possibilities for studying biochemical processes in vivo are mentioned. The price of NMR image scanners and the problems of the strong magnetic field around the machines are mentioned

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.

MRI of Heterogeneous Hydrogenation Reactions Using Parahydrogen Polarization

Energy Technology Data Exchange (ETDEWEB)

Burt, Scott Russell [Univ. of California, Berkeley, CA (United States)

2008-01-01

The power of magnetic resonance imaging (MRI) is its ability to image the internal structure of optically opaque samples and provide detailed maps of a variety of important parameters, such as density, diffusion, velocity and temperature. However, one of the fundamental limitations of this technique is its inherent low sensitivity. For example, the low signal to noise ratio (SNR) is particularly problematic for imaging gases in porous materials due to the low density of the gas and the large volume occluded by the porous material. This is unfortunate, as many industrially relevant chemical reactions take place at gas-surface interfaces in porous media, such as packed catalyst beds. Because of this severe SNR problem, many techniques have been developed to directly increase the signal strength. These techniques work by manipulating the nuclear spin populations to produce polarized} (i.e., non-equilibrium) states with resulting signal strengths that are orders of magnitude larger than those available at thermal equilibrium. This dissertation is concerned with an extension of a polarization technique based on the properties of parahydrogen. Specifically, I report on the novel use of heterogeneous catalysis to produce parahydrogen induced polarization and applications of this new technique to gas phase MRI and the characterization of micro-reactors. First, I provide an overview of nuclear magnetic resonance (NMR) and how parahydrogen is used to improve the SNR of the NMR signal. I then present experimental results demonstrating that it is possible to use heterogeneous catalysis to produce parahydrogen-induced polarization. These results are extended to imaging void spaces using a parahydrogen polarized gas. In the second half of this dissertation, I demonstrate the use of parahydrogen-polarized gas-phase MRI for characterizing catalytic microreactors. Specifically, I show how the improved SNR allows one to map parameters important for characterizing the heat and mass

DNP-enhanced solid-state NMR spectroscopy of active pharmaceutical ingredients.

Science.gov (United States)

Zhao, Li; Pinon, Arthur C; Emsley, Lyndon; Rossini, Aaron J

2017-11-28

Solid-state NMR spectroscopy has become a valuable tool for the characterization of both pure and formulated active pharmaceutical ingredients (APIs). However, NMR generally suffers from poor sensitivity that often restricts NMR experiments to nuclei with favorable properties, concentrated samples, and acquisition of one-dimensional (1D) NMR spectra. Here, we review how dynamic nuclear polarization (DNP) can be applied to routinely enhance the sensitivity of solid-state NMR experiments by one to two orders of magnitude for both pure and formulated APIs. Sample preparation protocols for relayed DNP experiments and experiments on directly doped APIs are detailed. Numerical spin diffusion models illustrate the dependence of relayed DNP enhancements on the relaxation properties and particle size of the solids and can be used for particle size determination when the other factors are known. We then describe the advanced solid-state NMR experiments that have been enabled by DNP and how they provide unique insight into the molecular and macroscopic structure of APIs. For example, with large sensitivity gains provided by DNP, natural isotopic abundance, 13 C- 13 C double-quantum single-quantum homonuclear correlation NMR spectra of pure APIs can be routinely acquired. DNP also enables solid-state NMR experiments with unreceptive quadrupolar nuclei such as 2 H, 14 N, and 35 Cl that are commonly found in APIs. Applications of DNP-enhanced solid-state NMR spectroscopy for the molecular level characterization of low API load formulations such as commercial tablets and amorphous solid dispersions are described. Future perspectives for DNP-enhanced solid-state NMR experiments on APIs are briefly discussed. Copyright © 2017 John Wiley & Sons, Ltd.

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

High-energy nuclear optics of polarized particles

CERN Document Server

Baryshevsky, Vladimir G

2012-01-01

The various phenomena caused by refraction and diffraction of polarized elementary particles in matter have opened up a new research area in the particle physics: nuclear optics of polarized particles. Effects similar to the well-known optical phenomena such as birefringence and Faraday effects, exist also in particle physics, though the particle wavelength is much less than the distance between atoms of matter. Current knowledge of the quasi-optical effects, which exist for all particles in any wavelength range (and energies from low to extremely high), will enable us to investigate different properties of interacting particles (nuclei) in a new aspect. This pioneering book will provide detailed accounts of quasi-optical phenomena in the particle polarization, and will interest physicists and professionals in experimental particle physics.

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

Dissolution Dynamic Nuclear Polarization capability study with fluid path

DEFF Research Database (Denmark)

Malinowski, Ronja Maja; Lipsø, Hans Kasper Wigh; Lerche, Mathilde Hauge

2016-01-01

Signal enhancement by hyperpolarization is a way of overcoming the low sensitivity in magnetic resonance; MRI in particular. One of the most well-known methods, dissolution Dynamic Nuclear Polarization, has been used clinically in cancer patients. One way of ensuring a low bioburden of the hyperp......Signal enhancement by hyperpolarization is a way of overcoming the low sensitivity in magnetic resonance; MRI in particular. One of the most well-known methods, dissolution Dynamic Nuclear Polarization, has been used clinically in cancer patients. One way of ensuring a low bioburden...... of the hyperpolarized product is by use of a closed fluid path that constitutes a barrier to contamination. The fluid path can be filled with the pharmaceuticals, i.e. imaging agent and solvents, in a clean room, and then stored or immediately used at the polarizer. In this study, we present a method of filling...

Development of a 3He nuclear spin flip system on an in-situ SEOP 3He spin filter and demonstration for a neutron reflectometer and magnetic imaging technique

International Nuclear Information System (INIS)

Hayashida, H; Kira, H; Miyata, N; Akutsu, K; Mizusawa, M; Parker, J D; Matsumoto, Y; Oku, T; Sakai, K; Hiroi, K; Shinohara, T; Takeda, M; Yamazaki, D; Oikawa, K; Harada, M; Ino, T; Imagawa, T; Ohkawara, M; Ohoyama, K; Kakurai, K

2016-01-01

We have been developing a 3 He neutron spin filter (NSF) using the spin exchange optical pumping (SEOP) technique. The 3 He NSF provides a high-energy polarized neutron beam with large beam size. Moreover the 3 He NSF can work as a π-flipper for a polarized neutron beam by flipping the 3 He nuclear spin using a nuclear magnetic resonance (NMR) technique. For NMR with the in-situ SEOP technique, the polarization of the laser must be reversed simultaneously because a non-reversed laser reduces the polarization of the spin-flipped 3 He. To change the polarity of the laser, a half-wavelength plate was installed. The rotation angle of the half-wavelength plate was optimized, and a polarization of 97% was obtained for the circularly polarized laser. The 3 He polarization reached 70% and was stable over one week. A demonstration of the 3 He nuclear spin flip system was performed at the polarized neutron reflectometer SHARAKU (BL17) and NOBORU (BL10) at J-PARC. Off-specular measurement from a magnetic Fe/Cr thin film and magnetic imaging of a magnetic steel sheet were performed at BL17 and BL10, respectively. (paper)

High-field EPR on membrane proteins - crossing the gap to NMR.

Science.gov (United States)

Möbius, Klaus; Lubitz, Wolfgang; Savitsky, Anton

2013-11-01

In this review on advanced EPR spectroscopy, which addresses both the EPR and NMR communities, considerable emphasis is put on delineating the complementarity of NMR and EPR concerning the measurement of molecular interactions in large biomolecules. From these interactions, detailed information can be revealed on structure and dynamics of macromolecules embedded in solution- or solid-state environments. New developments in pulsed microwave and sweepable cryomagnet technology as well as ultrafast electronics for signal data handling and processing have pushed to new horizons the limits of EPR spectroscopy and its multifrequency extensions concerning the sensitivity of detection, the selectivity with respect to interactions, and the resolution in frequency and time domains. One of the most important advances has been the extension of EPR to high magnetic fields and microwave frequencies, very much in analogy to what happens in NMR. This is exemplified by referring to ongoing efforts for signal enhancement in both NMR and EPR double-resonance techniques by exploiting dynamic nuclear or electron spin polarization via unpaired electron spins and their electron-nuclear or electron-electron interactions. Signal and resolution enhancements are particularly spectacular for double-resonance techniques such as ENDOR and PELDOR at high magnetic fields. They provide greatly improved orientational selection for disordered samples that approaches single-crystal resolution at canonical g-tensor orientations - even for molecules with small g-anisotropies. Exchange of experience between the EPR and NMR communities allows for handling polarization and resolution improvement strategies in an optimal manner. Consequently, a dramatic improvement of EPR detection sensitivity could be achieved, even for short-lived paramagnetic reaction intermediates. Unique structural and dynamic information is thus revealed that can hardly be obtained by any other analytical techniques. Micromolar

Electron and nuclear spin system polarization in semiconductors by light

Energy Technology Data Exchange (ETDEWEB)

Zakharchenya, B; Flejsher, V

1981-02-01

Discussed are the principles of optical electron spin orientation, dynamic polarization and cooling of nuclear spin systems in optical electron orientation, and behavioural characteristics of bound electron and nuclear spin systems of a semiconductor in the optical orientation situation.

Nuclear reactivity indices in the context of spin polarized density functional theory

International Nuclear Information System (INIS)

Cardenas, Carlos; Lamsabhi, Al Mokhtar; Fuentealba, Patricio

2006-01-01

In this work, the nuclear reactivity indices of density functional theory have been generalized to the spin polarized case and their relationship to electron spin polarized indices has been established. In particular, the spin polarized version of the nuclear Fukui function has been proposed and a finite difference approximation has been used to evaluate it. Applications to a series of triatomic molecules demonstrate the ability of the new functions to predict the geometrical changes due to a change in the spin multiplicity. The main equations in the different ensembles have also been presented

Deuterium NMR, induced and intrinsic cholesteric lyomesophases

International Nuclear Information System (INIS)

Alcantara, M.R.

1982-01-01

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

Electron and nuclear spin system polarization in semiconductors by light

International Nuclear Information System (INIS)

Zakharchenya, B.; Flejsher, V.

1981-01-01

Discussed are the principles of optical electron spin orientation, dynamic polarization and cooling of nuclear spin systems in optical electron orientation, and behavioural characteristics of bound electron and nuclear spin systems of a semiconductor in the optical orientation situation. (J.P.)

Theoretical and experimental NMR studies on muscimol from fly agaric mushroom (Amanita muscaria)

Science.gov (United States)

Kupka, Teobald; Wieczorek, Piotr P.

2016-01-01

In this article we report results of combined theoretical and experimental NMR studies on muscimol, the bioactive alkaloid from fly agaric mushroom (Amanita muscaria). The assignment of 1H and 13C NMR spectra of muscimol in DMSO-d6 was supported by additional two-dimensional heteronuclear correlated spectra (2D NMR) and gauge independent atomic orbital (GIAO) NMR calculations using density functional theory (DFT). The effect of solvent in theoretical calculations was included via polarized continuum model (PCM) and the hybrid three-parameter B3LYP density functional in combination with 6-311++G(3df,2pd) basis set enabled calculation of reliable structures of non-ionized (neutral) molecule and its NH and zwitterionic forms in the gas phase, chloroform, DMSO and water. GIAO NMR calculations, using equilibrium and rovibrationally averaged geometry, at B3LYP/6-31G* and B3LYP/aug-cc-pVTZ-J levels of theory provided muscimol nuclear magnetic shieldings. The theoretical proton and carbon chemical shifts were critically compared with experimental NMR spectra measured in DMSO. Our results provide useful information on its structure in solution. We believe that such data could improve the understanding of basic features of muscimol at atomistic level and provide another tool in studies related to GABA analogs.

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

International Nuclear Information System (INIS)

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

2016-01-01

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

The Spin Structure of the Neutron Determined Using a Polarized He-3 Target

Energy Technology Data Exchange (ETDEWEB)

Middleton, H

2004-01-06

Described is a study of the internal spin structure of the neutron performed by measuring the asymmetry in spin-dependent deep inelastic scattering of polarized electrons from nuclear polarized {sup 3}He. Stanford Linear Accelerator experiment E142's sample of 400 million scattering events collected at beam energies between 19 and 26 GeV led to the most precise measurement of a nucleon spin structure function to date. The {sup 3}He target represents a major advance in polarized target technology, using the technique of spin exchange with optically pumped rubidium vapor to produce a typical {sup 3}He nuclear polarization of 34% in a 30cm long target cell with a gas density of 2.3 x 10{sup 20} cm{sup -3}. The target polarization was measured to {+-}7% using an Adiabatic Fast Passage NMR system calibrated with the thermal equilibrium polarization of the protons in a sample of water. The relatively high polarization and target thickness were the result of the development of large volume glass target cells which had inherent nuclear spin relaxation times for the {sup 3}He gas of as long as 70 hours. A target cell production procedure is presented which focuses on special glass blowing techniques to minimize surface interactions with the {sup 3}He nuclei and careful gas purification and vacuum system procedures to reduce relaxation inducing impurities.

The role of level anti-crossings in nuclear spin hyperpolarization

NARCIS (Netherlands)

Ivanov, Konstantin L.; Pravdivtsev, Andrey N.; Yurkovskaya, Alexandra V.; Vieth, Hans Martin; Kaptein, R

2014-01-01

Nuclear spin hyperpolarization is an important resource for increasing the sensitivity of NMR spectroscopy and MRI. Signal enhancements can be as large as 3-4 orders of magnitude. In hyperpolarization experiments, it is often desirable to transfer the initial polarization to other nuclei of choice,

Novel nuclear magnetic resonance techniques for studying biological molecules

Energy Technology Data Exchange (ETDEWEB)

Laws, David Douglas [Univ. of California, Berkeley, CA (United States)

2000-06-01

Over the fifty-five year history of Nuclear Magnetic Resonance (NMR), considerable progress has been made in the development of techniques for studying the structure, function, and dynamics of biological molecules. The majority of this research has involved the development of multi-dimensional NMR experiments for studying molecules in solution, although in recent years a number of groups have begun to explore NMR methods for studying biological systems in the solid-state. Despite this new effort, a need still exists for the development of techniques that improve sensitivity, maximize information, and take advantage of all the NMR interactions available in biological molecules. In this dissertation, a variety of novel NMR techniques for studying biomolecules are discussed. A method for determining backbone (Φ/Ψ) dihedral angles by comparing experimentally determined ¹³C_a, chemical-shift anisotropies with theoretical calculations is presented, along with a brief description of the theory behind chemical-shift computation in proteins and peptides. The utility of the Spin-Polarization Induced Nuclear Overhauser Effect (SPINOE) to selectively enhance NMR signals in solution is examined in a variety of systems, as are methods for extracting structural information from cross-relaxation rates that can be measured in SPINOE experiments. Techniques for the production of supercritical and liquid laser-polarized xenon are discussed, as well as the prospects for using optically pumped xenon as a polarizing solvent. In addition, a detailed study of the structure of PrP 89-143 is presented. PrP 89-143 is a 54 residue fragment of the prion proteins which, upon mutation and aggregation, can induce prion diseases in transgenic mice. Whereas the structure of the wild-type PrP 89-143 is a generally unstructured mixture of α-helical and β-sheet conformers in the solid state, the aggregates formed from the PrP 89-143 mutants appear to be mostly β-sheet.

Structural investigation of molten fluorides of nuclear interest by NMR and XAFS spectroscopies

International Nuclear Information System (INIS)

Pauvert, Olivier

2009-01-01

In the frame of the renewal of the different nuclear plans, the molten salt reactor is one of the six concepts of reactors of 4. generation. This reactor has the particularity to use a liquid fuel based on LiF-ThF 4 mixtures. In order to develop and to optimize this concept, it is important to characterize the structure of the melt and to describe its physical and chemical properties. Our work has been based on the study of the system MF-ZrF 4 (M = Li, Na, K) selected as a model of ThF 4 based systems. We have combined two spectroscopic techniques, the Nuclear Magnetic Resonance and the X-ray Absorption at high temperature, with molecular dynamics calculations. We particularly focused on the local environments of the fluorine and the zirconium. In order to interpret the NMR data obtain in the molten state, we performed a preliminary study on zirconium halides and rare earth and alkali fluoro zirconates using the 91 Zr solid-state NMR at very high magnetic fields. New correlations between structural parameters and NMR data have been established. At high temperature, in MF-ZrF 4 melts we have shown the coexistence of three different kind of Zr-based complexes with different proportions depending on the amount of ZrF 4 and on the nature of the alkali. Depending on the ZrF 4 content, three kinds of fluorine have been characterized: form free fluorines at low amount of zirconium fluorides, fluorines involved in Zr-based complexes and bridging fluorines at higher ZrF 4 content. This original and innovative approach of molten fluorides mixtures, combining NMR and EXAFS at high temperature with molecular dynamics calculations, is very efficient to describe their speciation and thus their fluoro-acidity. (author)

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.

Effects of Quantum Nuclear Delocalisation on NMR Parameters from Path Integral Molecular Dynamics

Czech Academy of Sciences Publication Activity Database

Dračínský, Martin; Hodgkinson, P.

2014-01-01

Roč. 20, č. 8 (2014), s. 2201-2207 ISSN 0947-6539 Grant - others:Seventh Framework Programme of the European Union(XE) FP7-299242 People Institutional support: RVO:61388963 Keywords : density functional calculations * isotope effects * NMR spectroscopy * nuclear delocalisation * path integral molecular dynamics Subject RIV: CC - Organic Chemistry Impact factor: 5.731, year: 2014

High-efficiency optical pumping of nuclear polarization in a GaAs quantum well

Science.gov (United States)

Mocek, R. W.; Korenev, V. L.; Bayer, M.; Kotur, M.; Dzhioev, R. I.; Tolmachev, D. O.; Cascio, G.; Kavokin, K. V.; Suter, D.

2017-11-01

The dynamic polarization of nuclear spins by photoexcited electrons is studied in a high quality GaAs/AlGaAs quantum well. We find a surprisingly high efficiency of the spin transfer from the electrons to the nuclei as reflected by a maximum nuclear field of 0.9 T in a tilted external magnetic field of 1 T strength only. This high efficiency is due to a low leakage of spin out of the polarized nuclear system, because mechanisms of spin relaxation other than the hyperfine interaction are strongly suppressed, leading to a long nuclear relaxation time of up to 1000 s. A key ingredient to that end is the low impurity concentration inside the heterostructure, while the electrostatic potential from charged impurities in the surrounding barriers becomes screened through illumination by which the spin relaxation time is increased compared to keeping the system in the dark. This finding indicates a strategy for obtaining high nuclear spin polarization as required for long-lasting carrier spin coherence.

Determination of structural topology of a membrane protein in lipid bilayers using polarization optimized experiments (POE) for static and MAS solid state NMR spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Mote, Kaustubh R. [University of Minnesota, Department of Chemistry (United States); Gopinath, T. [University of Minnesota, Department of Biochemistry, Molecular Biology and Biophysics (United States); Veglia, Gianluigi, E-mail: vegli001@umn.edu [University of Minnesota, Department of Chemistry (United States)

2013-10-15

The low sensitivity inherent to both the static and magic angle spinning techniques of solid-state NMR (ssNMR) spectroscopy has thus far limited the routine application of multidimensional experiments to determine the structure of membrane proteins in lipid bilayers. Here, we demonstrate the advantage of using a recently developed class of experiments, polarization optimized experiments, for both static and MAS spectroscopy to achieve higher sensitivity and substantial time-savings for 2D and 3D experiments. We used sarcolipin, a single pass membrane protein, reconstituted in oriented bicelles (for oriented ssNMR) and multilamellar vesicles (for MAS ssNMR) as a benchmark. The restraints derived by these experiments are then combined into a hybrid energy function to allow simultaneous determination of structure and topology. The resulting structural ensemble converged to a helical conformation with a backbone RMSD {approx}0.44 A, a tilt angle of 24 Degree-Sign {+-} 1 Degree-Sign , and an azimuthal angle of 55 Degree-Sign {+-} 6 Degree-Sign . This work represents a crucial first step toward obtaining high-resolution structures of large membrane proteins using combined multidimensional oriented solid-state NMR and magic angle spinning solid-state NMR.

Methods of contrast variation by nuclear polarisation in small-angle neutron scattering: Observation of domains of nuclear polarisation by neutron scattering

International Nuclear Information System (INIS)

Leymarie, E.

2002-11-01

In this thesis we study the theoretical and experimental aspects of Contrast Variation by Nuclear Polarization (CVNP) applied to small-angle neutron scattering. The basics of neutron scattering theory is developed by highlighting the origin of the CVNP method: the strong spin dependence of thermal neutron scattering, especially on protons. We also present the principles of NMR with a special attention on the method of dynamic nuclear polarization by the solid effect which makes it possible to control the proton polarization and therefore the contrast for neutron scattering. We present a theoretical study of the CVNP method called static which supposes that the nuclear polarization is homogeneous in the sample and constant during the experiment. We show that it allows one to obtain partial structure functions of systems with multiple components, by carrying out several acquisitions with different polarizations on a single sample. For this purpose, we tested a simple device to stabilize the nuclear polarization. We describe finally a new application of the CVNP method called dynamic. In a solution of deuterated glycerol-water containing a small concentration of paramagnetic centres, we showed the existence of domains of polarized protons at the onset of dynamic polarization. This reinforces considerably the coherent scattering of paramagnetic centres. We describe the theoretical reasons explaining the appearance of these domains of polarization, as well as the various techniques used to observe them by neutron scattering. (author)

From single-site tantalum complexes to nanoparticles of Ta x N y and TaO x N y supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy.

Science.gov (United States)

Mohandas, Janet C; Abou-Hamad, Edy; Callens, Emmanuel; Samantaray, Manoja K; Gajan, David; Gurinov, Andrei; Ma, Tao; Ould-Chikh, Samy; Hoffman, Adam S; Gates, Bruce C; Basset, Jean-Marie

2017-08-01

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of Ta x N y and TaO x N y with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe 5 (Me = methyl) and dimeric Ta 2 (OMe) 10 with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of 1 H, 13 C, 29 Si, and 15 N at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O 2 insertion into Ta-CH 3 species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta 2 (OMe) 10 on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H 2 O 2 serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as Ta x N y /TaO x N y .

Phosphorus-31 NMR (nuclear magnetic resonance) analysis of gold plating baths

Energy Technology Data Exchange (ETDEWEB)

Smith, R.E.

1990-01-01

This report describes the nuclear magnetic resonance (NMR) analysis of the gold plating baths in the Micro-Miniature Electronic Assembly department of Allied-Signal Inc., Kansas City Division (KCD). The baths were analyzed for phosphorylated components. In freshly prepared gold plating baths, a 50-percent aqueous solution of aminotrimethylphosphonate (ATMP) is the principal compound observed. As the bath is used in production, the ATMP breaks down and new materials (phosphate, ADMP, and AMMP) are identified. The NMR method was used to monitor the concentrations of the ATMP and breakdown products for a nine-month period. The 225-liter bath had plated approximately 100 square feet of gold during the nine-month period. These results can be used to predict the performance of baths as they are used in production. The accuracy of the analysis is 96 percent for ATMP and 92 percent for phosphate. The precision (relative standard deviation) is 5.2 percent for ATMP and 4.5 percent for phosphate. 1 ref., 5 figs., 2 tabs.

Laser-polarized xenon-129 magnetic resonance spectroscopy and imaging. The development of a method for in vivo perfusion measurement

Science.gov (United States)

Rosen, Matthew Scot

2001-07-01

This thesis presents in vivo nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) studies with laser-polarized 129Xe delivered to living rats by inhalation and transported to tissue via blood flow. The results presented herein include the observation, assignment, and dynamic measurement of 129Xe resonances in the brain and body, the first one- and two-dimensional chemical-shift-resolved images of 129Xe in blood, tissue, and gas in the thorax, and the first images of 129Xe in brain tissue. These results establish that laser-polarized 129Xe can be used as a magnetic resonance tracer in vivo. NMR resonances at 0, 191, 198, and 209 ppm relative to the 129 Xe gas resonance are observed in the rat thorax and assigned to 129Xe in gas, fat, tissue, and blood respectively. Resonances at 189, 192, 195, 198, and 209 ppm are observed in the brain, and the 195 and 209 ppm resonances are assigned to 129Xe in grey matter, and blood, respectively. The design and construction of a laser-polarized 129Xe production and delivery system is described. This system produces liter-volumes of laser- polarized 129Xe by spin-exchange optical- pumping. It represented an order of magnitude increase over previously reported production volumes of polarized 129Xe. At approximately 3-7% polarization, 157 cc-atm of xenon is produced and stored as ice every 5 minutes. This reliable, effective, and simple production method for large volumes of 129Xe can be applied to other areas of research involving the use of laser-polarized noble gases. A model of the in vivo transport of laser polarized 129Xe to tissue under realistic experimental NMR conditions is described. Appropriate control of the NMR parameters is shown to allow tissue perfasion and 129Xe tissue T1 to be extracted from measurement of the steady-state 129Xe tissue signal. In vivo rodent 129Xe NMR results are used to estimate the signal-to-noise ratio of this technique, and an inhaled 30% xenon/70% O2 mixture polarized to 5

Nuclear polarization contribution to the Lamb-shift in heavy atoms

International Nuclear Information System (INIS)

Plunien, G.; Mueller, B.; Greiner, W.

1988-08-01

The energy shift of the 1s 1/2 -state in 238 92 U due to virtual excitation of nuclear rotational modes is shown to be considerable correction for atomic high precision experiments. In contrast to this nuclear polarization effects are of minor importance for Lamb-shift studies in 208 82 Pb. (orig.)

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...

Non-destructive ripeness sensing by using proton NMR [Nuclear Magnetic Resonance

International Nuclear Information System (INIS)

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

1990-01-01

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

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

Science.gov (United States)

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

1990-01-01

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

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)

A compact spin-exchange optical pumping system for 3He polarization based on a solenoid coil, a VBG laser diode, and a cosine theta RF coil

Science.gov (United States)

Lee, Sungman; Kim, Jongyul; Moon, Myung Kook; Lee, Kye Hong; Lee, Seung Wook; Ino, Takashi; Skoy, Vadim R.; Lee, Manwoo; Kim, Guinyun

2013-02-01

For use as a neutron spin polarizer or analyzer in the neutron beam lines of the HANARO (High-flux Advanced Neutron Application ReactOr) nuclear research reactor, a 3He polarizer was designed based on both a compact solenoid coil and a VBG (volume Bragg grating) diode laser with a narrow spectral linewidth of 25 GHz. The nuclear magnetic resonance (NMR) signal was measured and analyzed using both a built-in cosine radio-frequency (RF) coil and a pick-up coil. Using a neutron transmission measurement, we estimated the polarization ratio of the 3He cell as 18% for an optical pumping time of 8 hours.

Anomalous neutron scattering in nuclear-polarized media

International Nuclear Information System (INIS)

Bashkin, E.P.

1989-01-01

A novel inelastic scattering exchange mechanism involving spin flip is considered for slow neutrons moving through a nuclear-polarized medium. The scattering is accompanied by the emission or absorption of thermal fluctuations of the transverse magnetization of the medium. The main role in the fluctuations is played by weakly decaying Larmor precession of the nuclear spins in an external magnetic field. Under 'giant opalescence' conditions the effect is enormous and the respective cross sections exceed significantly those for ordinary elastic scattering. Thus, for 29 Si and 3 He in typical experimental conditions the cross sections for the inelastic processes are of the order of 10 5 -10 6 barn

Liquid-Liquid Phase Separation in Model Nuclear Waste Glasses: A Solid-State Double-Resonance NMR Study

Energy Technology Data Exchange (ETDEWEB)

Martineau, Ch.; Michaelis, V.K.; Kroeker, S. [Univ Manitoba, Dept Chem, Winnipeg, MB R3T 2N2 (Canada); Schuller, S. [CEA Valrho Marcoule, LDMC, SECM, DTCD, DEN, F-30207 Bagnols Sur Ceze (France)

2010-07-01

Double-resonance nuclear magnetic resonance (NMR) techniques are used in addition to single-resonance NMR experiments to probe the degree of mixing between network-forming cations Si and B, along with the modifier cations Cs{sup +} and Na{sup +} in two molybdenum-bearing model nuclear waste glasses. The double-resonance experiments involving {sup 29}Si in natural abundance are made possible by the implementation of a CPMG pulse-train during the acquisition period of the usual REDOR experiments. For the glass with lower Mo content, the NMR results show a high degree of Si-B mixing, as well as an homogeneous distribution of the cations within the borosilicate network, characteristic of a non-phase-separated glass. For the higher-Mo glass, a decrease of B-Si(Q{sup 4}) mixing is observed, indicating phase separation. {sup 23}Na and {sup 133}Cs NMR results show that although the Cs{sup +} cations, which do not seem to be influenced by the molybdenum content, are spread within the borate network, there is a clustering of the Na{sup +} cations, very likely around the molybdate units. The segregation of a Mo-rich region with Na{sup +} cations appears to shift the bulk borosilicate glass composition toward the metastable liquid liquid immiscibility region and induce additional phase separation. Although no crystallization is observed in the present case, this liquid liquid phase separation is likely to be the first stage of crystallization that can occur at higher Mo loadings or be driven by heat treatment. From this study emerges a consistent picture of the nature and extent of such phase separation phenomena in Mo-bearing glasses, and demonstrates the potential of double-resonance NMR methods for the investigation of phase separation in amorphous materials. (authors)

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Hydrogen and deuterium NMR of solids by magic-angle spinning

International Nuclear Information System (INIS)

Eckman, R.R.

1982-10-01

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

Two-dimensional NMR spectrometry

International Nuclear Information System (INIS)

Farrar, T.C.

1987-01-01

This article is the second in a two-part series. In part one (ANALYTICAL CHEMISTRY, May 15) the authors discussed one-dimensional nuclear magnetic resonance (NMR) spectra and some relatively advanced nuclear spin gymnastics experiments that provide a capability for selective sensitivity enhancements. In this article and overview and some applications of two-dimensional NMR experiments are presented. These powerful experiments are important complements to the one-dimensional experiments. As in the more sophisticated one-dimensional experiments, the two-dimensional experiments involve three distinct time periods: a preparation period, t 0 ; an evolution period, t 1 ; and a detection period, t 2

Push-through Direction Injectin NMR Automation

Science.gov (United States)

Nuclear magnetic resonance (NMR) and mass spectrometry (MS) are the two major spectroscopic techniques successfully used in metabolomics studies. The non-invasive, quantitative and reproducible characteristics make NMR spectroscopy an excellent technique for detection of endogeno...

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)

Preparation of a novel bioavailable curcuminoid formulation (Cureit™) using Polar-Nonpolar-Sandwich (PNS) technology and its characterization and applications

Energy Technology Data Exchange (ETDEWEB)

Amalraj, Augustine; Jude, Shintu; Varma, Karthik; Jacob, Joby [R& D Centre, Aurea Biolabs (P) Ltd, Kolenchery, Cochin, 682 311, Kerala (India); Gopi, Sreeraj, E-mail: sreeraj.gopi@plantlipids.com [R& D Centre, Aurea Biolabs (P) Ltd, Kolenchery, Cochin, 682 311, Kerala (India); Oluwafemi, Oluwatobi S. [Department of Applied Chemistry, University of Johannesburg, Doornfontein Campus, P.O. Box 17011, Doornfontein, 2028 Johannesburg (South Africa); Centre for Nanomaterials Science Research, University of Johannesburg, Johannesburg (South Africa); Thomas, Sabu [School of Chemical Sciences, Mahatma Gandhi University, Kottayam (India)

2017-06-01

Health benefits of curcuminoid are highly limited due to their poor aqueous solubility, very low systemic bioavailability, fast metabolic alterations and rapid elimination. In this study, a novel bioavailable curcuminoid formulation Cureit™ was prepared by using Polar-Nonpolar-Sandwich (PNS) technology with complete natural turmeric matrix (CNTM). The synthesized bioavailable curcuminoid formulation Cureit™ was characterizations by Nuclear magnetic resonance spectroscopy (NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infra-red (IR), current-voltage (I-V) study, Quadrupole Time-of-Flight Mass Spectrometry (Q-TOF), differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). NMR study showed the presence of hydrogen bonding interactions with curcuminoids, polar and non-polar compounds in the PNS technology. SEM images indicated that Cureit™ was almost spherical and well dispersed with rough morphology, and separated with three layers of PNS formulation. The chemical profile of Cureit™ was analyzed by Q-TOF confirmed the presence of curcuminoids (curcumin, demethoxycurcumin and bismethoxycurcumin), lactones, sesquiterpenes and their derivatives derived from polar layer, aromatic turmerone, dihydroturmerone, turmeronol, curdione and bisacurone derived from non-polar layer. IR, XRD, DSC and TGA also confirmed the presence of curcuminoids with high stability in the PNS formulation. Various biological activities of Cureit™ were also discussed. - Highlights: • A novel bioavailable curcuminoid formulation Cureit™ was prepared. • Polar-Nonpolar-Sandwich technology is used with complete natural turmeric matrix. • Cureit™ was analyzed and predicted by NMR, SEM, XRD, IR, I-V, Q-TOF, DSC and TGA. • Cureit™ exhibited 10 fold higher bioavailable curcuminoid than pure curcuminoid.

Preparation of a novel bioavailable curcuminoid formulation (Cureit™) using Polar-Nonpolar-Sandwich (PNS) technology and its characterization and applications

International Nuclear Information System (INIS)

Amalraj, Augustine; Jude, Shintu; Varma, Karthik; Jacob, Joby; Gopi, Sreeraj; Oluwafemi, Oluwatobi S.; Thomas, Sabu

2017-01-01

Health benefits of curcuminoid are highly limited due to their poor aqueous solubility, very low systemic bioavailability, fast metabolic alterations and rapid elimination. In this study, a novel bioavailable curcuminoid formulation Cureit™ was prepared by using Polar-Nonpolar-Sandwich (PNS) technology with complete natural turmeric matrix (CNTM). The synthesized bioavailable curcuminoid formulation Cureit™ was characterizations by Nuclear magnetic resonance spectroscopy (NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infra-red (IR), current-voltage (I-V) study, Quadrupole Time-of-Flight Mass Spectrometry (Q-TOF), differential scanning calorimeter (DSC) and thermogravimetric analysis (TGA). NMR study showed the presence of hydrogen bonding interactions with curcuminoids, polar and non-polar compounds in the PNS technology. SEM images indicated that Cureit™ was almost spherical and well dispersed with rough morphology, and separated with three layers of PNS formulation. The chemical profile of Cureit™ was analyzed by Q-TOF confirmed the presence of curcuminoids (curcumin, demethoxycurcumin and bismethoxycurcumin), lactones, sesquiterpenes and their derivatives derived from polar layer, aromatic turmerone, dihydroturmerone, turmeronol, curdione and bisacurone derived from non-polar layer. IR, XRD, DSC and TGA also confirmed the presence of curcuminoids with high stability in the PNS formulation. Various biological activities of Cureit™ were also discussed. - Highlights: • A novel bioavailable curcuminoid formulation Cureit™ was prepared. • Polar-Nonpolar-Sandwich technology is used with complete natural turmeric matrix. • Cureit™ was analyzed and predicted by NMR, SEM, XRD, IR, I-V, Q-TOF, DSC and TGA. • Cureit™ exhibited 10 fold higher bioavailable curcuminoid than pure curcuminoid.

Voltage switching technique for detecting nuclear spin polarization in a quantum dot

International Nuclear Information System (INIS)

Takahashi, Ryo; Kono, Kimitoshi; Tarucha, Seigo; Ono, Keiji

2010-01-01

We have introduced a source-drain voltage switching technique for studying nuclear spins in a vertical double quantum dot. Switching the source-drain voltage between the spin-blockade state and the zero-bias Coulomb blockade state can tune the energy difference between the spin singlet and triplet, and effectively turn on/off the hyperfine interaction. Since the change in the nuclear spin state affects the source-drain current, nuclear spin properties can only be detected by transport measurement. Using this technique, we have succeeded in measuring the timescale of nuclear spin depolarization. Furthermore, combining this technique and an RF ac magnetic field, we successfully detected continuous-wave NMR signals of 75 As, 69 Ga, and 71 Ga, which are contained in a quantum dot. (author)

Real-Time DNP NMR Observations of Acetic Acid Uptake, Intracellular Acidification, and of Consequences for Glycolysis and Alcoholic Fermentation in Yeast

DEFF Research Database (Denmark)

Jensen, Pernille Rose; Karlsson, Magnus; Lerche, Mathilde Hauge

2013-01-01

Uptake and upshot in vivo: Straightforward methods that permit the real-time observation of organic acid influx, intracellular acidification, and concomitant effects on cellular-reaction networks are crucial for improved bioprocess monitoring and control (see scheme). Herein, dynamic nuclear pola...... polarization (DNP) NMR is used to observe acetate influx, ensuing intracellular acidification and the metabolic consequences on alcoholic fermentation and glycolysis in living cells....

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...

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.

Measuring the spin polarization of alkali-metal atoms using nuclear magnetic resonance frequency shifts of noble gases

Directory of Open Access Journals (Sweden)

X. H. Liu

2015-10-01

Full Text Available We report a novel method of measuring the spin polarization of alkali-metal atoms by detecting the NMR frequency shifts of noble gases. We calculated the profile of 87Rb D1 line absorption cross sections. We then measured the absorption profile of the sample cell, from which we calculated the 87Rb number densities at different temperatures. Then we measured the frequency shifts resulted from the spin polarization of the 87Rb atoms and calculated its polarization degrees at different temperatures. The behavior of frequency shifts versus temperature in experiment was consistent with theoretical calculation, which may be used as compensative signal for the NMRG closed-loop control system.

NMR techniques in the study of cardiovascular structure and functions

International Nuclear Information System (INIS)

Osbakken, M.; Haselgrove, J.

1987-01-01

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

A novel method to assay special nuclear materials by measuring prompt neutrons from polarized photofission

Energy Technology Data Exchange (ETDEWEB)

Mueller, J.M., E-mail: mueller@tunl.duke.edu [Triangle Universities Nuclear Laboratory, Durham, NC 27710 (United States); Department of Physics, Duke University, Durham, NC 27708 (United States); Ahmed, M.W. [Triangle Universities Nuclear Laboratory, Durham, NC 27710 (United States); Department of Physics, Duke University, Durham, NC 27708 (United States); Department of Mathematics and Physics, North Carolina Central University, Durham, NC 27707 (United States); Weller, H.R. [Triangle Universities Nuclear Laboratory, Durham, NC 27710 (United States); Department of Physics, Duke University, Durham, NC 27708 (United States)

2014-08-01

A novel method of measuring the enrichment of special nuclear material is presented. Recent photofission measurements using a linearly polarized γ-ray beam were performed on samples of {sup 232}Th, {sup 233,235,238}U, {sup 237}Np, and {sup 239,240}Pu. Prompt neutron polarization asymmetries, defined to be the difference in the prompt neutron yields parallel and perpendicular to the plane of beam polarization divided by their sum, were measured. It was discovered that the prompt neutron polarization asymmetries differed significantly depending on the sample. Prompt neutrons from photofission of even–even (non-fissile) targets had significant polarization asymmetries (∼0.2 to 0.5), while those from odd-A (generally fissile) targets had polarization asymmetries close to zero. This difference in the polarization asymmetries could be exploited to measure the fissile versus non-fissile content of special nuclear materials, and potentially to detect the presence of fissile material during active interrogation. The proposed technique, its expected performance, and its potential applicability are discussed.

A novel method to assay special nuclear materials by measuring prompt neutrons from polarized photofission

International Nuclear Information System (INIS)

Mueller, J.M.; Ahmed, M.W.; Weller, H.R.

2014-01-01

A novel method of measuring the enrichment of special nuclear material is presented. Recent photofission measurements using a linearly polarized γ-ray beam were performed on samples of 232 Th, 233,235,238 U, 237 Np, and 239,240 Pu. Prompt neutron polarization asymmetries, defined to be the difference in the prompt neutron yields parallel and perpendicular to the plane of beam polarization divided by their sum, were measured. It was discovered that the prompt neutron polarization asymmetries differed significantly depending on the sample. Prompt neutrons from photofission of even–even (non-fissile) targets had significant polarization asymmetries (∼0.2 to 0.5), while those from odd-A (generally fissile) targets had polarization asymmetries close to zero. This difference in the polarization asymmetries could be exploited to measure the fissile versus non-fissile content of special nuclear materials, and potentially to detect the presence of fissile material during active interrogation. The proposed technique, its expected performance, and its potential applicability are discussed

NMR - from basic physics to images of the human body

International Nuclear Information System (INIS)

Richards, Rex.

1985-01-01

Nuclear magnetic resonance (NMR) is a remarkable phenomenon which involves the exchange of very weak radio frequency radiation between atomic nuclei and a sensitive detecting apparatus. It was originally regarded as a rather esoteric effect of great theoretical interest, but has since proved to have an amazing range of applications over many scientific disciplines, including nuclear physics, solid state physics, all branches of chemistry, biochemistry, physiology and most recently in medical diagnosis. In this Discourse the principles of NMR and trace briefly the history of its applications are examined and illustrated. Headings are: early history; nuclear resonance; relaxation time; the chemical shift; spin-spin coupling (NMR spectra); chemical shifts in biological tissue; NMR imaging; conclusions. (author)

Studies of nuclear structure via polarization transfer experiments

International Nuclear Information System (INIS)

Moss, J.M.

1985-01-01

Inelastic scattering and charge exchange reactions at medium energies are discussed. Theoretical treatments of these phenomena based on the Dirac equation are presented. A LAMPF experiment in which polarization observables were employed in the search for collective effects in the nuclear pion field is discussed. This experiment is compared with the EMC (European Muon Collaboration) effect. 37 refs., 11 figs

Inhomogeneous nuclear spin polarization induced by helicity-modulated optical excitation of fluorine-bound electron spins in ZnSe

Science.gov (United States)

Heisterkamp, F.; Greilich, A.; Zhukov, E. A.; Kirstein, E.; Kazimierczuk, T.; Korenev, V. L.; Yugova, I. A.; Yakovlev, D. R.; Pawlis, A.; Bayer, M.

2015-12-01

Optically induced nuclear spin polarization in a fluorine-doped ZnSe epilayer is studied by time-resolved Kerr rotation using resonant excitation of donor-bound excitons. Excitation with helicity-modulated laser pulses results in a transverse nuclear spin polarization, which is detected as a change of the Larmor precession frequency of the donor-bound electron spins. The frequency shift in dependence on the transverse magnetic field exhibits a pronounced dispersion-like shape with resonances at the fields of nuclear magnetic resonance of the constituent zinc and selenium isotopes. It is studied as a function of external parameters, particularly of constant and radio frequency external magnetic fields. The width of the resonance and its shape indicate a strong spatial inhomogeneity of the nuclear spin polarization in the vicinity of a fluorine donor. A mechanism of optically induced nuclear spin polarization is suggested based on the concept of resonant nuclear spin cooling driven by the inhomogeneous Knight field of the donor-bound electron.

Nuclear polarization and neutrons

International Nuclear Information System (INIS)

Glaettli, H.

1985-01-01

Different possibilities for the use of polarized nuclei in thermal neutron scattering on condensed matter are reviewed. Highly polarized nuclei are the starting point for studying dipolar magnetic order. Systematic measurement of spin-dependent scattering lengths is possible on samples with polarized nuclei. Highly polarized hydrogen should help to unravel complicated structures in chemistry and biology. The use of polarized proton targets as an energy-independent neutron polarizer in the thermal and epithermal region should be considered afresh. (author)

Some nitrogen-14 NMR studies in solids

International Nuclear Information System (INIS)

Pratum, T.K.

1983-11-01

The first order quadrupolar perturbation of the 14 N NMR spectrum yields information regarding the static and dynamic properties of the surrounding electronic environment. Signal to noise problems caused by long 14 N longitudinal relaxation times (T 1 ) and small equilibrium polarizations are reduced by rotating frame cross polarization (CP) experiments between 14 N and 1 H. Using quadrupolar echo and CP techniques, the 14 N quadrupolar coupling constants (e 2 qQ/h) and asymmetry parameters (eta) have been obtained for a variety of tetraalkylammonium compounds by observation of their quadrupolar powder patterns at various temperatures. For choline chloride and iodide the 14 N NMR powder patterns exhibit the effects of anisotropic molecular motion, while choline bromide spectra show no such effects

NMR spectroscopy and drug development

International Nuclear Information System (INIS)

Craik, D.; Munro, S.

1990-01-01

The use of nuclear magnetic resonance (NMR) spectroscopy for structural and conformational studies on drug molecules, the three-dimensional investigation of proteins structure and their interactions with ligands are discussed. In-vivo NMR studies of the effects of drugs on metabolism in perfused organs and whole animals are also briefly presented. 5 refs., ills

NMR in pulsed magnetic field

KAUST Repository

Abou-Hamad, Edy; Bontemps, P.; Rikken, Geert L J A

2011-01-01

Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

NMR in pulsed magnetic field

KAUST Repository

Abou-Hamad, Edy

2011-09-01

Nuclear magnetic resonance (NMR) experiments in pulsed magnetic fields up to 30.4 T focused on 1H and 93Nb nuclei are reported. Here we discuss the advantage and limitation of pulsed field NMR and why this technique is able to become a promising research tool. © 2011 Elsevier Inc. All Rights Reserved.

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.

Method of generating intense nuclear polarized beams by selective photodetachment of negative ions

International Nuclear Information System (INIS)

Hershcovitch, A.

1986-01-01

A novel method for production of nuclear polarized negative hydrogen ions by selective neutralization with a laser of negative hydrogen ions in a magnetic field is described. This selectivity is possible since a final state of the neutralized atom, and hence the neutralization energy, depends on its nuclear polarization. The main advantages of this scheme are the availability of multi-ampere negative ion sources and the possibility of neutralizing negative ions with very high efficiency. An assessment of the required laser power indicates that this method is in principle feasible with today's technology

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

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

International Nuclear Information System (INIS)

Zandomeneghi, Giorgia; Meier, Beat H.

2004-01-01

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

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.

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

Science.gov (United States)

Gopinath, T.; Veglia, Gianluigi

2015-04-01

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

Cation Hydration Constants by Proton NMR: A Physical Chemistry Experiment.

Science.gov (United States)

Smith, Robert L.; And Others

1988-01-01

Studies the polarization effect on water by cations and anions. Describes an experiment to illustrate the polarization effect of sodium, lithium, calcium, and strontium ions on the water molecule in the hydration spheres of the ions. Analysis is performed by proton NMR. (MVL)

Spin filtering neutrons with a proton target dynamically polarized using photo-excited triplet states

International Nuclear Information System (INIS)

Haag, M.; Brandt, B. van den; Eichhorn, T.R.; Hautle, P.; Wenckebach, W.Th.

2012-01-01

In a test of principle a neutron spin filter has been built, which is based on dynamic nuclear polarization (DNP) using photo-excited triplet states. This DNP method has advantages over classical concepts as the requirements for cryogenic equipment and magnets are much relaxed: the spin filter is operated in a field of 0.3 T at a temperature of about 100 K and has performed reliably over periods of several weeks. The neutron beam was also used to analyze the polarization of the target employed as a spin filter. We obtained an independent measurement of the proton spin polarization of ∼0.13 in good agreement with the value determined with NMR. Moreover, the neutron beam was used to measure the proton spin polarization as a function of position in the naphthalene sample. The polarization was found to be homogeneous, even at low laser power, in contradiction to existing models describing the photo-excitation process.

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.

Some nitrogen-14 NMR studies in solids

Energy Technology Data Exchange (ETDEWEB)

Pratum, T.K.

1983-11-01

The first order quadrupolar perturbation of the /sup 14/N NMR spectrum yields information regarding the static and dynamic properties of the surrounding electronic environment. Signal to noise problems caused by long /sup 14/N longitudinal relaxation times (T/sub 1/) and small equilibrium polarizations are reduced by rotating frame cross polarization (CP) experiments between /sup 14/N and /sup 1/H. Using quadrupolar echo and CP techniques, the /sup 14/N quadrupolar coupling constants (e/sup 2/qQ/h) and asymmetry parameters (eta) have been obtained for a variety of tetraalkylammonium compounds by observation of their quadrupolar powder patterns at various temperatures. For choline chloride and iodide the /sup 14/N NMR powder patterns exhibit the effects of anisotropic molecular motion, while choline bromide spectra show no such effects.

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

Selective sensitivity enhancement in FT-NMR

International Nuclear Information System (INIS)

Farrar, T.C.

1987-01-01

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

Dynamical nuclear spin polarization induced by electronic current through double quantum dots

International Nuclear Information System (INIS)

Lopez-Monis, Carlos; Platero, Gloria; Inarrea, Jesus

2011-01-01

We analyse electron-spin relaxation in electronic transport through coherently coupled double quantum dots (DQDs) in the spin blockade regime. In particular, we focus on hyperfine (HF) interaction as the spin-relaxation mechanism. We pay special attention to the effect of the dynamical nuclear spin polarization induced by the electronic current on the nuclear environment. We discuss the behaviour of the electronic current and the induced nuclear spin polarization versus an external magnetic field for different HF coupling intensities and interdot tunnelling strengths. We take into account, for each magnetic field, all HF-mediated spin-relaxation processes coming from different opposite spin level approaches. We find that the current as a function of the external magnetic field shows a peak or a dip and that the transition from a current dip to a current peak behaviour is obtained by decreasing the HF coupling or by increasing the interdot tunnelling strength. We give a physical picture in terms of the interplay between the electrons tunnelling out of the DQD and the spin-flip processes due to the nuclear environment.

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

Science.gov (United States)

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

2017-10-20

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

High-Throughput Screening by Nuclear Magnetic Resonance (HTS by NMR) for the Identification of PPIs Antagonists.

Science.gov (United States)

Wu, Bainan; Barile, Elisa; De, Surya K; Wei, Jun; Purves, Angela; Pellecchia, Maurizio

2015-01-01

In recent years the ever so complex field of drug discovery has embraced novel design strategies based on biophysical fragment screening (fragment-based drug design; FBDD) using nuclear magnetic resonance spectroscopy (NMR) and/or structure-guided approaches, most often using X-ray crystallography and computer modeling. Experience from recent years unveiled that these methods are more effective and less prone to artifacts compared to biochemical high-throughput screening (HTS) of large collection of compounds in designing protein inhibitors. Hence these strategies are increasingly becoming the most utilized in the modern pharmaceutical industry. Nonetheless, there is still an impending need to develop innovative and effective strategies to tackle other more challenging targets such as those involving protein-protein interactions (PPIs). While HTS strategies notoriously fail to identify viable hits against such targets, few successful examples of PPIs antagonists derived by FBDD strategies exist. Recently, we reported on a new strategy that combines some of the basic principles of fragment-based screening with combinatorial chemistry and NMR-based screening. The approach, termed HTS by NMR, combines the advantages of combinatorial chemistry and NMR-based screening to rapidly and unambiguously identify bona fide inhibitors of PPIs. This review will reiterate the critical aspects of the approach with examples of possible applications.

Polarized Electron Beams for Nuclear Physics at the MIT Bates Accelerator Center

CERN Document Server

Farkhondeh, Manouchehr; Franklin, Wilbur; Ihloff, Ernie; McAllister, Brian; Milner, Richard; North, William; Tschalär, C; Tsentalovich, Evgeni; Wang, Defa; Wang, Dong; Wang, Fuhua; Zolfaghari, Abbasali; Zwart, Townsend; van der Laan, Jan

2005-01-01

The MIT Bates Accelerator Center is delivering highly polarized electron beams to its South Hall Ring for use in Nuclear Physics Experiments. Circulating electron currents in excess of 200 mA with polarization of 70% are scattered from a highly polarized, but very thin atomic beam source deuterium target. At the electron source a compact diode laser creates photoemission of quasi-CW mA pulses of polarized electrons at low duty factors from a strained GaAs photocathode. Refurbished RF transmitters provide power to the 2856 MHz linac, accelerating the beam to 850 MeV in two passes before injection into the South Hall Ring. In the ring a Siberian snake serves to maintain a high degree of longitudinal polarization at the BLAST scattering target. A Compton laser back-scattering polarimeter measures the electron beam polarization with a statistical acuracy of 6% every 15 minutes.

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

Nuclear magnetic resonance (NMR) can probe the local structure and dynamic properties of liquids and solids, making it one of the most powerful and versatile analytical methods available today. However, its intrinsically low sensitivity precludes NMR analysis of very small samples - as frequently used when studying isotopically labelled biological molecules or advanced materials, or as preferred when conducting high-throughput screening of biological samples or 'lab-on-a-chip' studies. The sensitivity of NMR has been improved by using static micro-coils, alternative detection schemes and pre-polarization approaches. But these strategies cannot be easily used in NMR experiments involving the fast sample spinning essential for obtaining well-resolved spectra from non-liquid samples. Here we demonstrate that inductive coupling allows wireless transmission of radio-frequency pulses and the reception of NMR signals under fast spinning of both detector coil and sample. This enables NMR measurements characterized by an optimal filling factor, very high radio-frequency field amplitudes and enhanced sensitivity that increases with decreasing sample volume. Signals obtained for nano-litre-sized samples of organic powders and biological tissue increase by almost one order of magnitude (or, equivalently, are acquired two orders of magnitude faster), compared to standard NMR measurements. Our approach also offers optimal sensitivity when studying samples that need to be confined inside multiple safety barriers, such as radioactive materials. In principle, the co-rotation of a micrometer-sized detector coil with the sample and the use of inductive coupling (techniques that are at the heart of our method) should enable highly sensitive NMR measurements on any mass-limited sample that requires fast mechanical rotation to obtain well-resolved spectra. The method is easy to implement on a commercial NMR set-up and exhibits improved performance with miniaturization, and we

Polarization of nuclear spins by a cold nanoscale resonator

International Nuclear Information System (INIS)

Butler, Mark C.; Weitekamp, Daniel P.

2011-01-01

A cold nanoscale resonator coupled to a system of nuclear spins can induce spin relaxation. In the low-temperature limit where spin-lattice interactions are ''frozen out,'' spontaneous emission by nuclear spins into a resonant mechanical mode can become the dominant mechanism for cooling the spins to thermal equilibrium with their environment. We provide a theoretical framework for the study of resonator-induced cooling of nuclear spins in this low-temperature regime. Relaxation equations are derived from first principles, in the limit where energy donated by the spins to the resonator is quickly dissipated into the cold bath that damps it. A physical interpretation of the processes contributing to spin polarization is given. For a system of spins that have identical couplings to the resonator, the interaction Hamiltonian conserves spin angular momentum, and the resonator cannot relax the spins to thermal equilibrium unless this symmetry is broken by the spin Hamiltonian. The mechanism by which such a spin system becomes ''trapped'' away from thermal equilibrium can be visualized using a semiclassical model, which shows how an indirect spin-spin interaction arises from the coupling of multiple spins to one resonator. The internal spin Hamiltonian can affect the polarization process in two ways: (1) By modifying the structure of the spin-spin correlations in the energy eigenstates, and (2) by splitting the degeneracy within a manifold of energy eigenstates, so that zero-frequency off-diagonal terms in the density matrix are converted to oscillating coherences. Shifting the frequencies of these coherences sufficiently far from zero suppresses the development of resonator-induced correlations within the manifold during polarization from a totally disordered state. Modification of the spin-spin correlations by means of either mechanism affects the strength of the fluctuating spin dipole that drives the resonator. In the case where product states can be chosen as energy

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

Science.gov (United States)

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

2016-09-09

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

Fingerprinting analysis of Saposhnikovia divaricata using 1H nuclear magnetic resonance spectroscopy and high performance liquid chromatography.

Science.gov (United States)

Xin, Yue-Yang; Deng, An-Jun; Du, Guan-Hua; Zhang, Jin-Lan; Qin, Hai-Lin

2010-09-01

The (1)H nuclear magnetic resonance ((1)H NMR) fingerprints of fractionated non-polar and polar extracts (control substance for plant drug [CSPD] A and B) from the roots of 12 specimens of Saposhnikovia divaricata (Turcz.) Schischk were achieved with Fourier Transform (FT)-NMR spectrometer and assigned by comparison to each other and to the (1)H NMR spectra of the isolated individual compounds. These fingerprints were found to be uniform in terms of the specificity for the implication of all 12 specimens being systematically of the same origin. The uniformity was further affirmed by high performance liquid chromatography (HPLC), which also revealed exactly identical specificity for the identified S. divaricata species with the (1)H NMR appearances of corresponding CSPD on the part of the composition of characteristic constituents when comparing to corresponding individual compounds. This investigation unambiguously shows that the specific signals from the chemotaxonomically significant compounds of chromones and coumarins in S. divaricata are exhibited distinctively in the composite features of both (1)H NMR fingerprints and HPLC profiles. The (1)H NMR and HPLC profiles established can successfully be used as reference for the authentication of the origin of S. divaricata species as well as for chemotaxonomic studies.

Cholesteric lyomesophases based on sodium N-lauroyl asparte: characterization of new system by nuclear magnetic resonance and polarizing microscopy

International Nuclear Information System (INIS)

Melo, M.V.M.C. de.

1982-01-01

Lyomesophases based on di-sodium N-lauroyl aspartate (SNLA), bi-carboxilated amphiphile obtained from the reaction of n-lauroyl chloride with aspartic acid in racemic or levo form are studies. The different mesophases were characterized by 2 H and 23 Na NMR and by polarizing microscopy. (M.J.C.) [pt

Nuclear magnetic resonance (NMR) spectroscopy and its application to biomedical research

Energy Technology Data Exchange (ETDEWEB)

Nakazawa, Mikio; Imai, Shoichi

1988-07-01

The principles of nuclear magnetic resonance (NMR) spectroscopy were explained and its application to biomedical research discussed. With /sup 31/P-NMR, it is feasible to conduct a continuous, non-invasive measurement of the contents of myocardial high-energy phosphate compounds and the intracellular pH (determined by monitoring the pH dependent shift of the inorganic phosphate peak relative to that of creatine phosphate), and to correlate them with the mechanical function. The determination of the free magnesium concentration is also possible on a similar principle to that for pH determination (the shift of MgATP peaks relative to ATP is utilized in this case). It is estimated to be 0.3 mM and was found not to be changed during ischemia. Several examples of studies including our own conducted to delineate the ischemic derangements of the myocardial energy metabolism and the effects of various interventions thereupon were illustrated. Finally a brief mention was made of the saturation transfer technique. This is the only method with which one can study the kinetics of the enzyme reactions under in vivo conditions. The application of the method for analysis of the creatine kinase reaction and the ATP synthesis was demonstrated. (author) 49 refs.

Nuclear magnetic resonance (NMR) spectroscopy and its application to biomedical research

International Nuclear Information System (INIS)

Nakazawa, Mikio; Imai, Shoichi

1988-01-01

The principles of nuclear magnetic resonance (NMR) spectroscopy were explained and its application to biomedical research discussed. With 31 P-NMR, it is feasible to conduct a continuous, non-invasive measurement of the contents of myocardial high-energy phosphate compounds and the intracellular pH (determined by monitoring the pH dependent shift of the inorganic phosphate peak relative to that of creatine phosphate), and to correlate them with the mechanical function. The determination of the free magnesium concentration is also possible on a similar principle to that for pH determination (the shift of MgATP peaks relative to ATP is utilized in this case). It is estimated to be 0.3 mM and was found not to be changed during ischemia. Several examples of studies including our own conducted to delineate the ischemic derangements of the myocardial energy metabolism and the effects of various interventions thereupon were illustrated. Finally a brief mention was made of the saturation transfer technique. This is the only method with which one can study the kinetics of the enzyme reactions under in vivo conditions. The application of the method for analysis of the creatine kinase reaction and the ATP synthesis was demonstrated. (author) 49 refs

Increasing Spin Coherence in Nanodiamond via Dynamic Nuclear Polarization

Science.gov (United States)

Gaebel, Torsten; Rej, Ewa; Boele, Thomas; Waddington, David; Reilly, David

Nanodiamonds are of interest for quantum information technology, as metrological sensors, and more recently as a probe of biological environments. Here we present results examining how intrinsic defects can be used for dynamic nuclear polarization that leads to a dramatic increase in both T1 and T2 for 13C spins in nanodiamond. Mechanisms to explain this enhancement are discussed.

Polarization measurement for internal polarized gaseous targets

International Nuclear Information System (INIS)

Ye Zhenyu; Ye Yunxiu; Lv Haijiang; Mao Yajun

2004-01-01

The authors present an introduction to internal polarized gaseous targets, polarization method, polarization measurement method and procedure. To get the total nuclear polarization of hydrogen atoms (including the polarization of the recombined hydrogen molecules) in the target cell, authors have measured the parameters relating to atomic polarization and polarized hydrogen atoms and molecules. The total polarization of the target during our measurement is P T =0.853 ± 0.036. (authors)

Nuclear studies at TUNL using polarized neutron beams

International Nuclear Information System (INIS)

Walter, R.L.; Howell, C.R.; Tornow, W.

1992-01-01

Experimental data obtained using polarized neutron beams has proven to be essential for determining the nucleon-nucleon and the nucleon-nucleus interaction. The present paper reviews the experimental methods and some results of the Triangle Universities Nuclear Laboratory for a variety of polarization experiments involving neutron elastic scattering. A brief introduction to the nucleon-nucleon problem and its relation to the three-nucleon problem is presented; data for n-p and n-d analyzing powers are highlighted. Measurements involving heavier targets ( 93 Nb and 208 Pb) and their connection to the development of conventional and dispersive optical models are shown. The importance of the dispersive model for 27 Al in relation to conclusions about the nucleon-nucleus spin-spin potential is presented. Comparisons of microscopic models to data for 10 B and 28 Si are described

NMR polarization echoes in a nematic liquid crystal

Science.gov (United States)

Levstein, Patricia R.; Chattah, Ana K.; Pastawski, Horacio M.; Raya, Jésus; Hirschinger, Jérôme

2004-10-01

We have modified the polarization echo (PE) sequence through the incorporation of Lee-Goldburg cross polarization steps to quench the 1H-1H dipolar dynamics. In this way, the 13C becomes an ideal local probe to inject and detect polarization in the proton system. This improvement made possible the observation of the local polarization P00(t) and polarization echoes in the interphenyl proton of the liquid crystal N-(4-methoxybenzylidene)-4-butylaniline. The decay of P00(t) was well fitted to an exponential law with a characteristic time τC≈310 μs. The hierarchy of the intramolecular dipolar couplings determines a dynamical bottleneck that justifies the use of the Fermi Golden Rule to obtain a spectral density consistent with the structural parameters. The time evolution of P00(t) was reversed by the PE sequence generating echoes at the time expected by the scaling of the dipolar Hamiltonian. This indicates that the reversible 1H-1H dipolar interaction is the main contribution to the local polarization decrease and that the exponential decay for P00(t) does not imply irreversibility. The attenuation of the echoes follows a Gaussian law with a characteristic time τφ≈527 μs. The shape and magnitude of the characteristic time of the PE decay suggest that it is dominated by the unperturbed homonuclear dipolar Hamiltonian. This means that τφ is an intrinsic property of the dipolar coupled network and not of other degrees of freedom. In this case, one cannot unambiguously identify the mechanism that produces the decoherence of the dipolar order. This is because even weak interactions are able to break the fragile multiple coherences originated on the dipolar evolution, hindering its reversal. Other schemes to investigate these underlying mechanisms are proposed.

Different sets of ER-resident J-proteins regulate distinct polar nuclear-membrane fusion events in Arabidopsis thaliana.

Science.gov (United States)

Maruyama, Daisuke; Yamamoto, Masaya; Endo, Toshiya; Nishikawa, Shuh-ichi

2014-11-01

Angiosperm female gametophytes contain a central cell with two polar nuclei. In many species, including Arabidopsis thaliana, the polar nuclei fuse during female gametogenesis. We previously showed that BiP, an Hsp70 in the endoplasmic reticulum (ER), was essential for membrane fusion during female gametogenesis. Hsp70 function requires partner proteins for full activity. J-domain containing proteins (J-proteins) are the major Hsp70 functional partners. A. thaliana ER contains three soluble J-proteins, AtERdj3A, AtERdj3B, and AtP58(IPK). Here, we analyzed mutants of these proteins and determined that double-mutant ovules lacking AtP58(IPK) and AtERdj3A or AtERdj3B were defective in polar nuclear fusion. Electron microscopy analysis identified that polar nuclei were in close contact, but no membrane fusion occurred in mutant ovules lacking AtP58(IPK) and AtERdj3A. The polar nuclear outer membrane appeared to be connected via the ER remaining at the inner unfused membrane in mutant ovules lacking AtP58(IPK) and AtERdj3B. These results indicate that ER-resident J-proteins, AtP58(IPK)/AtERdj3A and AtP58(IPK)/AtERdj3B, function at distinct steps of polar nuclear-membrane fusion. Similar to the bip1 bip2 double mutant female gametophytes, the aterdj3a atp58(ipk) double mutant female gametophytes defective in fusion of the outer polar nuclear membrane displayed aberrant endosperm proliferation after fertilization with wild-type pollen. However, endosperm proliferated normally after fertilization of the aterdj3b atp58(ipk) double mutant female gametophytes defective in fusion of the inner membrane. Our results indicate that the polar nuclear fusion defect itself does not cause an endosperm proliferation defect. © The Author 2014. Published by Oxford University Press on behalf of Japanese Society of Plant Physiologists. All rights reserved. For permissions, please email: journals.permissions@oup.com.

VME online system of the Bonn polarized nucleon targets and polarization measurements on NH3

International Nuclear Information System (INIS)

Thiel, W.

1991-02-01

The measurement of spin observables is the main purpose of the PHOENICS detector at the Bonn Electron Accelerator ELSA. Therefore a new frosen spin target was built allowing any spin orientation by means of two perpendicular holding fields and the use of a polarizing field up to 7 Tesla. With a vertical dilution refrigerator the polarization can be frozen at a temperature of 70 mK. This thesis describe a VME based control and monitor system for the various parts of this target. It mainly consists of a VIP processor together with different kinds of I/O and interface boards. Caused by its modular structure in hard- and software it can be easyly set up to control and monitor different hardware environments. A menu and command oriented user interface running on an ATARI computer allows a comfortable operation. Secondly the new NMR system is described in detail. It is based on the Liferpool module allowing a dispersion user interface running on an ATARI computer allows a comfortable operation. Secondly the new NMR system is described in detail. It is based on the Liverpool module allowing a dispersion free detection and a simple adjustment to different magnetic fields. A similar VME system takes care of all the necessary task for the polarization measurements. Fast optodecoupled analog I/O modules a e used as an interface to the NMR hardware. Finally the first measurements with this target are presented. Using NH 3 as target material and a polarizing field of 3.5 Tesla a proton polarization of +94% and -100% could be achieved. By lowering the magnetic field to 0.35 Tesla a superradiance effect was observed. (orig.)

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....

Two-dimensional NMR spectroscopy of 13C methanol at less than 5 μT

Science.gov (United States)

Shim, Jeong Hyun; Lee, Seong-Joo; Hwang, Seong-min; Yu, Kwon-Kyu; Kim, Kiwoong

2014-09-01

Two-dimensional (2D) spectroscopy is one of the most significant applications of nuclear magnetic resonance (NMR). Here, we demonstrate that the 2D NMR can be performed even at a low magnetic field of less than 5 μT, which is ten times less than the Earth’s magnetic field. The pulses used in the experiment were composed of circularly polarized fields for coherent as well as wideband excitations. Since the excitation band covers the entire spectral range, the simplest two-pulse sequence delivered the full 2D spectrum. At 5 μT, methanol with 13C enriched up to 99% belongs to a strongly coupled regime, and thus its 2D spectrum exhibits complicated spectral correlations, which can be exploited as a fingerprint in chemical analysis. In addition, we show that, with compressive sensing, the acquisition of the 2D spectrum can be accelerated to take only 45% of the overall duration.

Structure and dynamics of paramagnetic transients by pulsed EPR and NMR detection of nuclear resonance. [Pulse radiolysis of methanol in D/sub 2/O

Energy Technology Data Exchange (ETDEWEB)

Trifunac, A.D.

1981-01-01

Structure and dynamics of transient radicals in pulse radiolysis can be studied by time resolved EPR and NMR techniques. EPR study of kinetics and relaxation is illustrated. The NMR detection of nuclear resonance in transient radicals is a new method which allows the study of hyperfine coupling, population dynamics, radical kinetics, and reaction mechanism. 9 figures.

Nuclear magnetic resonance with dc SQUID [Super-conducting QUantum Interference Device] preamplifiers

International Nuclear Information System (INIS)

Fan, N.Q.; Heaney, M.B.; Clark, J.; Newitt, D.; Wald, L.; Hahn, E.L.; Bierlecki, A.; Pines, A.

1988-08-01

Sensitive radio-frequency (rf) amplifiers based on dc Superconducting QUantum Interface Devices (SQUIDS) are available for frequencies up to 200 MHz. At 4.2 K, the gain and noise temperature of a typical tuned amplifier are 18.6 +- 0.5 dB and 1.7 +- 0.5 K at 93 MHz. These amplifiers are being applied to a series of novel experiments on nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR). The high sensitivity of these amplifiers was demonstrated in the observation of ''nuclear spin noise'', the emission of photons by 35 Cl nuclei in a state of zero polarization. In the more conventional experiments in which one applies a large rf pulse to the spins, a Q-spoiler, consisting of a series array of Josephson junctions, is used to reduce the Q of the input circuit to a very low value during the pulse. The Q-spoiler enables the circuit to recover quickly after the pulse, and has been used in an NQR experiment to achieve a sensitivity of about 2 /times/ 10 16 nuclear Bohr magnetons in a single free precession signal with a bandwidth of 10 kHz. In a third experiment, a sample containing 35 Cl nuclei was placed in a capacitor and the signal detected electrically using a tuned SQUID amplifier and Q-spoiler. In this way, the electrical polarization induced by the precessing Cl nuclear quadrupole moments was detected: this is the inverse of the Stark effect in NQR. Two experiments involving NMR have been carried out. In the first, the 30 MHz resonance in 119 Sn nuclei is detected with a tuned amplifier and Q-spoiler, and a single pulse resolution of 10 18 nuclear Bohr magnetons in a bandwidth of 25 kHz has been achieved. For the second, a low frequency NMR system has been developed that uses an untuned input circuit coupled to the SQUID. The resonance in 195 Pt nuclei has been observed at 55 kHz in a field of 60 gauss. 23 refs., 11 figs

Measurement of 14N quadrupole couplings in biomolecular solids using indirect-detection 14N solid-state NMR with DNP.

Science.gov (United States)

Jarvis, J A; Haies, I; Lelli, M; Rossini, A J; Kuprov, I; Carravetta, M; Williamson, P T F

2017-11-07

The quadrupolar interaction experienced by the spin-1 14 N nucleus is known to be extremely sensitive to local structure and dynamics. Furthermore, the 14 N isotope is 99.6% naturally abundant, making it an attractive target for characterisation of nitrogen-rich biological molecules by solid-state NMR. In this study, dynamic nuclear polarization (DNP) is used in conjunction with indirect 14 N detected solid-state NMR experiments to simultaneously characterise the quadrupolar interaction at multiple 14 N sites in the backbone of the microcrystalline protein, GB3. Considerable variation in the quadrupolar interaction (>700 kHz) is observed throughout the protein backbone. The distribution in quadrupolar interactions observed reports on the variation in local backbone conformation and subtle differences in hydrogen-bonding; demonstrating a new route to the structural and dynamic analysis of biomolecules.

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

Science.gov (United States)

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

2017-09-18

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

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

Czech Academy of Sciences Publication Activity Database

Hanzlíček, Tomáš; Perná, Ivana; Brus, Jiří

2013-01-01

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

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...

High-field Overhauser dynamic nuclear polarization in silicon below the metal-insulator transition.

Science.gov (United States)

Dementyev, Anatoly E; Cory, David G; Ramanathan, Chandrasekhar

2011-04-21

Single crystal silicon is an excellent system to explore dynamic nuclear polarization (DNP), as it exhibits a continuum of properties from metallic to insulating as a function of doping concentration and temperature. At low doping concentrations DNP has been observed to occur via the solid effect, while at very high-doping concentrations an Overhauser mechanism is responsible. Here we report the hyperpolarization of (29)Si in n-doped silicon crystals, with doping concentrations in the range of (1-3) × 10(17) cm(-3). In this regime exchange interactions between donors become extremely important. The sign of the enhancement in our experiments and its frequency dependence suggest that the (29)Si spins are directly polarized by donor electrons via an Overhauser mechanism within exchange-coupled donor clusters. The exchange interaction between donors only needs to be larger than the silicon hyperfine interaction (typically much smaller than the donor hyperfine coupling) to enable this Overhauser mechanism. Nuclear polarization enhancement is observed for a range of donor clusters in which the exchange energy is comparable to the donor hyperfine interaction. The DNP dynamics are characterized by a single exponential time constant that depends on the microwave power, indicating that the Overhauser mechanism is a rate-limiting step. Since only about 2% of the silicon nuclei are located within 1 Bohr radius of the donor electron, nuclear spin diffusion is important in transferring the polarization to all the spins. However, the spin-diffusion time is much shorter than the Overhauser time due to the relatively weak silicon hyperfine coupling strength. In a 2.35 T magnetic field at 1.1 K, we observed a DNP enhancement of 244 ± 84 resulting in a silicon polarization of 10.4 ± 3.4% following 2 h of microwave irradiation.

1H NMR-based metabolomics of time-dependent responses of Eisenia fetida to sub-lethal phenanthrene exposure

International Nuclear Information System (INIS)

Lankadurai, Brian P.; Wolfe, David M.; Simpson, Andre J.; Simpson, Myrna J.

2011-01-01

1 H NMR-based metabolomics was used to examine the response of the earthworm Eisenia fetida after exposure to sub-lethal concentrations of phenanthrene over time. Earthworms were exposed to 0.025 mg/cm 2 of phenanthrene (1/64th of the LC 50 ) via contact tests over four days. Earthworm tissues were extracted using a mixture of chloroform, methanol and water, resulting in polar and non-polar fractions that were analyzed by 1 H NMR after one, two, three and four days. NMR-based metabolomic analyses revealed heightened E. fetida responses with longer phenanthrene exposure times. Amino acids alanine and glutamate, the sugar maltose, the lipids cholesterol and phosphatidylcholine emerged as potential indicators of phenanthrene exposure. The conversion of succinate to fumarate in the Krebs cycle was also interrupted by phenanthrene. Therefore, this study shows that NMR-based metabolomics is a powerful tool for elucidating time-dependent relationships in addition to the mode of toxicity of phenanthrene in earthworm exposure studies. - Highlights: → NMR-based earthworm metabolomic analysis of the mode of action of phenanthrene is presented. → The earthworm species E. fetida were exposed to sub-lethal phenanthrene concentrations. → Both polar and non-polar metabolites of E. fetida tissue extracts were analyzed by 1 H NMR. → Longer phenanthrene exposure times resulted in heightened earthworm responses. → An interruption of the Krebs cycle was also observed due to phenanthrene exposure. - 1 H NMR metabolomics is used to determine the relationship between phenanthrene exposure and the metabolic response of the earthworm E. fetida over time and also to elucidate the phenanthrene mode of toxicity.

Electron paramagnetic resonance and dynamic nuclear polarization of char suspensions: surface science and oximetry

DEFF Research Database (Denmark)

Clarkson, R B; Odintsov, B M; Ceroke, P J

1998-01-01

; they can be calibrated and used for oximetry. Biological stability and low toxicity make chars good sensors for in vivo measurements. Scalar and dipolar interactions of water protons at the surfaces of chars may be utilized to produce dynamic nuclear polarization (DNP) of the nuclear spin population...

Nuclear-polarization correction to the bound-electron g factor in heavy hydrogenlike ions

OpenAIRE

Nefiodov, A. V.; Plunien, G.; Soff, G.

2002-01-01

The influence of nuclear polarization on the bound-electron $g$ factor in heavy hydrogenlike ions is investigated. Numerical calculations are performed for the K- and L-shell electrons taking into account the dominant virtual nuclear excitations. This determines the ultimate limit for tests of QED utilizing measurements of the bound-electron $g$ factor in highly charged ions.

Nuclear-polarization correction to the bound-electron g factor in heavy hydrogenlike ions.

Science.gov (United States)

Nefiodov, A V; Plunien, G; Soff, G

2002-08-19

The influence of nuclear polarization on the bound-electron g factor in heavy hydrogenlike ions is investigated. Numerical calculations are performed for the K- and L-shell electrons taking into account the dominant virtual nuclear excitations. This determines the ultimate limit for tests of QED utilizing measurements of the bound-electron g factor in highly charged ions.

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

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

Touch NMR: An NMR Data Processing Application for the iPad

Science.gov (United States)

Li, Qiyue; Chen, Zhiwei; Yan, Zhiping; Wang, Cheng; Chen, Zhong

2014-01-01

Nuclear magnetic resonance (NMR) spectroscopy has become one of the most powerful technologies to aid research in numerous scientific disciplines. With the development of consumer electronics, mobile devices have played increasingly important roles in our daily life. However, there is currently no application available for mobile devices able to…

Generalized nuclear Fukui functions in the framework of spin-polarized density-functional theory

International Nuclear Information System (INIS)

Chamorro, E.; Proft, F. de; Geerlings, P.

2005-01-01

An extension of Cohen's nuclear Fukui function is presented in the spin-polarized framework of density-functional theory (SP-DFT). The resulting new nuclear Fukui function indices Φ Nα and Φ Sα are intended to be the natural descriptors for the responses of the nuclei to changes involving charge transfer at constant multiplicity and also the spin polarization at constant number of electrons. These generalized quantities allow us to gain new insights within a perturbative scheme based on DFT. Calculations of the electronic and nuclear SP-DFT quantities are presented within a Kohn-Sham framework of chemical reactivity for a sample of molecules, including H 2 O, H 2 CO, and some simple nitrenes (NX) and phosphinidenes (PX), with X=H, Li, F, Cl, OH, SH, NH 2 , and PH 2 . Results have been interpreted in terms of chemical bonding in the context of Berlin's theorem, which provides a separation of the molecular space into binding and antibinding regions

Early history of NMR at Los Alamos

International Nuclear Information System (INIS)

Jackson, J.A.

1985-11-01

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

Recent advances in solid state NMR and its application to ceramics

International Nuclear Information System (INIS)

Maekawa, Hideki

2006-01-01

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

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...

Introduction to some basic aspects of NMR

International Nuclear Information System (INIS)

Goldman, M.

1992-01-01

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

{sup 1}H NMR-based metabolomics of time-dependent responses of Eisenia fetida to sub-lethal phenanthrene exposure

Energy Technology Data Exchange (ETDEWEB)

Lankadurai, Brian P.; Wolfe, David M.; Simpson, Andre J. [Department of Chemistry, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4 Canada (Canada); Simpson, Myrna J., E-mail: myrna.simpson@utoronto.ca [Department of Chemistry, University of Toronto, 1265 Military Trail, Toronto, Ontario M1C 1A4 Canada (Canada)

2011-10-15

{sup 1}H NMR-based metabolomics was used to examine the response of the earthworm Eisenia fetida after exposure to sub-lethal concentrations of phenanthrene over time. Earthworms were exposed to 0.025 mg/cm{sup 2} of phenanthrene (1/64th of the LC{sub 50}) via contact tests over four days. Earthworm tissues were extracted using a mixture of chloroform, methanol and water, resulting in polar and non-polar fractions that were analyzed by {sup 1}H NMR after one, two, three and four days. NMR-based metabolomic analyses revealed heightened E. fetida responses with longer phenanthrene exposure times. Amino acids alanine and glutamate, the sugar maltose, the lipids cholesterol and phosphatidylcholine emerged as potential indicators of phenanthrene exposure. The conversion of succinate to fumarate in the Krebs cycle was also interrupted by phenanthrene. Therefore, this study shows that NMR-based metabolomics is a powerful tool for elucidating time-dependent relationships in addition to the mode of toxicity of phenanthrene in earthworm exposure studies. - Highlights: > NMR-based earthworm metabolomic analysis of the mode of action of phenanthrene is presented. > The earthworm species E. fetida were exposed to sub-lethal phenanthrene concentrations. > Both polar and non-polar metabolites of E. fetida tissue extracts were analyzed by {sup 1}H NMR. > Longer phenanthrene exposure times resulted in heightened earthworm responses. > An interruption of the Krebs cycle was also observed due to phenanthrene exposure. - {sup 1}H NMR metabolomics is used to determine the relationship between phenanthrene exposure and the metabolic response of the earthworm E. fetida over time and also to elucidate the phenanthrene mode of toxicity.

Nuclear genomic sequences reveal that polar bears are an old and distinct bear lineage.

Science.gov (United States)

Hailer, Frank; Kutschera, Verena E; Hallström, Björn M; Klassert, Denise; Fain, Steven R; Leonard, Jennifer A; Arnason, Ulfur; Janke, Axel

2012-04-20

Recent studies have shown that the polar bear matriline (mitochondrial DNA) evolved from a brown bear lineage since the late Pleistocene, potentially indicating rapid speciation and adaption to arctic conditions. Here, we present a high-resolution data set from multiple independent loci across the nuclear genomes of a broad sample of polar, brown, and black bears. Bayesian coalescent analyses place polar bears outside the brown bear clade and date the divergence much earlier, in the middle Pleistocene, about 600 (338 to 934) thousand years ago. This provides more time for polar bear evolution and confirms previous suggestions that polar bears carry introgressed brown bear mitochondrial DNA due to past hybridization. Our results highlight that multilocus genomic analyses are crucial for an accurate understanding of evolutionary history.

Efficient DNP NMR of Membrane Proteins: Sample Preparation Protocols, Sensitivity, and Radical Location

Science.gov (United States)

Liao, Shu Y.; Lee, Myungwoon; Wang, Tuo; Sergeyev, Ivan V.; Hong, Mei

2016-01-01

Although dynamic nuclear polarization (DNP) has dramatically enhanced solid-state NMR spectral sensitivities of many synthetic materials and some biological macromolecules, recent studies of membrane-protein DNP using exogenously doped paramagnetic radicals as polarizing agents have reported varied and sometimes surprisingly limited enhancement factors. This motivated us to carry out a systematic evaluation of sample preparation protocols for optimizing the sensitivity of DNP NMR spectra of membrane-bound peptides and proteins at cryogenic temperatures of ~110 K. We show that mixing the radical with the membrane by direct titration instead of centrifugation gives a significant boost to DNP enhancement. We quantify the relative sensitivity enhancement between AMUPol and TOTAPOL, two commonly used radicals, and between deuterated and protonated lipid membranes. AMUPol shows ~4 fold higher sensitivity enhancement than TOTAPOL, while deuterated lipid membrane does not give net higher sensitivity for the membrane peptides than protonated membrane. Overall, a ~100 fold enhancement between the microwave-on and microwave-off spectra can be achieved on lipid-rich membranes containing conformationally disordered peptides, and absolute sensitivity gains of 105–160 can be obtained between low-temperature DNP spectra and high-temperature non-DNP spectra. We also measured the paramagnetic relaxation enhancement of lipid signals by TOTAPOL and AMUPol, to determine the depths of these two radicals in the lipid bilayer. Our data indicate a bimodal distribution of both radicals, a surface-bound fraction and a membrane-bound fraction where the nitroxides lie at ~10 Å from the membrane surface. TOTAPOL appears to have a higher membrane-embedded fraction than AMUPol. These results should be useful for membrane-protein solid-state NMR studies under DNP conditions and provide insights into how biradicals interact with phospholipid membranes. PMID:26873390

Efficient DNP NMR of membrane proteins: sample preparation protocols, sensitivity, and radical location

Energy Technology Data Exchange (ETDEWEB)

Liao, Shu Y.; Lee, Myungwoon; Wang, Tuo [Massachusetts Institute of Technology, Department of Chemistry (United States); Sergeyev, Ivan V. [Bruker Biospin (United States); Hong, Mei, E-mail: meihong@mit.edu [Massachusetts Institute of Technology, Department of Chemistry (United States)

2016-03-15

Although dynamic nuclear polarization (DNP) has dramatically enhanced solid-state NMR spectral sensitivities of many synthetic materials and some biological macromolecules, recent studies of membrane-protein DNP using exogenously doped paramagnetic radicals as polarizing agents have reported varied and sometimes surprisingly limited enhancement factors. This motivated us to carry out a systematic evaluation of sample preparation protocols for optimizing the sensitivity of DNP NMR spectra of membrane-bound peptides and proteins at cryogenic temperatures of ~110 K. We show that mixing the radical with the membrane by direct titration instead of centrifugation gives a significant boost to DNP enhancement. We quantify the relative sensitivity enhancement between AMUPol and TOTAPOL, two commonly used radicals, and between deuterated and protonated lipid membranes. AMUPol shows ~fourfold higher sensitivity enhancement than TOTAPOL, while deuterated lipid membrane does not give net higher sensitivity for the membrane peptides than protonated membrane. Overall, a ~100 fold enhancement between the microwave-on and microwave-off spectra can be achieved on lipid-rich membranes containing conformationally disordered peptides, and absolute sensitivity gains of 105–160 can be obtained between low-temperature DNP spectra and high-temperature non-DNP spectra. We also measured the paramagnetic relaxation enhancement of lipid signals by TOTAPOL and AMUPol, to determine the depths of these two radicals in the lipid bilayer. Our data indicate a bimodal distribution of both radicals, a surface-bound fraction and a membrane-bound fraction where the nitroxides lie at ~10 Å from the membrane surface. TOTAPOL appears to have a higher membrane-embedded fraction than AMUPol. These results should be useful for membrane-protein solid-state NMR studies under DNP conditions and provide insights into how biradicals interact with phospholipid membranes.

Study of the nuclear structure far from stability: Coulomb excitation of neutron-rich Rb isotopes around N=60; Production of nuclear spin polarized beams using the tilted foils technique

International Nuclear Information System (INIS)

Sotty, C.

2013-01-01

The underlying structure in the region A ∼ 100, N ∼ 60 has been under intensive and extensive investigation, mainly by β-decay and γ-ray spectroscopy from fission processes. Around N ∼ 60, by adding just few neutrons, protons a rapid shape change occurs from spherical-like to well deformed g.s. shape. Shape coexistence has been observed in the Sr and Zr nuclei, and is expected to take place in the whole region. The mechanisms involved in the appearance of the deformation is not well understood. The interplay between down-sloping and up-sloping neutron Nilsson orbital is evoked as one of the main reasons for the sudden shape change. However, a clear identification of the active proton and neutron orbitals was still on-going. For that purpose, the neutron rich 93;95;97;99 Rb isotopes have been studied by Coulomb excitation at CERN (ISOLDE) using the REX-ISOLDE post-accelerator and the MINIBALL setup. The completely unknown structures of 97;99 Rb have been populated and observed. Prompt γ-ray coincidences of low-lying states have been observed and time-correlated in order to build level schemes. The associated transition strengths have been extracted with the GOSIA code. The observed matrix elements of the electromagnetic operator constituted new inputs of further theoretical calculations giving new insight on the involved orbitals. The sensitivity of such experiment can be increased using nuclear spin polarized radioactive ion beam. For that purpose the Tilted Foils Technique (TFT) of polarization has been investigated at CERN. This technique consists to spin polarize the ion beam, passing through thin foils tilted at an oblique angle with respect to the beam direction. The initially obtained atomic polarization is transferred to the nucleus by hyperfine interaction. This technique does not depend on the chemical nature of the element. Short lived nuclei can be polarized in-flight without any need to be stopped in a catcher. It opens up the possibility to

Non-Invasive Detection of Adulterated Olive Oil in Full Bottles Using Time-Domain NMR Relaxometry

OpenAIRE

Santos, Poliana M.; Kock, Flávio Vinicius C.; Santos, Maiara S.; Lobo, Carlos Manuel S.; Carvalho, André S.; Colnago, Luiz Alberto

2017-01-01

A fast procedure using time-domain nuclear magnetic resonance (TD-NMR) to detect olive oil adulteration with polyunsaturated vegetable oils in filled bottles is proposed. The 1H transverse relaxation times (T2) of 37 commercial samples were measured using low-field nuclear magnetic resonance (LF-NMR) spectrometer and a unilateral nuclear magnetic resonance (UNMR) sensor. Results obtained with LF-NMR revealed better feasibility when compared with the UNMR sensor, with higher signal-to-noise (S...

Thermostatic properties of semi-infinite polarized nuclear matter

International Nuclear Information System (INIS)

Abd-Alla, M.; Hassan, M.Y.M.; Ramadan, S.

1988-03-01

The surface and curvature properties of semi-infinite polarized nuclear matter (SPNM) are calculated using an expansion for the Fermi integrals up to T 2 . A density matrix expansion is obtained for a modified form of Seyler-Blanchard interaction. New parameters that characterize the surface and curvature properties of SPNM are introduced. The level density parameter is extracted from the low temperature expansion of the free energy and compared with previous calculations. A reasonable agreement is obtained for the parameters calculated before. (author). 78 refs, 1 fig., 5 tabs

Monitoring of the insecticide trichlorfon by phosphorus-31 nuclear magnetic resonance (31P NMR) spectroscopy

International Nuclear Information System (INIS)

Talebpour, Zahra; Ghassempour, Alireza; Zendehzaban, Mehdi; Bijanzadeh, Hamid Reza; Mirjalili, Mohammad Hossein

2006-01-01

Trichlorfon is an organophosphorus insecticide, which is extensively being used for protection of fruit crops. Trichlorfon is a thermal labile compound, which cannot be easily determined by gas chromatography (GC) and has no suitable group for sensitive detection by high performance liquid chromatography (HPLC). In this study, a 31 P nuclear magnetic resonance ( 31 P NMR) has been described for monitoring of trichlorfon without any separation step. The quantitative works of 31 P NMR spectroscopy has been performed in the presence of an internal standard (hexamethylphosphoramide). Limit of detection (LOD) for this method has been found to be 55 mg L -1 , without any sample preparation, and the linear working range was 150-5500 mg L -1 . Relative standard deviation (R.S.D.%) of the method for three replicates within and between days was obtained ≤9%. The average recovery efficiency was approximately 99-112%. This method was applied for monitoring trichlorfon in a commercial insecticide sample and tomato sample

Polarized photoproduction from nuclear targets with arbitrary spin and relation to deep inelastic scattering

International Nuclear Information System (INIS)

Hoodbhoy, P.; Massachusetts Inst. of Tech., Cambridge; Quaid-i-Azam Univ., Islamabad

1990-01-01

Inclusive photo-production from polarized targets of arbitrary spin is analyzed by using multipoles. The Drell-Hearn-Gerasimov sum rule, which was originally fromulated for spin-1/2 targets, is generalized to all spins and multipoles, and shown to have some interesting consequences. Measurements to test the new rules, or to derive nuclear structure information from them, could be incorporated into existing plans at electron accelerator facilities. Finally, the possible relevance of these generalized sum rules to sum rules measurable in polarized lepton-polarized target deep inelastic inclusive scattering is discussed. (orig.)

Determination of the biogenic secondary organic aerosol fraction in the boreal forest by NMR spectroscopy

Directory of Open Access Journals (Sweden)

E. Finessi

2012-01-01

Full Text Available The study investigates the sources of fine organic aerosol (OA in the boreal forest, based on measurements including both filter sampling (PM₁ and online methods and carried out during a one-month campaign held in Hyytiälä, Finland, in spring 2007. Two aerosol mass spectrometers (Q-AMS, ToF-AMS were employed to measure on-line concentrations of major non-refractory aerosol species, while the water extracts of the filter samples were analyzed by nuclear magnetic resonance (NMR spectroscopy for organic functional group characterization of the polar organic fraction of the aerosol. AMS and NMR spectra were processed separately by non-negative factorization algorithms, in order to apportion the main components underlying the submicrometer organic aerosol composition and depict them in terms of both mass fragmentation patterns and functional group compositions.

The NMR results supported the AMS speciation of oxidized organic aerosol (OOA into two main fractions, which could be generally labelled as more and less oxidized organics. The more oxidized component was characterized by a mass spectrum dominated by the m/z 44 peak, and in parallel by a NMR spectrum showing aromatic and aliphatic backbones highly substituted with oxygenated functional groups (carbonyls/carboxyls and hydroxyls. Such component, contributing on average 50% of the OA mass throughout the observing period, was associated with pollution outbreaks from the Central Europe. The less oxidized component was enhanced in concomitance with air masses originating from the North-to-West sector, in agreement with previous investigations conducted at this site. NMR factor analysis was able to separate two distinct components under the less oxidized fraction of OA. One of these NMR-factors was associated with the formation of terrestrial biogenic secondary organic aerosol (BSOA, based on the comparison with spectral profiles obtained from laboratory experiments of

Hyperfine interaction with polarized atomic environment - the nuclear tilted-foil experiment

International Nuclear Information System (INIS)

Niv, Y.

1985-01-01

The nuclear tilted-foil experimental field has matured from the early time-integral measurements to the current multifoil time-differential precession and polarization configurations, leading to a wide range of measurements - magnetic moments, quadrupole moments and parity-non-conservation. The physical basis of these experiments is discussed and experimental results are reviewed. (Auth.)

Use of NMR as an online sensor in industrial processes

International Nuclear Information System (INIS)

Andrade, Fabiana Diuk de

2012-01-01

Nuclear magnetic resonance (NMR) is one of the most versatile analytical techniques for chemical, biochemical and medical applications. Despite this great success, NMR is seldom used as a tool in industrial applications. The first application of NMR in flowing samples was published in 1951. However, only in the last ten years Flow NMR has gained momentum and new and potential applications have been proposed. In this review we present the historical evolution of flow or online NMR spectroscopy and imaging, and current developments for use in the automation of industrial processes. (author)

Nuclear spin dynamics in soap solutions and related systems

International Nuclear Information System (INIS)

Bloom, M.

1973-01-01

Soap molecules consist of a hydrophilic head and a hydrophobic lipid tail. For example, potassium laureate, the soap molecule on which the most complete study of nuclear spin dynamics has been made has the chemical formula KCOO(CH 2 ) 10 CH 3 . High concentration (greater than or approximately equal to 20% soap molecules by weight) soap solutions in water form ordered, liquid crystal structures in which the polar heads are arranged on regular surfaces which define a lattice having long range order. The soap molecules diffuse very rapidly parallel to the surfaces and undergo rapid conformational changes. Studies of T 1 , Tsub(1p) and Tsub(D) have indicated a wide spectrum of correlation times associated with these changes. Because of the orientational order of the soap molecules, the dipolar interactions between nuclear spins on a single molecule are not averaged to zero by the molecular motions. Thus, it is possible to use NMR techniques normally applied to solids (i.e. transfer of Zeeman into dipolar order, etc.) to study their static and dynamical properties. These systems are unusual in that they are basically one-dimensional systems in which the effective, time-averaged, dipolar coupling constants become progressively stronger for protons closer to the polar heads ot the molecules. A review will be presented of the experimental and theoretical NMR work performed on such systems to date. (author)

Structure and function of the Juxta membrane domain of the human epidermal growth factor receptor by NMR spectroscopy

International Nuclear Information System (INIS)

Choowongkomon, Kiattawee; Carlin, Cathleen; Sonnichsen, Frank D.

2005-10-01

The epidermal growth factor receptor (EGFR) is a member of the receptor tyrosine kinase family involved in the regulation of cellular proliferation and differentiation. Its juxta membrane domain (JX), the region located between the transmembrane and kinase domains, plays important roles in receptor trafficking since both basolateral sorting in polarized epithelial cells and lysosomal sorting signals are identified in this region. In order to understand the regulation of these signals, we characterized the structural properties of recombinant JX domain in dodecyl phosphocholine detergent (DPC) by nuclear magnetic resonance (NMR) spectroscopy. In DPC micelles, structures derived from NMR data showed three amphipathic, helical segments. Two equivalent average structural models on the surface of micelles were obtained that differ only in the relative orientation between the first and second helices. Our data suggests that the activity of sorting signals may be regulated by their membrane association and restricted accessibility in the intact receptor

NMR study of Albemoschus esculentus characterization

International Nuclear Information System (INIS)

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

2001-01-01

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

Recommendations of the wwPDB NMR Validation Task Force

Science.gov (United States)

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

2013-01-01

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

Dynamic Nuclear Polarization at low temperature and high magnetic eld for biomedical applications in Magnetic Resonance Spectroscopic Imaging

International Nuclear Information System (INIS)

Goutailler, Florent

2011-01-01

The aim of this thesis work was to design, build and optimize a large volume multi-samples DNP (Dynamic Nuclear Polarization) polarizer dedicated to Magnetic Resonance Spectroscopic Imaging applications. The experimental system is made up of a high magnetic field magnet (3,35 T) in which takes place a cryogenic system with a pumped bath of liquid helium ("4He) allowing temperatures lower than 1,2 K. A set of inserts is used for the different steps of DNP: irradiation of the sample by a microwave field (f=94 GHz and P=50 mW), polarization measurement by Nuclear Magnetic Resonance... With this system, up to three samples of 1 mL volume can be polarized to a rate of few per-cents. The system has a long autonomy of four hours, so it can be used for polarizing molecules with a long time constant of polarization. Finally, the possibility to get quasi-simultaneously, after dissolution, several samples with a high rate of polarization opens the way of new applications in biomedical imaging. (author) [fr

Contribution to the experimental study of the polarized liquid helium-3; Contributions a l'etude experimentale de l'helium-3 liquide polarise

Energy Technology Data Exchange (ETDEWEB)

Villard, B

1999-07-15

Spin-polarized liquid helium-3 is prepared by laser optical pumping in low magnetic field and at room temperature, prior to fast liquefaction of the polarized sample. The use of a new helium-3 cryostat enabled us to obtain liquid helium-3 with polarization rates up to 25 % at well-stabilized temperatures (around 0.5 K). We could thereby study the effect of nuclear polarization on liquid-vapour equilibrium, and particularly on the saturated vapour pressure. Very sensitive capacitive gauges were developed. We estimated (to first order in M{sup 2}) the expected effects when the polarization M is suddenly destroyed. These effects were experimentally observed in helium-3/helium-4 mixtures, in pure helium-3, only a transient increase in pressure has been recorded. We then describe in a third part a preliminary experiment which aimed at determining the longitudinal relaxation time T1 in mixtures. Relaxation on the walls is efficiently reduced by a cesium coating and T1s of order 20 minutes were observed. A careful determination of the helium-3 concentration in the liquid phase was made. Finally we studied the effects of dipolar field on transverse polarisation decay in our strongly polarized samples. We observed the free precession of polarization after a NMR pulse, and analysed in detail its decay time constant as a function of different parameters. This time constant drastically varied with the tipping angle, an effect which could be linked to NMR dynamical instabilities. (author)

Polarization phenomena of nuclear force and weak interaction

International Nuclear Information System (INIS)

Konuma, Michitsugu

1982-01-01

As one of the projects at the National Laboratory of High Energy Physics (KEK), the measurement of parity non-conservation component in nuclear force was proposed. The theoretical survey of this proposal is reported. The non-relativistic parity non-conserving potential between nucleons can be obtained from the interaction between a quark and a gauge boson. The wave function of a nucleus, which includes the inverse components of the parity, can be written. A practical experiment was designed. The mixing of the inverse components and the interference of an inverse component in the 1042 keV and 1081 keV levels of F 18 may produce the parity non-conservation. The processes which suggest the existence of parity non-conservation were studied. The processes are the circular polarization of gamma-ray emitted from a nucleus, the angular distribution of gamma-ray emitted from polarized nuclei, the collision of the proton beam with helicity of plus and minus on other nuclei, the spin rotation of neutrons, and the alpha decay of the parity non-conservation. The preliminary results of the experiment on the effects of parity non-conservation in the collision process of polarized proton beam have been reported, and the theoretical analyses were performed. The violation of parity conservation in large momentum collision is discussed. The comparison of the theoretical results with the experimental ones is presented. (Kato, T.)

LC-NMR coupling technology: recent advancements and applications in natural products analysis

NARCIS (Netherlands)

Exarchou, V.; Krucker, M.; Beek, van T.A.; Vervoort, J.J.M.; Gerothanassis, I.P.; Albert, K.

2005-01-01

An overview of recent advances in nuclear magnetic resonance (NMR) coupled with separation technologies and their application in natural product analysis is given and discussed. The different modes of LC-NMR operation are described, as well as how technical improvements assist in establishing LC-NMR

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)

Nuclear magnetic resonance and medicine. Present applications

International Nuclear Information System (INIS)

1984-01-01

At the workshop on nuclear magnetic resonance and medicine held at Saclay, the following topics were presented: physical principles of NMR; NMR spectroscopy signal to noise ratio; principles of NMR imaging; methods of NMR imaging; image options in NMR; biological significance of contrast in proton NMR imaging; measurement and significance of relaxation times in cancers; NMR contrast agents; NMR for in-vivo biochemistry; potential effects and hazards of NMR applications in Medicine; difficulties of NMR implantation in Hospitals; NMR imaging of brain tumors and diseases of the spinal cord; NMR and Nuclear Medicine in brain diseases [fr

Medium effects in DIS from polarized nuclear targets

Energy Technology Data Exchange (ETDEWEB)

Fanchiotti, Huner; Garcia Canal, Carlos A.; Tarutina, Tatiana [Universidad Nacional de La Plata, Departamento de Fisica, C.C. 67, La Plata (Argentina); Universidad Nacional de La Plata, IFLP(CONICET), C.C. 67, La Plata (Argentina); Vento, Vicente [Universidad de Valencia, Consejo Superior de Investigaciones Cientificas, Departamento de Fisica Teorica and Instituto de Fisica Corpuscular, Burjassot (Valencia) (Spain)

2014-07-15

The behavior of the nucleon structure functions in lepton nuclei deep inelastic scattering, both polarized and unpolarized, due to nuclear structure effects is reanalyzed. The study is performed in two schemes: an x-rescaling approach, and one in which there is an increase of sea quark components in the in-medium nucleon, related to the low-energy N-N interaction. In view of a recent interesting experimental proposal to study the behavior of the proton spin structure functions in nuclei we proceed to compare these approaches in an effort to enlighten the possible phenomenological interest of such difficult experiment. (orig.)

Hydrogen exchange kinetics in a membrane protein determined by 15N NMR spectroscopy: Use of the INEPT [insensitive nucleus enhancement by polarization transfer] experiment to follow individual amides in detergent-solubilized M13 coat protein

International Nuclear Information System (INIS)

Henry, G.D.; Sykes, B.D.

1990-01-01

The coat protein of the filamentous coliphage M13 is a 50-residue polypeptide which spans the inner membrane of the Escherichia coli host upon infection. Amide hydrogen exchange kinetics have been used to probe the structure and dynamics of M13 coat protein which has been solubilized in sodium dodecyl sulfate (SDS) micelles. In a previous 1 H nuclear magnetic resonance (NMR) study, multiple exponential analysis of the unresolved amide proton envelope revealed the existence of two slow kinetic sets containing a total of about 30 protons. The slower set (15-20 amides) originates from the hydrophobic membrane-spanning region and exchanges at least 10 5 -fold slower than the unstructured, non-H-bonded model polypeptide poly(DL-alanine). Herein the authors use 15 N NMR spectroscopy of biosynthetically labeled coat protein to follow individual, assigned, slowly exchanging amides in or near the hydrophobic segment. The INEPT (insensitive nucleus enhancement by polarization transfer) experiments can be used to transfer magnetization to the 15 N nucleus from a coupled proton; when 15 N-labeled protonated protein is dissolved in 2 H 2 O, the INEPT signal disappears with time as the amide protons are replaced by solvent deuterons. Amide hydrogen exchange is catalyzed by both H + and OH - ions. The time-dependent exchange-out experiment is suitable for slow exchange rates (k ex ). The INEPT experiment was also adapted to measure some of the more rapidly exchanging amides in the coat protein using either saturation transfer from water or exchange effects on the polarization transfer step itself. The results of all of these experiments are consistent with previous models of the coat protein in which a stable segment extends from the hydrophobic membrane-spanning region through to the C-terminus, whereas the N-terminal region is undergoing more extensive dynamic fluctuations

Structural Elucidation of Metabolites of Synthetic Cannabinoid UR-144 by Cunninghamella elegans Using Nuclear Magnetic Resonance (NMR) Spectroscopy.

Science.gov (United States)

Watanabe, Shimpei; Kuzhiumparambil, Unnikrishnan; Fu, Shanlin

2018-03-08

The number of new psychoactive substances keeps on rising despite the controlling efforts by law enforcement. Although metabolism of the newly emerging drugs is continuously studied to keep up with the new additions, the exact structures of the metabolites are often not identified due to the insufficient sample quantities for techniques such as nuclear magnetic resonance (NMR) spectroscopy. The aim of the study was to characterise several metabolites of the synthetic cannabinoid (1-pentyl-1H-indol-3-yl) (2,2,3,3-tetramethylcyclopropyl) methanone (UR-144) by NMR spectroscopy after the incubation with the fungus Cunninghamella elegans. UR-144 was incubated with C. elegans for 72 h, and the resulting metabolites were chromatographically separated. Six fractions were collected and analysed by NMR spectroscopy. UR-144 was also incubated with human liver microsomes (HLM), and the liquid chromatography-high resolution mass spectrometry analysis was performed on the HLM metabolites with the characterised fungal metabolites as reference standards. Ten metabolites were characterised by NMR analysis including dihydroxy metabolites, carboxy and hydroxy metabolites, a hydroxy and ketone metabolite, and a carboxy and ketone metabolite. Of these metabolites, dihydroxy metabolite, carboxy and hydroxy metabolites, and a hydroxy and ketone metabolite were identified in HLM incubation. The results indicate that the fungus is capable of producing human-relevant metabolites including the exact isomers. The capacity of the fungus C. elegans to allow for NMR structural characterisation by enabling production of large amounts of metabolites makes it an ideal model to complement metabolism studies.

A biofilm microreactor system for simultaneous electrochemical and nuclear magnetic resonance techniques

International Nuclear Information System (INIS)

Renslow, Ryan S.; Babauta, Jerome T.; Majors, Paul D.; Mehta, Hardeep S.; Ewing, R. James; Ewing, Thomas; Mueller, Karl T.; Beyenal, Haluk

2014-01-01

In order to fully understand electrochemically active biofilms and the limitations to their scale-up in industrial biofilm reactors, a complete picture of the microenvironments inside the biofilm is needed. Nuclear magnetic resonance (NMR) techniques are ideally suited for the study of biofilms and for probing their microenvironments because these techniques allow for non-invasive interrogation and in situ monitoring with high resolution. By combining NMR with simultaneous electrochemical techniques, it is possible to sustain and study live electrochemically active biofilms. Here, we introduce a novel biofilm microreactor system that allows for simultaneous electrochemical and NMR techniques (EC-NMR) at the microscale. Microreactors were designed with custom radiofrequency resonator coils, which allowed for NMR measurements of biofilms growing on polarized gold electrodes. For an example application of this system, we grew Geobacter sulfurreducens biofilms. NMR was used to investigate growth media flow velocities, which were compared to simulated laminar flow, and electron donor concentrations inside the biofilms. We use Monte Carlo error analysis to estimate standard deviations of the electron donor concentration measurements within the biofilm. The EC-NMR biofilm microreactor system can ultimately be used to correlate extracellular electron transfer rates with metabolic reactions and explore extracellular electron transfer mechanisms

Nuclear-charge polarization at scission in fission from moderately excited light-actinide nuclei

International Nuclear Information System (INIS)

Nishinaka, Ichiro

2009-01-01

Fragment mass yields and the average neutron multiplicity in the proton-induced fission of 232 Th and 238 U were measured by a double time-of-flight method. The most probable charges of secondary fragments were evaluated from the fragment mass yields measured by the double time-of-flight method and the fractional cumulative and independent yields reported in literature. The nuclear-charge polarization of primary fragments at scission was obtained by correcting the most probable charge of secondary fragments for neutron evaporation. The results show that the nuclear-charge polarization at scission is associated with the liquid-drop properties of nuclei and the proton shell effect with Z = 50 of heavy fragments and that it is practically insensitive to mass and excitation energy of the fissioning nucleus in the region of light-actinide nuclei. (author)

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 .

Superconducting polarizing magnet for a movable polarized target

International Nuclear Information System (INIS)

Anishchenko, N.G.; Bartenev, V.D.; Blinov, N.A.

1998-01-01

The superconducting polarizing magnet was constructed for the JINR (Dubna) movable polarized target (MPT) with working volume 200 mm long and 30 mm in diameter. The magnet provides a polarizing magnetic field up to 6 T in the centre with the uniformity of 4.5 x 10 -4 in the working volume of the target. The magnet contains a main solenoidal winding 558 mm long and 206/144 mm in diameters, and compensating and correcting winding placed at its ends. The windings are made of a NbTi wire, impregnated with the epoxy resin and placed in the horizontal cryostat. The diameter of the 'warm' aperture of the magnet cryostat is 96 mm. The design and technology of the magnet winding are described. Results of the magnetic field map measurements, using a NMR-magnetometer are given. A similar magnet constructed at DAPNIA, CEA/Saclay (France), represented a model for the present development. The MPT array is installed in the beam line of polarized neutrons produced by break-up of polarized deuterons extracted from the synchrophasotron of the Laboratory of High Energies (LHE), JINR (Dubna)

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

Spin Choreography: Basic Steps in High Resolution NMR (by Ray Freeman)

Science.gov (United States)

Minch, Michael J.

1998-02-01

There are three orientations that NMR courses may take. The traditional molecular structure course focuses on the interpretation of spectra and the use of chemical shifts, coupling constants, and nuclear Overhauser effects (NOE) to sort out subtle details of structure and stereochemistry. Courses can also focus on the fundamental quantum mechanics of observable NMR parameters and processes such a spin-spin splitting and relaxation. More recently there are courses devoted to the manipulation of nuclear spins and the basic steps of one- and two-dimensional NMR experiments. Freeman's book is directed towards the latter audience. Modern NMR methods offer a myriad ways to extract information about molecular structure and motion by observing the behavior of nuclear spins under a variety of conditions. In Freeman's words: "We can lead the spins through an intricate dance, carefully programmed in advance, to enhance, simplify, correlate, decouple, edit or assign NMR spectra." This is a carefully written, well-illustrated account of how this dance is choreographed by pulse programming, double resonance, and gradient effects. Although well written, this book is not an easy read; every word counts. It is recommended for graduate courses that emphasize the fundamentals of magnetic resonance. It is not a text on interpretation of spectra.

Basis of the nuclear magnetic resonance

International Nuclear Information System (INIS)

Bahceli, S.

1996-08-01

The aim of this book which is translated from English language is to explain the physical and mathematical basis of nuclear magnetic resonance (NMR). There are nine chapters covering different aspects of NMR. In the firs chapter fundamental concepts of quantum mechanics are given at a level suitable for readers to understand NMR fully. The remaining chapters discuss the magnetic properties of nucleus, the interactions between atoms and molecules, continuous wave NMR, pulsed NMR, nuclear magnetic relaxation and NMR of liquids

Two-dimensional NMR spectroscopy: correlated, homonuclear-correlated, and nuclear Overhauser spectroscopy. January 1975-December 1988 (Citations from the INSPEC: Information Services for the Physics and Engineering Communities data base). Report for January 1975-December 1988

International Nuclear Information System (INIS)

1988-12-01

This bibliography contains citations concerning the enhanced analytical techniques of two-dimensional nuclear magnetic resonance (2-D NMR). Applications to specific molecules, biomolecules, and compounds as well as comparisons of three 2-D NMR techniques: correlated spectroscopy (COSY), nuclear Overhauser (NOSEY), and homonuclear-correlated spectroscopy (HOMCOR). (Contains 190 citations fully indexed and including a title list.)

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

Fingerprinting analysis of Rhizoma chuanxiong of commercial types using 1H nuclear magnetic resonance spectroscopy and high performance liquid chromatography method.

Science.gov (United States)

Qin, Hai-Lin; Deng, An-Jun; Du, Guan-Hua; Wang, Peng; Zhang, Jin-Lan; Li, Zhi-Hong

2009-06-01

The (1)H nuclear magnetic resonance ((1)H NMR) fingerprints of fractionated non-polar extracts (control substance for a plant drug (CSPD) A) from Rhizoma chuanxiong, the rhizomes of Ligusticum chuanxiong Hort., of seven specimens from different sources were measured on Fourier Transform (FT)-NMR spectrometer and assigned by comparing them with the (1)H NMR spectra of the isolated pure compounds. The (1)H NMR fingerprints showed exclusively characteristic resonance signals of the major special constituents of the plant. Although the differences in the relative intensity of the (1)H NMR signals due to a discrepancy in the ratio of the major constituents among these samples could be confirmed by high performance liquid chromatography analysis, the general features of the (1)H NMR fingerprint established for an authentic sample of the rhizomes of L. chuanxiong exhibited exclusive data from those special compounds and can be used for authenticating L. Chuanxiong species.

Fingerprinting Analysis of Rhizoma Chuanxiong of Commercial Types using 1H Nuclear Magnetic Resonance Spectroscopy and High Performance Liquid Chromatography Method

Institute of Scientific and Technical Information of China (English)

Hai-Lin Qin; An-Jun Deng; Guan-Hua Du; Peng Wang; Jin-Lan Zhang; Zhi-Hong Li

2009-01-01

The 1H nuclear magnetic resonance (1H NMR) fingerprints of fractionated non-polar extracts (control substance for a plant drug (CSPD) A) from Rhizoma chuanxiong, the rhizomes of Ligusticum chuanxiong Hort., of seven specimens from different sources were measured on Fourier Transform (FT)-NMR spectrometer and assigned by comparing them with the 1H NMR spectra of the isolated pure compounds. The 1H NMR fingerprints showed exclusively characteristic resonance signals of the major special constituents of the plant. Although the differences in the relative intensity of the 1H NMR signals due to a discrepancy in the ratio of the major constituents among these samples could be confirmed by high performance liquid chromatography analysis, the general features of the 1H NMR fingerprint established for an authentic sample of the rhizomes of L. chuanxiong exhibited exclusive data from those special compounds and can be used for authenticating L. Chuanxiong species.

New method for preparing a liquid crystal polymer that exhibits linearly polarized white fluorescence

International Nuclear Information System (INIS)

Zheng Shijun; Kun, Wang; Kobayashi, Takaomi

2011-01-01

With the aim of developing a single-chain white-light-emitting polymer, liquid crystal (LC) polymers with a shish-kebab-type moiety on their cross-conjugated (p-phenylene)s-poly(p-phenylenevinylene)s main chain were synthesized by Gilch polymerization. They were characterized by nuclear magnetic resonance (NMR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), X-ray diffraction (XRD), and polarizing optical microscopy (POM). 1 H-NMR indicated that the polymers had a shish-kebab structure, which strongly suppressed the formation of structural defects in the polymers. DSC revealed that the polymers had thermotropic LC properties, indicating that the LC polymers were enantiotropic. XRD showed that the polymers had a mesophase, which implies that they were in a smectic LC phase. A polymer with 'kebabs' of 2,5-bis(4'-alkoxyphenyl)benzene was combined with an aligned polyimide film with orientated microgrooves. The polymer main chain was aligned due to the orientation of the 'kebabs' of the uniform cross-conjugated structure. It lay between the kebabs and the 'shish' of the polymer main chains. The aligned polymer main chain emitted yellow light while and the oriented LC side chains emitted blue light emission. These two emissions resulted in linearly polarized white fluorescence.

Introduction to quantum calculation methods in high resolution NMR

International Nuclear Information System (INIS)

Goldman, M.

1996-01-01

New techniques as for instance the polarization transfer, the coherence with several quanta and the double Fourier transformation have appeared fifteen years ago. These techniques constitute a considerable advance in NMR. Indeed, they allow to study more complex molecules than it was before possible. But with these advances, the classical description of the NMR is not enough to understand precisely the physical phenomena induced by these methods. It is then necessary to resort to quantum calculation methods. The aim of this work is to present these calculation methods. After some recalls of quantum mechanics, the author describes the NMR with the density matrix, reviews the main methods of double Fourier transformation and then gives the principle of the relaxation times calculation. (O.M.)

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

Science.gov (United States)

Thurber, Kent R; Tycko, Robert

2012-08-28

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

Detailed NMR investigation of cyclodextrin-perfluorinated surfactant interactions in aqueous media

Energy Technology Data Exchange (ETDEWEB)

Weiss-Errico, Mary Jo; O’Shea, Kevin E., E-mail: osheak@fiu.edu

2017-05-05

Highlights: • Perfluorochemicals (PFCs) are strongly encapsulated by cyclodextrins (CDs). • Competition studies confirm strong CD:PFC host-guest interactions. • {sup 19}F NMR Spectroscopy demonstrates association constants up to 10{sup 5} M{sup −1}. • Position of CD along PFC chain is elucidated from NMR results. • CD:PFC complex is not disturbed under a variety of water quality conditions. - Abstract: Perfluorochemicals (PFCs) are contaminants of serious concern because of their toxicological properties, widespread presence in drinking water sources, and incredible stability in the environment. To assess the potential application of α-, β-, and γ-cyclodextrins for PFC remediation, we investigated their complexation with linear fluorinated carboxylic acids, sulfonates, and a sulfonamide with carbon backbones ranging from C4-C9. {sup 19}F Nuclear Magnetic Resonance (NMR) spectroscopy studies demonstrated β-CD formed the strongest complexes with these PFCs. The polar head group had a modest influence, but for PFCs with backbones longer than six carbons, strong association constants are observed for 1:1 (K{sub 1:1} ∼ 10{sup 5} M{sup −1}) and 2:1 (K{sub 2:1} ∼ 10{sup 3} M{sup −1}) β-CD:PFC complexes. Excess β-CD can be used to complex 99.5% of the longer chain PFCs. Competition studies with adamantane-carboxylic acid and phenol confirmed the nature and persistence of the β-CD:PFC complex. Detailed analyses of the individual NMR chemical shifts and Job plots indicate the favored positions of the β-CD along the PFC chain. Solution pH, ionic strength, and the presence of humic acid have modest influence on the β-CD:PFC complexes. The strong encapsulation of PFCs by β-CD under a variety of water quality conditions demonstrates the tremendous potential of CD-based materials for the environmental remediation of PFCs.

Laser-perturbed nuclear magnetic resonance spectroscopy and the conservation of parity

International Nuclear Information System (INIS)

Harris, R.A.; Tinoco, I. Jr.

1994-01-01

The effect of polarized incident light on NMR spectra is evaluated; shifts in energy levels and changes in population are calculated. For unoriented systems there is no effect of the amplitude of the field of the light on NMR spectra. The effect of light intensity on NMR spectra produces negligible changes in chemical shifts; fractional changes of less than 10 -6 are calculated for light intensities of 10 W cm -2 . The fundamental concept of conservation of parity is used to obtain general conclusions about the effect of light on NMR spectra of optical isomers. The NMR spectrum of a molecule in right circularly polarized light must be the same as its mirror image molecule in left circularly polarized light. A recent report [Warren et al., Science 255, 1683 (1992)] gives experimental results which are not consistent with any of these conclusions

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.

Inelastic scattering of polarized protons and nuclear deformation in 16O, 18O

International Nuclear Information System (INIS)

de Swiniarski, R.; Pham, D.L.

1984-01-01

Many data concerning inelastic scattering of polarized protons at intermediate energy are now available. We have analyzed some of these data coming from LAMPF at 800 MeV for 16 O (6) and 18 O (7) in order to further study nuclear deformations for these light nuclei. Analyzing powers (A(theta)) and cross-sections ((σ/theta)) for elastic and inelastic scattering of 800 MeV polarized protons from 16 O and 18 O have been analyzed in the coupled-channels (CC) collective model using the code ECIS from Raynal

Unified integration intervals for the structural characterization of oil, coal or fractions there of by 1h NMR and 13c NMR

International Nuclear Information System (INIS)

Avella, Eliseo; Fierro, Ricardo

2010-01-01

Based on an analysis of publications reported between 1972 and 2006, it became clear that there are inaccuracies in the limits of the ranges of integration that the authors assigned to signals in nuclear magnetic resonance (NMR) to the structural characterization of petroleum, coals and their derived fractions, from their hydrogen (1H NMR) and carbon (13C NMR) spectra. Consequently, consolidated limits were determined for the integration of 1H NMR spectra and 13C NMR of these samples using a statistical treatment applied to the limits of integration intervals already published. With these unified limits, correlation NMR charts were developed that are useful for the allocation of the integral at such intervals, and at smaller intervals defined in terms of the intersection between different assignments. Also raised equations needed to establish the integral attributable to specific fragments in an attempt to make a more accurate structural characterization from NMR spectra of oil, coal or fractions derived.

Comparison among Magnus/Floquet/Fer expansion schemes in solid-state NMR

Science.gov (United States)

Takegoshi, K.; Miyazawa, Norihiro; Sharma, Kshama; Madhu, P. K.

2015-04-01

We here revisit expansion schemes used in nuclear magnetic resonance (NMR) for the calculation of effective Hamiltonians and propagators, namely, Magnus, Floquet, and Fer expansions. While all the expansion schemes are powerful methods there are subtle differences among them. To understand the differences, we performed explicit calculation for heteronuclear dipolar decoupling, cross-polarization, and rotary-resonance experiments in solid-state NMR. As the propagator from the Fer expansion takes the form of a product of sub-propagators, it enables us to appreciate effects of time-evolution under Hamiltonians with different orders separately. While 0th-order average Hamiltonian is the same for the three expansion schemes with the three cases examined, there is a case that the 2nd-order term for the Magnus/Floquet expansion is different from that obtained with the Fer expansion. The difference arises due to the separation of the 0th-order term in the Fer expansion. The separation enables us to appreciate time-evolution under the 0th-order average Hamiltonian, however, for that purpose, we use a so-called left-running Fer expansion. Comparison between the left-running Fer expansion and the Magnus expansion indicates that the sign of the odd orders in Magnus may better be reversed if one would like to consider its effect in order.

Comparison among Magnus/Floquet/Fer expansion schemes in solid-state NMR

International Nuclear Information System (INIS)

Takegoshi, K.; Miyazawa, Norihiro; Sharma, Kshama; Madhu, P. K.

2015-01-01

We here revisit expansion schemes used in nuclear magnetic resonance (NMR) for the calculation of effective Hamiltonians and propagators, namely, Magnus, Floquet, and Fer expansions. While all the expansion schemes are powerful methods there are subtle differences among them. To understand the differences, we performed explicit calculation for heteronuclear dipolar decoupling, cross-polarization, and rotary-resonance experiments in solid-state NMR. As the propagator from the Fer expansion takes the form of a product of sub-propagators, it enables us to appreciate effects of time-evolution under Hamiltonians with different orders separately. While 0th-order average Hamiltonian is the same for the three expansion schemes with the three cases examined, there is a case that the 2nd-order term for the Magnus/Floquet expansion is different from that obtained with the Fer expansion. The difference arises due to the separation of the 0th-order term in the Fer expansion. The separation enables us to appreciate time-evolution under the 0th-order average Hamiltonian, however, for that purpose, we use a so-called left-running Fer expansion. Comparison between the left-running Fer expansion and the Magnus expansion indicates that the sign of the odd orders in Magnus may better be reversed if one would like to consider its effect in order

Comparison among Magnus/Floquet/Fer expansion schemes in solid-state NMR

Energy Technology Data Exchange (ETDEWEB)

Takegoshi, K., E-mail: takeyan@kuchem.kyoto-u.ac.jp; Miyazawa, Norihiro [Division of Chemistry, Graduate School of Science, Kyoto University, 606-8502 Kyoto (Japan); Sharma, Kshama [TIFR Centre for Interdisciplinary Sciences, 21 Brundavan Colony, Narsingi, Hyderabad 500 075 (India); Madhu, P. K. [TIFR Centre for Interdisciplinary Sciences, 21 Brundavan Colony, Narsingi, Hyderabad 500 075 (India); Department of Chemical Sciences, Tata Institute of Fundamental Research, Homi Bhabha Road, Colaba, Mumbai 400 005 (India)

2015-04-07

We here revisit expansion schemes used in nuclear magnetic resonance (NMR) for the calculation of effective Hamiltonians and propagators, namely, Magnus, Floquet, and Fer expansions. While all the expansion schemes are powerful methods there are subtle differences among them. To understand the differences, we performed explicit calculation for heteronuclear dipolar decoupling, cross-polarization, and rotary-resonance experiments in solid-state NMR. As the propagator from the Fer expansion takes the form of a product of sub-propagators, it enables us to appreciate effects of time-evolution under Hamiltonians with different orders separately. While 0th-order average Hamiltonian is the same for the three expansion schemes with the three cases examined, there is a case that the 2nd-order term for the Magnus/Floquet expansion is different from that obtained with the Fer expansion. The difference arises due to the separation of the 0th-order term in the Fer expansion. The separation enables us to appreciate time-evolution under the 0th-order average Hamiltonian, however, for that purpose, we use a so-called left-running Fer expansion. Comparison between the left-running Fer expansion and the Magnus expansion indicates that the sign of the odd orders in Magnus may better be reversed if one would like to consider its effect in order.

Structural Characterization of Amadori Rearrangement Product of Glucosylated Nα-Acetyl-Lysine by Nuclear Magnetic Resonance Spectroscopy

Directory of Open Access Journals (Sweden)

Chuanjiang Li

2014-01-01

Full Text Available Maillard reaction is a nonenzymatic reaction between reducing sugars and free amino acid moieties, which is known as one of the most important modifications in food science. It is essential to characterize the structure of Amadori rearrangement products (ARPs formed in the early stage of Maillard reaction. In the present study, the Nα-acetyl-lysine-glucose model had been successfully set up to produce ARP, Nα-acetyl-lysine-glucose. After HPLC purification, ARP had been identified by ESI-MS with intense [M+H]+ ion at 351 m/z and the purity of ARP was confirmed to be over 90% by the relative intensity of [M+H]+ ion. Further structural characterization of the ARP was accomplished by using nuclear magnetic resonance (NMR spectroscopy, including 1D 1H NMR and 13C NMR, the distortionless enhancement by polarization transfer (DEPT-135 and 2D 1H-1H and 13C-1H correlation spectroscopy (COSY and 2D nuclear overhauser enhancement spectroscopy (NOESY. The complexity of 1D 1H NMR and 13C NMR was observed due to the presence of isomers in glucose moiety of ARP. However, DEPT-135 and 2D NMR techniques provided more structural information to assign the 1H and 13C resonances of ARP. 2D NOESY had successfully confirmed the glycosylated site between 10-N in Nα-acetyl-lysine and 7′-C in glucose.

Graphical programming for pulse automated NMR experiments

International Nuclear Information System (INIS)

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

1999-01-01

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

{beta}-Ray angular distribution from purely nuclear spin aligned {sup 20}F

Energy Technology Data Exchange (ETDEWEB)

Nagatomo, T., E-mail: nagatomo@riken.jp [RIKEN Nishina Center (Japan); Matsuta, K. [Osaka University (Japan); Minamisono, K. [NSCL/MSU (United States); Sumikama, T. [Tokyo University of Science (Japan); Mihara, M. [Osaka University (Japan); Ozawa, A.; Tagishi, Y. [University of Tsukuba (Japan); Ogura, M.; Matsumiya, R.; Fukuda, M. [Osaka University (Japan); Yamaguchi, M.; Yasuno, T.; Ohta, H.; Hashizume, Y. [University of Tsukuba (Japan); Fujiwara, H. [Osaka University (Japan); Chiba, A. [University of Tsukuba (Japan); Minamisono, T. [Fukui University of Technology (Japan)

2007-11-15

The alignment correlation term in the {beta}-ray angular distribution from purely nuclear spin aligned {sup 20}F has been measured to test the G-parity conservation law which is one of the fundamental symmetries in the weak nucleon current. We utilized the hyperfine interaction of {sup 20}F in an MgF{sub 2} single crystal and successfully created the pure alignment from the polarization by means of the spin manipulation technique based on the {beta}-NMR method.

Nondestructive NMR technique for moisture determination in radioactive materials

International Nuclear Information System (INIS)

Aumeier, S.; Gerald, R.E. II; Growney, E.; Nunez, L.; Kaminski, M.

1998-01-01

This progress report focuses on experimental and computational studies used to evaluate nuclear magnetic resonance (NMR) spectroscopy and magnetic resonance imaging (MRI) for detecting, quantifying, and monitoring hydrogen and other magnetically active nuclei ( 3 H, 3 He, 239 Pu, 241 Pu) in Spent nuclear fuels and packaging materials. The detection of moisture by using a toroid cavity NMR imager has been demonstrated in SiO 2 and UO 2 systems. The total moisture was quantified by means of 1 H NMR detection of H 2 O with a sensitivity of 100 ppm. In addition, an MRI technique that was used to determine the moisture distribution also enabled investigators to discriminate between bulk and stationary water sorbed on the particles. This imaging feature is unavailable in any other nondestructive assay (NDA) technique. Following the initial success of this program, the NMR detector volume was scaled up from the original design by a factor of 2000. The capacity of this detector exceeds the size specified by DOE-STD-3013-96

Recent progress in the development of a polarized proton target for reactions with radioactive ion beams

International Nuclear Information System (INIS)

Urrego-Blanco, J.P.; Bingham, C.R.; Brandt, B. van den; Galindo-Uribarri, A.; Gomez del Campo, J.; Hautle, P.; Konter, J.A.; Padilla-Rodal, E.; Schmelzbach, P.A.

2007-01-01

Polarization observables in nuclear reactions with stable beams have provided important information concerning structural properties of nuclei and reaction mechanisms and hold great promise in the context of exotic nuclei. We report on the development of a polarized target based on plastic foils of 20-200 μm thickness to be used with radioactive ion beams. The operation of such a target requires a moderately high magnetic field and very low temperatures. The plastic foil is placed inside a chamber attached to the mixing chamber of a 3 He- 4 He dilution refrigerator. Cooling of the foil is achieved via a superfluid film of 4 He that can be supplied through two capillaries. The chamber has two thin, highly uniform silicon nitride windows. An NMR coil is attached to the target to monitor the polarization. Results of a first test to characterize the target system, using the elastic scattering of 38 MeV 12 C by protons in inverse kinematics are presented

Tunable 13C/1H dual channel matching circuit for dynamic nuclear polarization system with cross-polarization

DEFF Research Database (Denmark)

Rybalko, Oleksandr; Bowen, Sean; Zhurbenko, Vitaliy

2016-01-01

In this paper we report initial results of design and practical implementation of tuning and matching circuit to estimate a performance of Dynamic Nuclear Polarization (DNP) at a magnetic field of 6.7 T. It is shown that developed circuit for signal observation is compact, easy to make and provides....... Measurement results with a tuning and matching circuit prototype are presented including obtained spectra (13C and 1H) and estimation of the signal-to-noise ratio....

Measurements of nuclear polarization and nuclear magnetic moment of 170Tm in 170Tm:SrF2 by optical pumping

International Nuclear Information System (INIS)

Shimomura, K.

1988-01-01

Significant nuclear polarization of unstable 170 Tm in Tm 2+ :SrF 2 was for the first time achieved with β-ray radiation detected optical pumping in solids, providing a new powerful method to measure magnetic moments of unstable nuclei. (author)

Polarized proton target with horizontal spin orientation

International Nuclear Information System (INIS)

Bunyatova, Eh.I.; Kiselev, Yu.F.; Kozlenko, N.G.

1988-01-01

Proton target, the polarization vector of which may be arbitrary oriented in horizontal plane relatively to the beam, is developed and tested. 70% value of polarization is obtained. 0.6 K temperature is acquired through 3 He pumping out continuous cycle. 1.2-propylene glycol - Cr(V) was used as working medium. Magnetic system is made in the form of Helmholtz sperconducting coils with working curren close to critical one. Target polarization is measured by NMR technique using original system of proton signal processing

PSYCHE Pure Shift NMR Spectroscopy.

Science.gov (United States)

Foroozandeh, Mohammadali; Morris, Gareth; Nilsson, Mathias

2018-03-13

Broadband homodecoupling techniques in NMR, also known as "pure shift" methods, aim to enhance spectral resolution by suppressing the effects of homonuclear coupling interactions to turn multiplet signals into singlets. Such techniques typically work by selecting a subset of "active" nuclear spins to observe, and selectively inverting the remaining, "passive", spins to reverse the effects of coupling. Pure Shift Yielded by Chirp Excitation (PSYCHE) is one such method; it is relatively recent, but has already been successfully implemented in a range of different NMR experiments. Paradoxically, PSYCHE is one of the trickiest of pure shift NMR techniques to understand but one of the easiest to use. Here we offer some insights into theoretical and practical aspects of the method, and into the effects and importance of the experimental parameters. Some recent improvements that enhance the spectral purity of PSYCHE spectra will be presented, and some experimental frameworks including examples in 1D and 2D NMR spectroscopy, for the implementation of PSYCHE will be introduced. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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)

NMR Phase Noise in Bitter Magnets

Science.gov (United States)

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

2001-02-01

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

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)

Investigating the Hydrolysis Reactions of a Chemical Warfare Agent Surrogate. A Systematic Study using ¹H, ¹³C, ¹⁷O, ¹⁹F, ³¹P, and ³⁵Cl NMR Spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Alam, Todd M. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Wilson, Brendan W. [West Virginia Univ., Morgantown, WV (United States)

2015-07-24

During the summer of 2015, I participated in the DHS HS-STEM fellowship at Sandia National Laboratories (SNL, NM) under the supervision of Dr. Todd M. Alam in his Nuclear Magnetic Resonance (NMR) Spectroscopy research group. While with the group, my main project involved pursing various hydrolysis reactions with Diethyl Chlorophosphate (DECP), a surrogate for the agent Sarin (GB). Specifically, I performed different hydrolysis reactions, monitored and tracked the different phosphorous containing species using phosphorous (³¹P) NMR spectroscopy. With the data collected, I performed kinetics studies mapping the rates of DECP hydrolysis. I also used the NMR of different nuclei such as ¹H, ¹³C, ¹⁷O, and ³⁵Cl to help understand the complexity of the reactions that take place. Finally, my last task at SNL was to work with Insensitive Nuclei Enhanced by Polarization Transfer (INEPT) NMR Spectroscopy optimizing conditions for ¹⁹F- ³¹P filtering NMR experiments.

Bayesian Peak Picking for NMR Spectra

KAUST Repository

Cheng, Yichen

2014-02-01

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

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

Structural biology by NMR: structure, dynamics, and interactions.

Directory of Open Access Journals (Sweden)

Phineus R L Markwick

2008-09-01

Full Text Available The function of bio-macromolecules is determined by both their 3D structure and conformational dynamics. These molecules are inherently flexible systems displaying a broad range of dynamics on time-scales from picoseconds to seconds. Nuclear Magnetic Resonance (NMR spectroscopy has emerged as the method of choice for studying both protein structure and dynamics in solution. Typically, NMR experiments are sensitive both to structural features and to dynamics, and hence the measured data contain information on both. Despite major progress in both experimental approaches and computational methods, obtaining a consistent view of structure and dynamics from experimental NMR data remains a challenge. Molecular dynamics simulations have emerged as an indispensable tool in the analysis of NMR data.

Physical processes in spin polarized plasmas

International Nuclear Information System (INIS)

Kulsrud, R.M.; Valeo, E.J.; Cowley, S.

1984-05-01

If the plasma in a nuclear fusion reactor is polarized, the nuclear reactions are modified in such a way as to enhance the reactor performance. We calculate in detail the modification of these nuclear reactions by different modes of polarization of the nuclear fuel. We also consider in detail the various physical processes that can lead to depolarization and show that they are by and large slow enough that a high degree of polarization can be maintained

Nontargeted nuclear magnetic resonance (NMR) analysis to detect hazardous substances including methanol in unrecorded alcohol from Novosibirsk, Russia

OpenAIRE

Hausler, Thomas; Okaru,  Alex O.; Neufeld, Maria; Rehm, Jürgen; Kuballa, Thomas; Luy, Burkhard; Lachenmeier, Dirk W.

2016-01-01

Nuclear magnetic resonance (NMR) spectroscopy was applied to the analysis of alcoholic products in the context of health and safety control. A total of 86 samples of unrecorded alcohol were collected in Novosibirsk and nearby cities in Russia. Sampling was based on interviews with alcohol dependent patients, and unrecorded alcohol thus defined included illegally or informally produced alcoholic products (e.g., counterfeit or home-made alcoholic beverages) or surrogate alcohol in the form of c...

Dynamic nuclear polarization and optimal control spatial-selective 13C MRI and MRS

DEFF Research Database (Denmark)

Vinding, Mads Sloth; Laustsen, Christoffer; Maximov, Ivan I.

2013-01-01

. This is achieved through the development of spatial-selective single-shot spiral-readout MRI and MRS experiments combined with dynamic nuclear polarization hyperpolarized [1-13C]pyruvate on a 4.7T pre-clinical MR scanner. The method stands out from related techniques by facilitating anatomic shaped region...

Nuclear magnetic and electric dipole moments of neon-19

International Nuclear Information System (INIS)

MacArthur, D.W.

1983-01-01

This thesis presents a detailed discussion of a series of experiments designed to measure the magnetic and electric dipole moments of the β-emitting nucleus 19 Ne. The 19 Ne is generated in the reaction 19 F(p,n) 19 Ne and is polarized by a ''stern-Gerlach'' magnet in a rare gas atomic beams machine. The atoms are stored in a cell for many seconds without depolarizing. The parity violating asymmetry in the β angular distribution is used to monitor the nuclear polarization. The polarized atoms are stored in a cell in a uniform magnetic field. The β-asymmetry is monitored by a pair of β-detectors located on either side of the cell. Transitions between the M/sub J/ = +1/2 and M/sub J/ = -1/2 spin states are induced by an rf field generated by a small Helmholtz coil pair surrounding the cell. Nuclear magnetic resonance lines are observed and the magnetic moment of 19 Ne measured to be μ( 19 Ne) = -1.88542(8)μ/sub N/. A new magnet, cell and detectors were designed to give narrow resonance lines. The equipment is described in detail and several resonance line shapes are discussed. The narrowest resonance line achieved with this system was 0.043 Hz FWHM. This width is primarily due to the 19 Ne lifetime. Pulsed NMR lineshapes were also observed. The narrow NMR lines observed in the previous experiment were then used as a probe to look for an electric dipole moment (EDM) in 19 Ne. Any shift in the resonance frequency correlated with changes in an externally applied electric field would be evidence for an EDM. The EDM of the 19 Ne atom was measured to (7.2 +/- 6.2 X 10 -22 e-cm. This experiment and possible improvements are discussed in detail

Kinematic approximation in the theory of stimulated nuclear polarization in radical recombination

International Nuclear Information System (INIS)

Mikhailov, S.A.; Purtov, P.A.

1989-01-01

Within the kinematic approximation, we have developed the theory of stimulated nuclear polarization (SNP) in reactions of geminal recombination of radicals in a strong d.c. magnetic field. We have obtained analytical formulas which are applicable for analysis of SNP effects occurring when the reactions are carried out in nonviscous solutions. The result is represented in the form of integrals with respect to the Green's function determining the kinematics of reagent approach. As an illustration of the proposed theory, we have calculated the polarization of nuclei formed in the reaction products of p-benzoquinone in CD 3 OD and in C 6 D 6 with addition of phenol, and we compare with experiment

Polarity dependent photoisomerization of ether substituted azodyes: Synthesis and photoswitching behavior.

Science.gov (United States)

Gan, Siew Mei; Pearl, Zynia Fernandes; Yuvaraj, A R; Lutfor, M R; Gurumurthy, Hegde

2015-10-05

Two new ether substituted azodyes were synthesized and characterized by different spectral analysis such as (1)H NMR, (13)C NMR, FTIR and UV/Vis. Synthesized compounds were used to study the photoisomerization phenomenon by using UV-Vis spectro-photometer. Interesting polarity dependent effect is observed for the first time on these materials. Trans-cis (E-Z) and cis-trans (Z-E) conversion occurred within 41 s and 445 min, respectively for both the compounds in solutions. Polarizing optical microscopy studies revealed that there is no liquid crystal phase for both the compounds. The dramatic variation in the optical property is speculated to be the polarity of the chemical species. These derivatives are useful to fabricate optical data storage devices. Copyright © 2015 Elsevier B.V. All rights reserved.

Generation of nuclear magnetic resonance images

International Nuclear Information System (INIS)

Beckmann, N.X.

1986-01-01

Two generation techniques of nuclear magnetic resonance images, the retro-projection and the direct transformation method are studied these techniques are based on the acquisition of NMR signals which phases and frequency components are codified in space by application of magnetic field gradients. The construction of magnet coils is discussed, in particular a suitable magnet geometry with polar pieces and air gap. The obtention of image contrast by T1 and T2 relaxation times reconstructed from generated signals using sequences such as spin-echo, inversion-recovery and stimulated echo, is discussed. The mathematical formalism of matrix solution for Bloch equations is also presented. (M.C.K.)

Comment on "Nuclear genomic sequences reveal that polar bears are an old and distinct bear lineage".

Science.gov (United States)

Nakagome, Shigeki; Mano, Shuhei; Hasegawa, Masami

2013-03-29

Based on nuclear and mitochondrial DNA, Hailer et al. (Reports, 20 April 2012, p. 344) suggested early divergence of polar bears from a common ancestor with brown bears and subsequent introgression. Our population genetic analysis that traces each of the genealogies in the independent nuclear loci does not support the evolutionary model proposed by the authors.

Dynamic nuclear polarization by frequency modulation of a tunable gyrotron of 260GHz.

Science.gov (United States)

Yoon, Dongyoung; Soundararajan, Murari; Cuanillon, Philippe; Braunmueller, Falk; Alberti, Stefano; Ansermet, Jean-Philippe

2016-01-01

An increase in Dynamic Nuclear Polarization (DNP) signal intensity is obtained with a tunable gyrotron producing frequency modulation around 260GHz at power levels less than 1W. The sweep rate of frequency modulation can reach 14kHz, and its amplitude is fixed at 50MHz. In water/glycerol glassy ice doped with 40mM TEMPOL, the relative increase in the DNP enhancement was obtained as a function of frequency-sweep rate for several temperatures. A 68 % increase was obtained at 15K, thus giving a DNP enhancement of about 80. By employing λ/4 and λ/8 polarizer mirrors, we transformed the polarization of the microwave beam from linear to circular, and achieved an increase in the enhancement by a factor of about 66% for a given power. Copyright © 2015 Elsevier Inc. All rights reserved.

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

Spin-polarized 3He nuclear targets and metastable 4He atoms by optical pumping with a tunable, Nd:YAP laser

International Nuclear Information System (INIS)

Bohler, C.L.; Schearer, L.D.; Leduc, M.; Nacher, P.J.; Zachorowski, L.; Milner, R.G.; McKeown, R.D.; Woodward, C.E.

1988-01-01

Several Nd:YAP lasers were constructed which could be broadly tuned in the 1083-nm region which includes the helium 2 3 S-2 3 P transition, using a Lyot filter and thin, uncoated etalons within the laser cavity. 1 W of power could be extracted at 1083 nm through a 1% transmitting output coupler. This laser beam was used to optically pump metastable 4 He and 3 He 2 3 S helium atoms in a weak discharge cell, spin polarizing the metastable ensemble. In a 3 He cell the polarization is transferred to the nuclear spin system. A 3 He target cell at 0.3 Torr was polarized to 52% in a few minutes. We describe the application of this system to the design of polarized targets for experiments in nuclear physics

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.

Nuclear signals in magnetically ordered media

International Nuclear Information System (INIS)

Ignatchenko, V.A.; Tsifrinovich, V.I.

1993-01-01

The book contains a review of theoretical and experimental investigations in the field of nuclear magnetism in magnetically ordered media. The semiclassical theory of nuclear spins motion is developed that takes into consideration three main features of magnetically ordered media: Suhl-Nakamura interaction, quadrupole interaction and microscopic inhomogeneity of nuclear frequencies. The detailed classification of nuclear spin echo signals is given for standard conditions of experiments, when the Suhl-Nakamura interaction is small in comparison with the NMR line width. The extremal states of the electron - nuclear magnetic system are described in detail: the coexistence of NMR and FMR, nuclear ferromagnetism and NMR at fast remagnetization of a ferromagnet. 157 refs., 20 figs

NUCLEON POLARIZATION IN 3-BODY MODELS OF POLARIZED LI-6

NARCIS (Netherlands)

SCHELLINGERHOUT, NW; KOK, LP; COON, SA; ADAM, RM

1993-01-01

Just as He-3 --> can be approximately characterized as a polarized neutron target, polarized Li-6D has been advocated as a good isoscalar nuclear target for the extraction of the polarized gluon content of the nucleon. The original argument rests upon a presumed ''alpha + deuteron'' picture of Li-6,

Development of a micro flow-through cell for high field NMR spectroscopy.

Energy Technology Data Exchange (ETDEWEB)

Alam, Todd Michael; McIntyre, Sarah K.

2011-05-01

A highly transportable micro flow-through detection cell for nuclear magnetic resonance (NMR) spectroscopy has been designed, fabricated and tested. This flow-through cell allows for the direct coupling between liquid chromatography (LC) and gel permeation chromatography (GPC) resulting in the possibility of hyphenated LC-NMR and GPC-NMR. The advantage of the present flow cell design is that it is independent and unconnected to the detection probe electronics, is compatible with existing commercial high resolution NMR probes, and as such can be easily implemented at any NMR facility. Two different volumes were fabricated corresponding to between {approx}3.8 and 10 {micro}L detection volume. Examples of the performance of the cell on different NMR instruments, and using different NMR detection probes were demonstrated.

Ejectile polarization and nuclear orbitals

International Nuclear Information System (INIS)

Ohnishi, A.; Maruyama, T.; Horiuchi, H.

1992-01-01

Ejectile polarization phenomena are studied by the use of 'Quantum Molecular Dynamics plus external mean field' model. It is shown that the far-side contribution increases as the incident energy increases or the target charge decreases. The incident energy and the target dependence of ejectile polarization data is reproduced qualitatively. The near- and far-side contributions themselves are calculated to be almost monotone functions of ejectile momentum as is predicted in a simple projectile fragmentation scheme without the assumption that the linear and angular momentum transfers are negligible, and their statistical average results in various shapes in ejectile polarization

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

Novel NMR tools to study structure and dynamics of biomembranes.

Science.gov (United States)

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

2002-06-01

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

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

Residue specific hydration of primary cell wall potato pectin identified by solid-state 13C single-pulse MAS and CP/MAS NMR spectroscopy

DEFF Research Database (Denmark)

Larsen, Flemming Hofmann; Chrestensen, Inge Byg; Damager, Iben

2011-01-01

Hydration of rhamnogalacturonan-I (RG-I) derived from potato cell wall was analyzed by 13C single-pulse (SP) magic-angle-spinning (MAS) and 13C cross-polarization (CP) MAS nuclear magnetic resonance (NMR) and supported by 2H SP/MAS NMR experiments. The study shows that the arabinan side chains...... hydrate more readily than the galactan side chains and suggests that the overall hydration properties can be controlled by modifying the ratio of these side chains. Enzymatic modification of native (NA) RG-I provided samples with reduced content of arabinan (sample DA), galactan (sample DG), or both side...... chains (sample DB). Results of these samples suggested that hydration properties were determined by the length and character of the side chains. NA and DA exhibited similar hydration characteristics, whereas DG and DB were difficult to hydrate because of the less hydrophilic properties of the rhamnose...

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-06-14

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

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

Fourier transform zero field NMR and NQR

International Nuclear Information System (INIS)

Zax, D.B.

1985-01-01

In many systems the chemical shifts measured by traditional high resolution solid state NMR methods are insufficiently sensitive, or the information contained in the dipole-dipole couplings is more important. In these cases, Fourier transform zero field magnetic resonance may make an important contribution. Zero field NMR and NQR is the subject of this thesis. Chapter I presents the quantum mechanical background and notational formalism for what follows. Chapter II gives a brief review of high resolution magnetic resonance methods, with particular emphasis on techniques applicable to dipole-dipole and quadrupolar couplings. Level crossings between spin-1/2 and quadrupolar spins during demagnetization transfer polarization from high to low λ nuclei. This is the basis of very high sensitivity zero field NQR measurements by field cycling. Chapter III provides a formal presentation of the high resolution Fourier transform zero field NMR method. Theoretical signal functions are calculated for common spin systems, and examples of typical spectra are presented. Chapters IV and V review the experimental progress in zero field NMR of dipole-dipole coupled spin-1/2 nuclei and for quadrupolar spin systems. Variations of the simple experiment describe in earlier chapters that use pulsed dc fields are presented in Chapter VI

NMR characteristics of low-grade glioma. Comparison with CT

Energy Technology Data Exchange (ETDEWEB)

Asato, Reinin; Tokuriki, Yasuhiko; Nakano, Yoshihisa; Itoh, Harumi; Torizuka, Kanji; Ueda, Tohru; Yamashita, Junkoh; Handa, Hajime

1985-08-01

Sixteen low-grade gliomas were evaluated both with nuclear magnetic resonance (NMR) imaging and with computed tomography (CT). In 13 cases (81%), the NMR images were much better in tissue contrast than the contrast-enhanced CT images. The tumors were shown as well-circumscribed oval lesions in the NMR, though they appeared as ill-defined, irregular, low-attenuation areas in the CT. The extent of the lesion, which was supposed to represent the active tumor tissue, was greater in the NMR than in the CT, because NMR tissue parameters (T/sub 1/, T/sub 2/) are more sensitive to pathological changes in brain tissue than is the X-ray attenuation coefficient. Though, in an optic glioma and a brain-stem astrocytoma, the CT with contrast enhancement displayed the contour of the mass as well as did NMR, it was inferior to the NMR in showing the cephalocaudal extension of the tumors. Calcification does not give a proton NMR signal under the present measuring conditions; thus the calcified cystic wall of a hypothalamic astrocytoma was displayed only in the CT images. In conclusion, the NMR imaging was apparently superior to contrast-enhanced CT in demonstrating the lesions due to low-grade glioma.

Long-Lifetime Low-Scatter Neutron Polarization Target

International Nuclear Information System (INIS)

Richardson, Jonathan M.

2004-01-01

Polarized neutrons scattering is an important technology for characterizing magnetic and other materials. Polarized helium three (P-3He) is a novel technology for creating polarized beams and, perhaps more importantly, for the analysis of polarization in highly divergent scattered beams. Analysis of scattered beams requires specialized targets with complex geometries to ensure accurate results. Special materials and handling procedures are required to give the targets a long useful lifetime. In most cases, the targets must be shielded from stray magnetic fields from nearby equipment. SRL has developed and demonstrated hybrid targets made from glass and aluminum. We have also developed and calibrated a low-field NMR system for measuring polarization lifetimes. We have demonstrated that our low-field system is able to measure NMR signals in the presence of conducting (metallic) cell elements. We have also demonstrated a non-magnetic valve that can be used to seal the cells. We feel that these accomplishments in Phase I are sufficient to ensure a successful Phase II program. The commercial market for this technology is solid. There are over nine neutron scattering centers in the US and Canada and over 22 abroad. Currently, the US plans to build a new $1.4B scattering facility called the Spallation Neutron Source (SNS). The technology developed in this project will allow SRL to supply targets to both existing and future facilities. SRL is also involved with the application of P-3He to medical imaging

High resolution NMR theory and chemical applications

CERN Document Server

Becker, Edwin D

2012-01-01

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

ECG gated NMR-CT for cardiovascular diseases

International Nuclear Information System (INIS)

Nishikawa, J.; Machida, K.; Iio, M.; Yoshimoto, N.; Sugimoto, T.; Kawaguchi, H.; Mano, H.

1984-01-01

The authors applied NMR-CT to cardiac study with ECG gated technique to evaluate the left ventricular (LV) function and compared it with cardiovascular nuclear medicine study (NM). The NMR-CT machine has resistive air-core magnet with 0.15 Tesla. The saturation recovery image or inversion recovery image were obtained as 256 x 256 matrix and 15 mm in thickness. The study population was ten patients who were evaluated both by NMR image and by NM performed within one week interval. The heart muscle was able to be visualized without any contrast material nor radioisotopes in inversion recovery images, whereas saturation recovery images failed to separate heart muscle from blood pool. The wall motions of LV in both methods were well correlated except for inferior wall. The values of ejection fraction in NMR image were moderately low, but two modalities showed satisfactory correlation (r=0.85). The region of myocardial infarction was revealed as wall thinning and/or wall motion abnormality. It is still preliminary to draw a conclusion, however, it can be said that in the evaluation of LV function, method by NMR might be of equal value to those of NM. It can be certain that eventually gated NMR-CT will become more effective method for various aspects of cardiovascular evaluation

Evaluation of PHB nanocomposite by low field NMR

International Nuclear Information System (INIS)

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

2009-01-01

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

TG/DTG, FT-ICR Mass Spectrometry, and NMR Spectroscopy Study of Heavy Fuel Oil

KAUST Repository

Elbaz, Ayman M.; Abdul Jameel, Abdul Gani; Hourani, Nadim; Emwas, Abdul-Hamid M.; Sarathy, Mani; Roberts, William L.

2015-01-01

infusion atmospheric pressure chemical ionization Fourier transform ion cyclotron resonance mass spectrometry (APCI-FTICR MS), high resolution 1H nuclear magnetic resonance (NMR), 13C NMR, and two-dimensional heteronuclear multiple bond correlation (HMBC

PVT Degradation Studies: NMR Analysis

Energy Technology Data Exchange (ETDEWEB)

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

2017-06-06

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

NMR-based stable isotope resolved metabolomics in systems biochemistry

International Nuclear Information System (INIS)

Fan, Teresa W-M.; Lane, Andrew N.

2011-01-01

An important goal of metabolomics is to characterize the changes in metabolic networks in cells or various tissues of an organism in response to external perturbations or pathologies. The profiling of metabolites and their steady state concentrations does not directly provide information regarding the architecture and fluxes through metabolic networks. This requires tracer approaches. NMR is especially powerful as it can be used not only to identify and quantify metabolites in an unfractionated mixture such as biofluids or crude cell/tissue extracts, but also determine the positional isotopomer distributions of metabolites derived from a precursor enriched in stable isotopes such as 13 C and 15 N via metabolic transformations. In this article we demonstrate the application of a variety of 2-D NMR editing experiments to define the positional isotopomers of compounds present in polar and non-polar extracts of human lung cancer cells grown in either [U– 13 C]-glucose or [U– 13 C, 15 N]-glutamine as source tracers. The information provided by such experiments enabled unambiguous reconstruction of metabolic pathways, which is the foundation for further metabolic flux modeling.

An extrapolation scheme for solid-state NMR chemical shift calculations

Science.gov (United States)

Nakajima, Takahito

2017-06-01

Conventional quantum chemical and solid-state physical approaches include several problems to accurately calculate solid-state nuclear magnetic resonance (NMR) properties. We propose a reliable computational scheme for solid-state NMR chemical shifts using an extrapolation scheme that retains the advantages of these approaches but reduces their disadvantages. Our scheme can satisfactorily yield solid-state NMR magnetic shielding constants. The estimated values have only a small dependence on the low-level density functional theory calculation with the extrapolation scheme. Thus, our approach is efficient because the rough calculation can be performed in the extrapolation scheme.

Time reversal tests in polarized neutron reactions

International Nuclear Information System (INIS)

Asahi, Koichiro; Bowman, J.D.; Crawford, B.

1998-01-01

This is the final report of a three-year, Laboratory-Directed Research and Development (LDRD) project at the Los Alamos National Laboratory (LANL). In recent years the nuclear weak interaction has been studied in the compound nucleus via parity violation. The observed parity-violating effects are strongly enhanced by nuclear structure. The predictions are that the interaction of polarized neutrons with polarized nuclear targets could be also used to perform sensitive tests of time-reversal-violation because of the nuclear enhancements. The author has designed experiments to search for time-reversal violation in neutron-nucleus interactions. He has also developed techniques to polarize neutrons with laser-polarized 3 He gas targets. Using the polarized 3 He neutron spin filter, he has performed two experiments at LANSCE: an absolute neutron beam polarization measurement with an accuracy of 0.2--0.3% and a neutron spin-rotation measurement on a 139 La sample

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

Calibration of the Fermilab E-704 polarized target

International Nuclear Information System (INIS)

Hill, D.A.

1992-01-01

This report lists the final, best estimate of the target polarization P T as a function of time for all of the periods during which scattering data were (or may have been) collected. The information under ''RUN'' refers to Δσ L -runs. The notation ''sfs'' stands for ''start of frozen spin,'' ''efs'' for ''end of frozen spin,'' ''→ la'' for ''go to large-aperture'' target magnet position, and ''nla'' for ''not large-aperture'' position, i.e., the target magnet is in ''polarizing'' position. Where the ''NOTE'' column is blank it means that all standard frozen-spin conditions were in effect: the target temperature was reduced and the magnet was in large-aperture position. The timing marks were developed on the basis of three criteria: (1) the availability of direct NMR data, (2) the inclusion of major Target and Run boundaries, and (3) the arbitrary inclusion of enough ''minor'' Run boundaries to shorten large timing gaps. The sign of the P T -values is given in the NMR convention: (+) corresponds to predominant occupation of the Zeeman ground state (the ''thermal'' NMR-signals are considered positive). Since the target magnet field pointed upstream, (+) corresponds to target spin antiparallel to the beam momentum. The estimated uncertainty on P T is ±6.5% (2σ), and the estimated uncertainty on the ratio of values for the two signs of polarization, P T (+)/PT(-), is ±4.3% (2σ)

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.

Polarimetry of the polarized hydrogen deuteride HDice target under an electron beam

Energy Technology Data Exchange (ETDEWEB)

Laine, Vivien E. [Blaise Pascal Univ., Aubiere (France)

2013-10-01

The study of the nucleon structure has been a major research focus in fundamental physics in the past decades and still is the main research line of the Thomas Jefferson National Accelerator Facility (Jefferson Lab). For this purpose and to obtain statistically meaningful results, having both a polarized beam and a highly efficient polarized target is essential. For the target, this means high polarization and high relative density of polarized material. A Hydrogen Deuteride (HD) target that presents both such characteristics has been developed first at Brookhaven National Lab (BNL) and brought to the Hall B of Jefferson Lab in 2008. The HD target has been shown to work successfully under a high intensity photon beam (BNL and Jefferson Lab). However, it remained to be seen if the target could stand an electron beam of reasonably high current (nA). In this perspective, the target was tested for the first time in its frozen spin mode under an electron beam at Jefferson Lab in 2012 during the g14 experiment. This dissertation presents the principles and usage procedures of this HD target. The polarimetry of this target with Nuclear Magnetic Resonance (NMR) during the electron beam tests is also discussed. In addition, this dissertation also describes another way to perform target polarimetry with the elastic scattering of electrons off a polarized target by using data taken on helium-3 during the E97-110 experiment that occurred in Jefferson Lab's Hall A in 2003.

Dynamic nuclear polarization at high Landau levels in a quantum point contact

Science.gov (United States)

Fauzi, M. H.; Noorhidayati, A.; Sahdan, M. F.; Sato, K.; Nagase, K.; Hirayama, Y.

2018-05-01

We demonstrate a way to polarize and detect nuclear spin in a gate-defined quantum point contact operating at high Landau levels. Resistively detected nuclear magnetic resonance (RDNMR) can be achieved up to the fifth Landau level and at a magnetic field lower than 1 T. We are able to retain the RDNMR signals in a condition where the spin degeneracy of the first one-dimensional (1D) subband is still preserved. Furthermore, the effects of orbital motion on the first 1D subband can be made smaller than those due to electrostatic confinement. This developed RDNMR technique is a promising means to study electronic states in a quantum point contact near zero magnetic field.

Electron spin resonance and its implication on the maximum nuclear polarization of deuterated solid target materials

International Nuclear Information System (INIS)

Heckmann, J.; Meyer, W.; Radtke, E.; Reicherz, G.; Goertz, S.

2006-01-01

ESR spectroscopy is an important tool in polarized solid target material research, since it allows us to study the paramagnetic centers, which are used for the dynamic nuclear polarization (DNP). The polarization behavior of the different target materials is strongly affected by the properties of these centers, which are added to the diamagnetic materials by chemical doping or irradiation. In particular, the ESR linewidth of the paramagnetic centers is a very important parameter, especially concerning the deuterated target materials. In this paper, the results of the first precise ESR measurements of the deuterated target materials at a DNP-relevant magnetic field of 2.5 T are presented. Moreover, these results allowed us to experimentally study the correlation between ESR linewidth and maximum deuteron polarization, as given by the spin-temperature theory

Advances in solid-state NMR of cellulose.

Science.gov (United States)

Foston, Marcus

2014-06-01

Nuclear magnetic resonance (NMR) spectroscopy is a well-established analytical and enabling technology in biofuel research. Over the past few decades, lignocellulosic biomass and its conversion to supplement or displace non-renewable feedstocks has attracted increasing interest. The application of solid-state NMR spectroscopy has long been seen as an important tool in the study of cellulose and lignocellulose structure, biosynthesis, and deconstruction, especially considering the limited number of effective solvent systems and the significance of plant cell wall three-dimensional microstructure and component interaction to conversion yield and rate profiles. This article reviews common and recent applications of solid-state NMR spectroscopy methods that provide insight into the structural and dynamic processes of cellulose that control bulk properties and biofuel conversion. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

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...

Application of Solution NMR Spectroscopy to Study Protein Dynamics

Directory of Open Access Journals (Sweden)

Christoph Göbl

2012-03-01

Full Text Available Recent advances in spectroscopic methods allow the identification of minute fluctuations in a protein structure. These dynamic properties have been identified as keys to some biological processes. The consequences of this structural flexibility can be far‑reaching and they add a new dimension to the structure-function relationship of biomolecules. Nuclear Magnetic Resonance (NMR spectroscopy allows the study of structure as well as dynamics of biomolecules in a very broad range of timescales at atomic level. A number of new NMR methods have been developed recently to allow the measurements of time scales and spatial fluctuations, which in turn provide the thermodynamics associated with the biological processes. Since NMR parameters reflect ensemble measurements, structural ensemble approaches in analyzing NMR data have also been developed. These new methods in some instances can even highlight previously hidden conformational features of the biomolecules. In this review we describe several solution NMR methods to study protein dynamics and discuss their impact on important biological processes.

NMR espectroscopic parameters of HX and Si (Sn)X4 (X = H, F, Cl, Br and I) and SnBr4−nIn model compounds

International Nuclear Information System (INIS)

Maldonado, Alejandro F.; Gimenez, Carlos A.; Aucar, Gustavo A.

2012-01-01

Graphical abstract: Optimized fully relativistic calculations of NMR J-couplings (HBr, HI), chemical shifts (Si, Sn) and absolute shielding for reference compounds of heavy atoms (Si, Sn) are given. Highlights: ► In this article we show a procedure to get accurate NMR σ Ref of Si and Sn. ► Calculations of σ on more than three heavy-atom-containing molecules are given. ► Our results are closer to δ exp than previous calculations for SnX 4 (X = H, Cl, Br, I). ► Optimized basis sets were considered for full R and NR calculations of NMR J and σ. ► Relativistic effects enlarge electron correlation effects on J-couplings. - Abstract: The NMR spectroscopic parameters are largely influenced by relativistic effects. They are highly dependent on the electronic behavior inside the spatial regions occupied by nuclei. Full relativistic calculations of indirect nuclear spin–spin couplings at random phase level of approach (RPA) in the title compounds with reoptimized Dyall cVTZ basis sets are given. A comparison with the results of calculations with other basis sets that are mostly used within the non-relativistic (NR) domain is presented. We analyzed the dependence of that couplings with the speed of light over the whole range of values, from the full relativistic to the NR regimes. Within this last regime, calculations at the second-order level of approach (SOPPA) indicated that electron correlation effects may not be as important for nuclear magnetic shieldings, but they must be included with care for J-coupling calculations. From these calculations, we determined that relativity enlarges the electron correlation effects of the J-couplings of HBr and HI. Because the results of nuclear magnetic shielding calculations within polarization propagators at the RPA level were reliable, we were able to show a new and easy procedure to obtain absolute nuclear magnetic shieldings on reference compounds for both Si and Sn nuclei: σ[Si (CH 3 ) 4 ] = 421.28 ± 29.33 ppm

Joint inversion of NMR and SIP data to estimate pore size distribution of geomaterials

Science.gov (United States)

Niu, Qifei; Zhang, Chi

2018-03-01

There are growing interests in using geophysical tools to characterize the microstructure of geomaterials because of the non-invasive nature and the applicability in field. In these applications, multiple types of geophysical data sets are usually processed separately, which may be inadequate to constrain the key feature of target variables. Therefore, simultaneous processing of multiple data sets could potentially improve the resolution. In this study, we propose a method to estimate pore size distribution by joint inversion of nuclear magnetic resonance (NMR) T2 relaxation and spectral induced polarization (SIP) spectra. The petrophysical relation between NMR T2 relaxation time and SIP relaxation time is incorporated in a nonlinear least squares problem formulation, which is solved using Gauss-Newton method. The joint inversion scheme is applied to a synthetic sample and a Berea sandstone sample. The jointly estimated pore size distributions are very close to the true model and results from other experimental method. Even when the knowledge of the petrophysical models of the sample is incomplete, the joint inversion can still capture the main features of the pore size distribution of the samples, including the general shape and relative peak positions of the distribution curves. It is also found from the numerical example that the surface relaxivity of the sample could be extracted with the joint inversion of NMR and SIP data if the diffusion coefficient of the ions in the electrical double layer is known. Comparing to individual inversions, the joint inversion could improve the resolution of the estimated pore size distribution because of the addition of extra data sets. The proposed approach might constitute a first step towards a comprehensive joint inversion that can extract the full pore geometry information of a geomaterial from NMR and SIP data.

Polarized secondary radioactive beams

International Nuclear Information System (INIS)

Zaika, N.I.

1992-01-01

Three methods of polarized radioactive nuclei beam production: a) a method nuclear interaction of the non-polarized or polarized charged projectiles with target nuclei; b) a method of polarization of stopped reaction radioactive products in a special polarized ion source with than following acceleration; c) a polarization of radioactive nuclei circulating in a storage ring are considered. Possible life times of the radioactive ions for these methods are determined. General schemes of the polarization method realizations and depolarization problems are discussed

Heteronuclear cross-polarization in multinuclear multidimensional NMR: Prospects for triple-resonance CP

Energy Technology Data Exchange (ETDEWEB)

Majumdar, A.; Zuiderweg, E.R.P. [Univ. of Michigan, Ann Arbor, MI (United States)

1994-12-01

Heteronuclear multiple-pulse-based Cross Polarization (HECP) between scalar coupled spins is gaining an important role in high-resolution multidimensional NMR of isotopically labeled biomolecules, especially in experiments involving net magnetization transfer. It has generally been observed that in these situations, the performance of HECP is superior to that of INEPT-based sequences. In particular, HECP-based three-dimensional HCCH spectroscopy is more efficient than the INEPT version of the same experiment. Differences in sensitivity have been intuitively attributed to relaxation effects and technical factors such as radiofrequency (rf) inhomogeneity We present theoretical analyses and computer simulations to probe the effects of these factors. Relaxation effects were treated phenomenologically; we found that relaxation differences are relatively small (up to 25%) between pulsed-free-precession (INEPT) and HECP-although always in favor of HECP. We explored the rf effects by employing a Gaussian distribution of rf amplitude over sample volume. We found that inhomogeneity effects significantly favor HECP over INEPT, especially under conditions of {open_quotes}matched {close_quotes} inhomogeneity in the two rf coils. The differences in favor of HECP indicate that an extension of HECP to triple resonance experiments (TRCP) in I -> S -> Q net transfers might yield better results relative to analogous INEPT-based net transfers. We theoretically analyze the possibilities of TRCP and find that transfer functions are critically dependent on the ratio J{sub IS}/J{sub SQ}. When J{sub IS} equals J{sub SQ}, we find that 100% transfer is possible for truly simultaneous TRCP and this transfer is obtained in a time 1.41 /J. The TRCP time requirement compares favorably with optimally concatenated INEPT-transfers, where net transfer I -> S -> Q is complete at 1.5 /J.

'In vivo' and high resolution spectroscopy in solids by NMR: an instrument for transgenic plants study

International Nuclear Information System (INIS)

Colnago, L.A.; Herrmann, P.S.P.; Bernardes Filho, R.

1995-01-01

This work has developed a study on transgenic plants using two different techniques of nuclear magnetic resonance, in vivo NMR and high resolution NMR. In order to understand the gene mutations and characterize the plants constituents, NMR spectral data were analysed and discussed, then the results were presented

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

Correlated calculations of indirect nuclear spin-spin coupling constants using second-order polarization propagator approximations: SOPPA and SOPPA(CCSD)

DEFF Research Database (Denmark)

Enevoldsen, Thomas; Oddershede, Jens; Sauer, Stephan P. A.

1998-01-01

We present correlated calculations of the indirect nuclear spin-spin coupling constants of HD, HF, H2O, CH4, C2H2, BH, AlH, CO and N2 at the level of the second-order polarization propagator approximation (SOPPA) and the second-order polarization propagator approximation with coupled-cluster sing...

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.

The microwave heating mechanism of N-(4-methoxybenzyliden)-4-butylaniline in liquid crystalline and isotropic phases as determined using in situ microwave irradiation NMR spectroscopy.

Science.gov (United States)

Tasei, Yugo; Tanigawa, Fumikazu; Kawamura, Izuru; Fujito, Teruaki; Sato, Motoyasu; Naito, Akira

2015-04-14

Microwave heating effects are widely used in the acceleration of organic, polymerization and enzymatic reactions. These effects are primarily caused by the local heating induced by microwave irradiation. However, the detailed molecular mechanisms associated with microwave heating effects on the chemical reactions are not yet well understood. This study investigated the microwave heating effect of N-(4-methoxybenzylidene)-4-butylaniline (MBBA) in liquid crystalline and isotropic phases using in situ microwave irradiation nuclear magnetic resonance (NMR) spectroscopy, by obtaining (1)H NMR spectra of MBBA under microwave irradiation. When heated simply using the temperature control unit of the NMR instrument, the liquid crystalline MBBA was converted to the isotropic phase exactly at its phase transition temperature (Tc) of 41 °C. The application of microwave irradiation at 130 W for 90 s while maintaining the instrument temperature at 20 °C generated a small amount of isotropic phase within the bulk liquid crystal. The sample temperature of the liquid crystalline state obtained during microwave irradiation was estimated to be 35 °C by assessing the linewidths of the (1)H NMR spectrum. This partial transition to the isotropic phase can be attributed to a non-equilibrium local heating state induced by the microwave irradiation. The application of microwave at 195 W for 5 min to isotropic MBBA while maintaining an instrument temperature of 50 °C raised the sample temperature to 160 °C. In this study, the MBBA temperature during microwave irradiation was estimated by measuring the temperature dependent chemical shifts of individual protons in the sample, and the different protons were found to indicate significantly different temperatures in the molecule. These results suggest that microwave heating polarizes bonds in polar functional groups, and this effect may partly explain the attendant acceleration of organic reactions.

Climate Drives Polar Bear Origins

Science.gov (United States)

In their provocative analysis of northern bears (“Nuclear genomic sequences reveal that polar bears are an old and distinct bear lineage,” Reports, 20 April, p. 344), F. Hailer et al. use independent nuclear loci to show that polar bears originated during the middle Pleistocene, rather than during t...

Broadband cross-polarization-based heteronuclear dipolar recoupling for structural and dynamic NMR studies of rigid and soft solids

International Nuclear Information System (INIS)

Kharkov, B. B.; Chizhik, V. I.; Dvinskikh, S. V.

2016-01-01

Dipolar recoupling is an essential part of current solid-state NMR methodology for probing atomic-resolution structure and dynamics in solids and soft matter. Recently described magic-echo amplitude- and phase-modulated cross-polarization heteronuclear recoupling strategy aims at efficient and robust recoupling in the entire range of coupling constants both in rigid and highly dynamic molecules. In the present study, the properties of this recoupling technique are investigated by theoretical analysis, spin-dynamics simulation, and experimentally. The resonance conditions and the efficiency of suppressing the rf field errors are examined and compared to those for other recoupling sequences based on similar principles. The experimental data obtained in a variety of rigid and soft solids illustrate the scope of the method and corroborate the results of analytical and numerical calculations. The technique benefits from the dipolar resolution over a wider range of coupling constants compared to that in other state-of-the-art methods and thus is advantageous in studies of complex solids with a broad range of dynamic processes and molecular mobility degrees

Magnetization-dependent viscosity in brute-force-polarized liquid 3He

DEFF Research Database (Denmark)

Vermeulen, G.A.; Schuhl, A.; Joffrin, J.

1988-01-01

A new method to measure the magnetization dependence of the viscosity in polarized liquid He3 is presented. The magnetization is obtained by "brute-force polarization" at 45 mK in magnetic fields up to 11 T; it is subsequently destroyed by saturation of the NMR signal. Our result, a relative...... increase of the viscosity of (31.5)×10-3 at 3.9% polarization and a pressure of 30 bars, disagrees with a prediction based on the "nearly metamagnetic" model....

Indirect detection in solid state NMR: An illustrious history and a bright future

Science.gov (United States)

Tycko, Robert

2018-03-01

Many of us have a love/hate relationship with nuclear magnetic resonance (NMR). We love the information content of NMR data, which provides us with essential information about structure, dynamics, and material properties that is not available from any other measurement, and we love the fact that NMR methods can be applied to almost any problem in almost any area of science. But we hate the low sensitivity of NMR, which forces us to make big samples, spend many tedious hours or days taking data, or live with marginal signal-to-noise.

NMR studies of Na+-anion association effects in polymer electrolytes

International Nuclear Information System (INIS)

Greenbaum, S.G.; Pak, Y.S.; Wintergill, M.C.; Fontanella, J.J.

1988-01-01

23 Na nuclear magnetic resonance (NMR) measurements on poly (propylene oxide) (PPO) and siloxane based polymer electrolytes containing various sodium salts at a single nominal concentration are reported. In addition, differential scanning calorimetry (DSC) and electrical conductivity studies were carried out on the PPO materials. The NMR-determined mobile Na + concentrations and DSC results provide evidence for ionic aggregation effects which, for some samples, result in salt precipitation at elevated temperatures. 23 Na chemical shifts observed in solid state NMR due to mobile Na + -anion interactions influence ionic transport as well as the number of available carriers. (author). 19 refs.; 7 figs

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

Science.gov (United States)

Urbanova, Martina; Sturcova, Adriana; Brus, Jiri; Benes, Hynek; Skorepova, Eliska; Kratochvil, Bohumil; Cejka, Jan; Sedenkova, Ivana; Kobera, Libor; Policianova, Olivia; Sturc, Antonin

2013-04-01

Analysis of C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (NMR), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR), and X-ray powder diffraction data of trospium chloride (TCl) products crystallized from different mixtures of water-ethanol [φ(EtOH) = 0.5-1.0] at various temperatures (0°C, 20°C) and initial concentrations (saturated solution, 30%-50% excess of solvent) revealed extensive structural variability of TCl. Although (13) C CP/MAS NMR spectra indicated broad variety of structural phases arising from molecular disorder, temperature-modulated DSC identified presence of two distinct components in the products. FTIR spectra revealed alterations in the hydrogen bonding network (ionic hydrogen bond formation), whereas the X-ray diffraction reflected unchanged unit cell parameters. These results were explained by a two-component character of TCl products in which a dominant polymorphic form is accompanied by partly separated nanocrystalline domains of a secondary phase that does not provide clear Bragg reflections. These phases slightly differ in the degree of molecular disorder, in the quality of crystal lattice and hydrogen bonding network. It is also demonstrated that, for the quality control of such complex products, (13) C CP/MAS NMR spectroscopy combined with factor analysis (FA) can satisfactorily be used for categorizing the individual samples: FA of (13) C CP/MAS NMR spectra found clear relationships between the extent of molecular disorder and crystallization conditions. © 2013 Wiley Periodicals, Inc. and the American Pharmacists Association J Pharm Sci 102:1235-1248, 2013. Copyright © 2013 Wiley Periodicals, Inc.

Dynamic nuclear polarization tests in some polymers for polarized targets

International Nuclear Information System (INIS)

Brandt, B. van den; Hautle, P.; Konter, J.A.; Mango, S.; Bunyatova, E.I.

1998-01-01

The results of dynamic polarization tests in polyethylene (PE) and ethylene propylene copolymer (EPC), doped with the stable free radical 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO), are presented. Sizable proton polarizations have been achieved in a magnetic field of 2.5 T at a temperature below 0.3 K and 5T at 1 K

Thermometry of hot spot using NMR for hyperthermia

International Nuclear Information System (INIS)

Amemiya, Yoshifumi; Kamimura, Yoshitsugu

1983-01-01

Lately noticed hyperthermia in cancer therapy requires non-invasive measurement of the temperature at the warmed site in the deep portion of human body. Nuclear magnetic relaxation time of NMR is also usable for cancer diagnosis. For coordination of these two techniques, it was judged suitable to measure temperature by NMR so that cancer diagnosis and treatment and evaluation of therapeutic effect might be incorporated into one system. This report dealt with concrete procedures of measuring the temperature of deep portions by NMR. Computations revealed that the coefficient of temperature of the thermal equilibrium magnetization was useful, that magnetic field focusing was the most effective imaging technique and that temperature rise in areas about 2 cm in radius could be measured without large errors. (Chiba, N.)

Dynamic nuclear polarization of membrane proteins: covalently bound spin-labels at protein–protein interfaces

International Nuclear Information System (INIS)

Wylie, Benjamin J.; Dzikovski, Boris G.; Pawsey, Shane; Caporini, Marc; Rosay, Melanie; Freed, Jack H.; McDermott, Ann E.

2015-01-01

We demonstrate that dynamic nuclear polarization of membrane proteins in lipid bilayers may be achieved using a novel polarizing agent: pairs of spin labels covalently bound to a protein of interest interacting at an intermolecular interaction surface. For gramicidin A, nitroxide tags attached to the N-terminal intermolecular interface region become proximal only when bimolecular channels forms in the membrane. We obtained signal enhancements of sixfold for the dimeric protein. The enhancement effect was comparable to that of a doubly tagged sample of gramicidin C, with intramolecular spin pairs. This approach could be a powerful and selective means for signal enhancement in membrane proteins, and for recognizing intermolecular interfaces

Evaluation of thermoplastic starch/MMT nanocomposites by nuclear magnetic resonance (NMR)

International Nuclear Information System (INIS)

Schlemmer, D.; Rodrigues, Tiago C.A.F.; Resck, I.S.; Sales, M.J.A.

2010-01-01

Starch has been studied for replace petrochemical plastics for short shelf life. However, the starch films have limitations: sensitivity to moisture and poor mechanical strength. This can be improved by incorporating loads such as montmorillonite, forming nanocomposites. Nanocomposites were prepared with 1, 3, 5 and 10% of montmorillonite, using vegetable oils of Brazilian Cerrado as plasticizers. The NMR spectra of oils are similar, but the intensities of the signals varying with the proportion of fatty acids. The molar mass of the oils was also calculated by NMR. The spectrum of CP/MAS 13 C NMR for starch presented a duplet in 97 and 98 ppm, on the amorphous domains of C-1, indicating a crystal type A. The spectra of the nanocomposites are similar to those of starch and oils. No new peaks appear, suggesting that there are no strong chemical bonds between components. (author)

NMR methods for the investigation of structure and transport

Energy Technology Data Exchange (ETDEWEB)

Hardy, Edme H. [Karlsruher Institut fuer Technologie (KIT), Karlsruhe (Germany). Inst. fuer Mechanische Verfahrenstechnik und Mechanik

2012-07-01

Extensive derivations of required fundamental relations for readers with engineering background New applications based on MRI, PGSE-NMR, and low-field NMR New concepts in quantitative data evaluation and image analysis Methods of nuclear magnetic resonance (NMR) are increasingly applied in engineering sciences. The book summarizes research in the field of chemical and process engineering performed at the Karlsruhe Institute of Technology (KIT). Fundamentals of the methods are exposed for readers with an engineering background. Applications cover the fields of mechanical process engineering (filtration, solid-liquid separation, powder mixing, rheometry), chemical process engineering (trickle-bed reactor, ceramic sponges), bioprocess engineering (biofilm growth), and food process engineering (microwave heating, emulsions). Magnetic Resonance Imaging (MRI) as well as low-field NMR are covered with notes on hardware. Emphasis is placed on quantitative data analysis and image processing. (orig.)

NMR methods for the investigation of structure and transport

International Nuclear Information System (INIS)

Hardy, Edme H.

2012-01-01

Extensive derivations of required fundamental relations for readers with engineering background New applications based on MRI, PGSE-NMR, and low-field NMR New concepts in quantitative data evaluation and image analysis Methods of nuclear magnetic resonance (NMR) are increasingly applied in engineering sciences. The book summarizes research in the field of chemical and process engineering performed at the Karlsruhe Institute of Technology (KIT). Fundamentals of the methods are exposed for readers with an engineering background. Applications cover the fields of mechanical process engineering (filtration, solid-liquid separation, powder mixing, rheometry), chemical process engineering (trickle-bed reactor, ceramic sponges), bioprocess engineering (biofilm growth), and food process engineering (microwave heating, emulsions). Magnetic Resonance Imaging (MRI) as well as low-field NMR are covered with notes on hardware. Emphasis is placed on quantitative data analysis and image processing. (orig.)

Nuclear reactivity control using laser induced polarization

International Nuclear Information System (INIS)

Bowman, C.D.

1990-01-01

This patent describes a control element for reactivity control of a fission source provides an atomic density of 3 He in a control volume which is effective to control criticality as the 3 He is spin-polarized. Spin-polarization of the 3 He affects the cross section of the control volume for fission neutrons and hence, the reactivity. An irradiation source is directed within the 3 He for spin-polarizing the 3 He. An alkali-metal vapor may be included with the 3 He where a laser spin-polarizes the alkali-metal atoms which in turn, spin-couple with 3 He to spin-polarize the 3 He atoms

13C-NMR of diterpenes with pimarane skeleton

International Nuclear Information System (INIS)

Garcez, W.S.; Pereira, A.L.; Silva Queiroz, P.P. da; Silva, R.S. da; Valente, L.M.M.; Peixoto, E.M.; Cunha Pinto, A. da

1981-01-01

The effect of substituent groups on the chemical shift of carbons using nuclear magnetic resonance spectra of carbon 13 ( 13 C-NMR) is discussed. Diterpenes having pimarane skeleton, isolated from plants of Velloziaceae family are analysed. (ARHC) [pt

Characterization of bioactive compounds of Annona cherimola L. leaves using a combined approach based on HPLC-ESI-TOF-MS and NMR.

Science.gov (United States)

Díaz-de-Cerio, Elixabet; Aguilera-Saez, Luis Manuel; Gómez-Caravaca, Ana María; Verardo, Vito; Fernández-Gutiérrez, Alberto; Fernández, Ignacio; Arráez-Román, David

2018-06-01

Annona cherimola Mill. (cherimoya) has widely been used as food crop. The leaves of this tree possess several health benefits, which are, in general, attributed mainly to its bioactive composition. However, literature concerning a comprehensive characterization based on a combined approach, which consists of nuclear magnetic resonance (NMR) and high-performance liquid chromatography coupled with time-of-flight mass spectrometry (HPLC-TOF-MS), from these leaves is scarce. Thus, the aim of this work was to study the polar profile of full extracts of cherimoya leaves by using these tools. Thus, a total of 77 compounds have been characterized, 12 of which were identified by both techniques. Briefly, 23 compounds were classified as amino acids, organic acids, carbohydrates, cholines, phenolic acid derivatives, and flavonoids by NMR, while 66 metabolites were divided into sugars, amino acids, phenolic acids and derivatives, flavonoids, phenylpropanoids, and other polar compounds by HPLC-TOF-MS. It is worth mentioning that different solvent mixtures were tested and the total phenolic content in the extracts quantified (TPC via HPLC-TOF-MS). The tendency observed was EtOH/water 80/20 (v/v) (17.0 ± 0.2 mg TPC/g leaf dry weight (d.w.)) ≥ acetone/water 70/30 (v/v) (16.1 ± 0.7 mg TPC/g leaf d.w.) > EtOH/water 70/30 (v/v) (14.0 ± 0.3 mg TPC/g leaf d.w.) > acetone/water 80/20 (v/v) (13.5 ± 0.4 mg TPC/g leaf d.w.). Importantly, flavonoids derivatives were between 63 and 76% of the TPC in those extracts. Major compounds were sucrose, glucose (α and β), and proline, and chlorogenic acid and rutin for NMR and HPLC-TOF-MS, respectively. Graphical abstract The combined use of LC-HRMS and NMR is a potential synergic combination for a comprehensive metabolite composition of cherimoya leaves.

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.

Interactive NMR: A Simulation Based Teaching Tool for Fundamentals to Applications with Tangible Analogies

Science.gov (United States)

Griesse-Nascimento, Sarah; Bridger, Joshua; Brown, Keith; Westervelt, Robert

2011-03-01

Interactive computer simulations increase students' understanding of difficult concepts and their ability to explain complex ideas. We created a module of eight interactive programs and accompanying lesson plans for teaching the fundamental concepts of Nuclear Magnetic Resonance (NMR) and Magnetic Resonance Imaging (MRI) that we call interactive NMR (iNMR). We begin with an analogy between nuclear spins and metronomes to start to build intuition about the dynamics of spins in a magnetic field. We continue to explain T1, T2, and pulse sequences with the metronome analogy. The final three programs are used to introduce and explain the Magnetic Resonance Switch, a recent diagnostic technique based on NMR. A modern relevant application is useful to generate interest in the topic and confidence in the students' ability to apply their knowledge. The iNMR module was incorporated into a high school AP physics class. In a preliminary evaluation of implementation, students expressed enthusiasm and demonstrated enhanced understanding of the material relative to the previous year. Funded by NSF PHY-0646094 grant.

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.

A comparison of chemical shift sensitivity of trifluoromethyl tags: optimizing resolution in {sup 19}F NMR studies of proteins

Energy Technology Data Exchange (ETDEWEB)

Ye, Libin; Larda, Sacha Thierry; Frank Li, Yi Feng [University of Toronto, UTM, Department of Chemistry (Canada); Manglik, Aashish [Stanford University School of Medicine, Department of Molecular and Cellular Physiology (United States); Prosser, R. Scott, E-mail: scott.prosser@utoronto.ca [University of Toronto, UTM, Department of Chemistry (Canada)

2015-05-15

The elucidation of distinct protein conformers or states by fluorine ({sup 19}F) NMR requires fluorinated moieties whose chemical shifts are most sensitive to subtle changes in the local dielectric and magnetic shielding environment. In this study we evaluate the effective chemical shift dispersion of a number of thiol-reactive trifluoromethyl probes [i.e. 2-bromo-N-(4-(trifluoromethyl)phenyl)acetamide (BTFMA), N-(4-bromo-3-(trifluoromethyl)phenyl)acetamide (3-BTFMA), 3-bromo-1,1,1-trifluoropropan-2-ol (BTFP), 1-bromo-3,3,4,4,4-pentafluorobutan-2-one (BPFB), 3-bromo-1,1,1-trifluoropropan-2-one (BTFA), and 2,2,2-trifluoroethyl-1-thiol (TFET)] under conditions of varying polarity. In considering the sensitivity of the {sup 19}F NMR chemical shift to the local environment, a series of methanol/water mixtures were prepared, ranging from relatively non-polar (MeOH:H{sub 2}O = 4) to polar (MeOH:H{sub 2}O = 0.25). {sup 19}F NMR spectra of the tripeptide, glutathione ((2S)-2-amino-4-{[(1R)-1-[(carboxymethyl)carbamoyl] -2-sulfanylethyl]carbamoyl}butanoic acid), conjugated to each of the above trifluoromethyl probes, revealed that the BTFMA tag exhibited a significantly greater range of chemical shift as a function of solvent polarity than did either BTFA or TFET. DFT calculations using the B3LYP hybrid functional and the 6-31G(d,p) basis set, confirmed the observed trend in chemical shift dispersion with solvent polarity.

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.

Search for a nematic phase in the quasi-two-dimensional antiferromagnet CuCrO2 by NMR in an electric field

Science.gov (United States)

Sakhratov, Yu. A.; Kweon, J. J.; Choi, E. S.; Zhou, H. D.; Svistov, L. E.; Reyes, A. P.

2018-03-01

The magnetic phase diagram of CuCrO2 was studied with an alternative method of simultaneous Cu NMR and electric polarization techniques with the primary goal of demonstrating that, regardless of cooling history of the sample, the magnetic phase with specific helmet-shaped NMR spectra associated with interplanar disorder possesses electric polarization. Our result unequivocally confirms the assumption of Sakhratov et al. [Phys. Rev. B 94, 094410 (2016), 10.1103/PhysRevB.94.094410] that the high-field low-temperature phase is in fact a three-dimensional (3D) polar phase characterized by a 3D magnetic order with tensor order parameter. In comparison with the results obtained in pulsed fields, a modified phase diagram is introduced defining the upper boundary of the first-order transition from the 3D spiral to the 3D polar phase.

Quantification of organic acids in beer by nuclear magnetic resonance (NMR)-based methods

International Nuclear Information System (INIS)

Rodrigues, J.E.A.; Erny, G.L.; Barros, A.S.; Esteves, V.I.; Brandao, T.; Ferreira, A.A.; Cabrita, E.; Gil, A.M.

2010-01-01

The organic acids present in beer provide important information on the product's quality and history, determining organoleptic properties and being useful indicators of fermentation performance. NMR spectroscopy may be used for rapid quantification of organic acids in beer and different NMR-based methodologies are hereby compared for the six main acids found in beer (acetic, citric, lactic, malic, pyruvic and succinic). The use of partial least squares (PLS) regression enables faster quantification, compared to traditional integration methods, and the performance of PLS models built using different reference methods (capillary electrophoresis (CE), both with direct and indirect UV detection, and enzymatic essays) was investigated. The best multivariate models were obtained using CE/indirect detection and enzymatic essays as reference and their response was compared with NMR integration, either using an internal reference or an electrical reference signal (Electronic REference To access In vivo Concentrations, ERETIC). NMR integration results generally agree with those obtained by PLS, with some overestimation for malic and pyruvic acids, probably due to peak overlap and subsequent integral errors, and an apparent relative underestimation for citric acid. Overall, these results make the PLS-NMR method an interesting choice for organic acid quantification in beer.

Quantification of organic acids in beer by nuclear magnetic resonance (NMR)-based methods

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, J.E.A. [CICECO-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Erny, G.L. [CESAM - Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Barros, A.S. [QOPNAA-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Esteves, V.I. [CESAM - Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal); Brandao, T.; Ferreira, A.A. [UNICER, Bebidas de Portugal, Leca do Balio, 4466-955 S. Mamede de Infesta (Portugal); Cabrita, E. [Department of Chemistry, New University of Lisbon, 2825-114 Caparica (Portugal); Gil, A.M., E-mail: agil@ua.pt [CICECO-Department of Chemistry, University of Aveiro, Campus de Santiago, 3810-193 Aveiro (Portugal)

2010-08-03

The organic acids present in beer provide important information on the product's quality and history, determining organoleptic properties and being useful indicators of fermentation performance. NMR spectroscopy may be used for rapid quantification of organic acids in beer and different NMR-based methodologies are hereby compared for the six main acids found in beer (acetic, citric, lactic, malic, pyruvic and succinic). The use of partial least squares (PLS) regression enables faster quantification, compared to traditional integration methods, and the performance of PLS models built using different reference methods (capillary electrophoresis (CE), both with direct and indirect UV detection, and enzymatic essays) was investigated. The best multivariate models were obtained using CE/indirect detection and enzymatic essays as reference and their response was compared with NMR integration, either using an internal reference or an electrical reference signal (Electronic REference To access In vivo Concentrations, ERETIC). NMR integration results generally agree with those obtained by PLS, with some overestimation for malic and pyruvic acids, probably due to peak overlap and subsequent integral errors, and an apparent relative underestimation for citric acid. Overall, these results make the PLS-NMR method an interesting choice for organic acid quantification in beer.

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

Science.gov (United States)

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

2004-06-01

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

A nonsense mutation of γD-crystallin associated with congenital nuclear and posterior polar cataract in a Chinese family.

Science.gov (United States)

Zhai, Yi; Li, Jinyu; Zhu, Yanan; Xia, Yan; Wang, Wei; Yu, Yinhui; Yao, Ke

2014-01-01

The goal of this study was to characterize the disease-causing mutations in a Chinese family with congenital nuclear and posterior polar cataracts. Clinical data of patients in the family were recorded using slit-lamp photography and high definition video. Genomic DNA samples were extracted from the peripheral blood of the pedigree members and 100 healthy controls. Mutation screening was performed in the candidate genes by bi-directional sequencing of the amplified products. The congenital cataract phenotype of the pedigree was identified by slit-lamp examinations and observation during surgery as nuclear and posterior polar cataracts. Through the sequencing of the candidate genes, a heterozygous c. 418C>T change was detected in the coding region of the γD-crystallin gene (CRYGD). As a result of this change, a highly conserved arginine residue was replaced by a stop codon (p. R140X). This change was discovered among all of the affected individuals with cataracts, but not among the unaffected family members or the 100 ethnically matched controls. This study identified a novel congenital nuclear and posterior polar cataract phenotype caused by the recurrent mutation p. R140X in CRYGD.

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.

Synthesis and Analysis of Methacryloyl-L-Alanine Methyl Ester using fourier Transform Nuclear Magnetic Resonance

International Nuclear Information System (INIS)

Tri Darwinto

2008-01-01

Methacryloyl-L-alanine methyl ester was synthesized by reacting methacrylic acid with L-alanine methyl ester hydrochloride in triethylamine at temperature of 90 o C. Hydrogel polymer of poly(methacryloyl-L-alanine methyl ester) was much used for diagnosis and therapy of vascular tumor. The molecular structure methacryloyl-L-alanine methyl ester analyzed by fourier transform nuclear magnetic resonance (FT-NMR) for analyzing of carbon atom ( 13 C) using Distortionless Enhancement by Polarization Transfer (DEPT) measurement mode with coupling as well as without coupling from proton atom ( 1 H). Molecular structure analysis result showed that DEPT FT-NMR measurement mode with coupling as well as without coupling from 1 H was very fast, exact and accurate method for molecular analysis of organic compound especially methacryloyl-L-alanine methyl ester. (author)

A novel strategy for NMR resonance assignment and protein structure determination

International Nuclear Information System (INIS)

Lemak, Alexander; Gutmanas, Aleksandras; Chitayat, Seth; Karra, Murthy; Farès, Christophe; Sunnerhagen, Maria; Arrowsmith, Cheryl H.

2011-01-01

The quality of protein structures determined by nuclear magnetic resonance (NMR) spectroscopy is contingent on the number and quality of experimentally-derived resonance assignments, distance and angular restraints. Two key features of protein NMR data have posed challenges for the routine and automated structure determination of small to medium sized proteins; (1) spectral resolution – especially of crowded nuclear Overhauser effect spectroscopy (NOESY) spectra, and (2) the reliance on a continuous network of weak scalar couplings as part of most common assignment protocols. In order to facilitate NMR structure determination, we developed a semi-automated strategy that utilizes non-uniform sampling (NUS) and multidimensional decomposition (MDD) for optimal data collection and processing of selected, high resolution multidimensional NMR experiments, combined it with an ABACUS protocol for sequential and side chain resonance assignments, and streamlined this procedure to execute structure and refinement calculations in CYANA and CNS, respectively. Two graphical user interfaces (GUIs) were developed to facilitate efficient analysis and compilation of the data and to guide automated structure determination. This integrated method was implemented and refined on over 30 high quality structures of proteins ranging from 5.5 to 16.5 kDa in size.

Effects of CO2 injection and Kerogen Maturation on Low-Field Nuclear Magnetic Resonance Response

Science.gov (United States)

Prasad, M.; Livo, K.

2017-12-01

Low-field Nuclear Magnetic Resonance (NMR) is commonly used in petrophysical analysis of petroleum reservoir rocks. NMR experiments record the relaxation and polarization of in-situ hydrogen protons present in gaseous phases such as free-gas intervals and solution gas fluids, bulk fluid phases such as oil and aquifer intervals, and immovable fractions of kerogen and bitumen. Analysis of NMR relaxation spectra is performed to record how fluid composition, maturity, and viscosity change NMR experimental results. We present T1-T2 maps as thermal maturity of a water-saturated, sub-mature Woodford shale is increased at temperatures from 125 to 400 degrees Celsius. Experiments with applied fluid pressure in paraffinic mineral oil and DI water with varying fluid pH have been performed to mimic reservoir conditions in analysis of the relaxation of bulk fluid phases. We have recorded NMR spectra, T1-T2 maps, and fluid diffusion coefficients using a low-field (2 MHz) MagritekTM NMR. CO2 was injected at a pressure of 900 psi in an in house developed NMR pressure vessel made of torlon plastic. Observable 2D NMR shifts in immature kerogen formations as thermal maturity is increased show generation of lighter oils with increased maturity. CO2 injection leads to a decrease in bulk fluid relaxation time that is attributed to viscosity modification with gas presence. pH variation with increased CO2 presence were shown to not effect NMR spectra. From this, fluid properties have been shown to greatly affect NMR readings and must be taken into account for more accurate NMR reservoir characterization.

Solvent polarity controls the helical conformation of short peptides rich in Calpha-tetrasubstituted amino acids.

Science.gov (United States)

Bellanda, Massimo; Mammi, Stefano; Geremia, Silvano; Demitri, Nicola; Randaccio, Lucio; Broxterman, Quirinus B; Kaptein, Bernard; Pengo, Paolo; Pasquato, Lucia; Scrimin, Paolo

2007-01-01

The two peptides, rich in C(alpha)-tetrasubstituted amino acids, Ac-[Aib-L-(alphaMe)Val-Aib](2)-L-His-NH(2) (1) and Ac-[Aib-L-(alphaMe)Val-Aib](2)-O-tBu (2 a) are prevalently helical. They present the unique property of changing their conformation from the alpha- to the 3(10)-helix as a function of the polarity of the solvent: alpha in more polar solvents, 3(10) in less polar ones. Conclusive evidence of this reversible change of conformation is reported on the basis of the circular dichroism (CD) spectra and a detailed two-dimensional NMR analysis in two solvents (trifluoroethanol and methanol) refined with molecular dynamics calculations. The X-ray diffractometric analysis of the crystals of both peptides reveals that they assume a prevalent 3(10)-helix conformation in the solid state. This conformation is practically superimposable on that obtained from the NMR analysis of 1 in methanol. The NMR results further validate the reported CD signature of the 3(10)-helix and the use of the CD technique for its assessment.

A metal-ion NMR investigation of the antibiotic facilitated transport of monovalent cations through the walls of phospholipid vesicles. II. Sulfur-33 NMR

International Nuclear Information System (INIS)

Buster, D.C.

1988-01-01

A technique has been developed to investigate the antibiotic facilitated transmembrane transport of monovalent cations using 23 Na and 7 Li Nuclear Magnetic Resonance spectroscopy. The initial portion of this thesis outlines the production and characterization of a model lipid system amenable to the NMR detection of cation transport. Large unilamellar vesicles (LUV) have been prepared from a 4:1 mixture of phosphatidylcholine and phosphatidylglycerol. The presence of the anionic chemical shift reagent dysprosium (III) tripolyphosphate, either inside or outside of the vesicles, allows for the spectroscopic separation of the NMR resonances arising from the inter- and extravesicular cation pools. The cation transporting properties of the channel-forming pentadecapeptide, gramicidin D, have been studied using the NMR technique

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.

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

NMR study of the interactions of polymyxin B, gramicidin S, and valinomycin with dimyristoyllecithin bilayers

International Nuclear Information System (INIS)