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Sample records for 19f nuclear magnetic

  1. Xenobiotic Monitoring in Plants by 19F and 1H Nuclear Magnetic Resonance Imaging and Spectroscopy

    PubMed Central

    Rollins, Andrew; Barber, Jill; Elliott, Raymond; Wood, Brian

    1989-01-01

    19F and 1H nuclear magnetic resonance imaging and spectroscopy have been used to monitor the uptake of trifluoroacetic acid in stems and leaves of Lycopersicon esculentum. The movement and location of a xenobiotic have been demonstrated in vivo by a noninvasive technique. Images Figure 5 PMID:16667169

  2. Xenobiotic monitoring in plants by sup 19 F and sup 1 H nuclear magnetic resonance imaging and spectroscopy

    SciTech Connect

    Rollins, A.; Barber, J.; Wood, B. ); Elliott, R. )

    1989-12-01

    {sup 19}F and {sup 1}H nuclear magnetic resonance imaging and spectroscopy have been used to monitor the uptake of trifluoroacetic acid in stems and leaves of Lycopersicon esculentum. The movement and location of a xenobiotic have been demonstrated in vivo by a noninvasive technique.

  3. 19F-nuclear magnetic resonance: measurements of [O2] and pH in biological systems.

    PubMed Central

    Taylor, J; Deutsch, C

    1988-01-01

    19F-nuclear magnetic resonance (NMR) has been used to determine both intracellular pH and oxygen concentrations in cell suspensions. Oxygen concentrations in Paracoccus denitrificans and insulinoma cells, RINm5F, in the NMR probe can be monitored directly by 1/T1 measurements of perfluorotripropylamine (FTPA)/lecithin emulsion added to the suspensions. With FTPA oxygen monitoring, we investigated the relative aeration capabilities of two types of NMR chambers. Both normal and transformed eucaryotic cells can be maintained in either chamber for at least 1-2 h at cytocrits of up to 20-25%, with 30% oxygen saturation and cell viabilities of 90-95%. Similar concentrations of procaryotes were maintained aerobic with high FTPA concentrations in the more efficient of the two NMR chambers. A new precursor molecule for the 19F-NMR pH indicator difluoromethylalanine, the para-chlorophenyl ester, has been tested and used in RINm5F cells and P. denitrificans, neither of which hydrolyzes methyl esters. PMID:3345331

  4. Molecular dynamics of 1-ethyl-3-methylimidazolium triflate ionic liquid studied by (1)H and (19)F nuclear magnetic resonances.

    PubMed

    Wencka, Magdalena; Apih, Tomaž; Korošec, Romana Cerc; Jenczyk, Jacek; Jarek, Marcin; Szutkowski, Kosma; Jurga, Stefan; Dolinšek, Janez

    2017-06-14

    The molecular dynamics of an ionic liquid (IL) composed of a 1-ethyl-3-methylimidazolium cation and a triflate (trifluoromethanesulfonate) anion, abbreviated as [Emim][TfO], were studied by NMR spectroscopy. By measuring the temperature-dependent high-field 1H and (19)F spin-lattice relaxation (SLR) rates, the frequency-dependent (1)H and (19)F SLR dispersion curves using fast-field-cycling relaxometry, and the temperature-dependent 1H and (19)F diffusion constants, and by utilizing the fact that the primary NMR-active nucleus on the Emim cation is (1)H, whereas on the TfO anion it is (19)F, the cationic and anionic dynamics were studied separately. A single theoretical relaxation model successfully reproduced all the experimental data of both types of resonant nuclei by fitting all the data simultaneously with the same set of fit parameters. Upon cooling, [Emim][TfO] exhibited a supercooled liquid phase between TSL = 256 K and the crystallization temperature TCr ≈ 227-222 K, as confirmed by differential scanning calorimetry (DSC) experiments. Theoretical analysis revealed that within the liquid and the supercooled liquid states of [Emim][TfO], the (1)H and (19)F relaxation rates are affected by both the rotational and translational diffusional processes with no discontinuous change at TSL. While the rotational diffusion is well described as an Arrhenius thermally activated process, the translational diffusion undergoes strong freezing dynamics that are well described by the Vogel-Fulcher model assuming a freezing temperature of T0 = 157 K. The existence of the supercooled liquid region in the [Emim][TfO] IL should be taken into account when using this IL for a specific application.

  5. Conformation of gramicidin A channel in phospholipid vesicles: a 13C and 19F nuclear magnetic resonance study.

    PubMed Central

    Weinstein, S; Wallace, B A; Blout, E R; Morrow, J S; Veatch, W

    1979-01-01

    We have determined the conformation of the channel-forming polypeptide antibiotic gramicidin A in phosphatidylcholine vesicles by using 13C and 19F NMR spectroscopy. The models previously proposed for the conformation of the dimer channel differ in the surface localization of the NH2 and COOH termini. We have incorporated specific 13C and 19F nuclei at both the NH2, and COOH termini of gramicidin and have used 13C and 19F chemical shifts and spin lattice relaxation time measurements to determine the accessibility of these labels to three paramagnetic NMR probes--two in aqueous solution and one attached to the phosphatidylcholine fatty acid chain9 all of our results indicate that the COOH terminus of gramicidin in the channel is located near the surface of the membrane and the NH2 terminus is buried deep within the lipid bilayer. These findings strongly favor an NH2-terminal to NH2-terminal helical dimer as the major conformation for the gramicidin channel in phosphatidylcholine vesicles. PMID:92025

  6. Understanding solution-state noncovalent interactions between xenobiotics and natural organic matter using 19F/1H heteronuclear saturation transfer difference nuclear magnetic resonance spectroscopy.

    PubMed

    Longstaffe, James G; Simpson, André J

    2011-08-01

    A combination of forward and reverse heteronuclear ((19)F/(1)H) saturation transfer difference (STD) nuclear magnetic resonance (NMR) spectroscopic techniques were applied to characterize the noncovalent interactions between perfluorinated aromatic xenobiotics and dissolved humic acid. These NMR techniques produce detailed molecular-level descriptions of weak noncovalent associations between components in complex environmental mixtures, allowing the mechanisms underlying these interactions to be explored; (19)F observed heteronuclear STD (H-STD) is used to describe the average molecular orientation of the xenobiotics during their interactions with humic acid, whereas (1)H observed reverse-heteronuclear STD (RH-STD) is used to both identify and quantify preferences exhibited by xenobiotics for interactions at different types of humic acid moieties. First, by using H-STD, it is shown that selected aromatic organofluorides orient with their nonfluorine functional groups (OH, NH(2), and COOH) directed away from humic acid during the interactions, suggesting that these functional groups are not specifically involved. Second, the RH-STD experiment is shown to be sensitive to subtle differences in preferred interaction sites in humic acid and is used here to demonstrate preferential interactions at aromatic humic acid sites for selected aromatic xenobiotics, C(10)F(7)OH, and C(6)F(4)X(2), (where X = F, OH, NH(2), NO(2), or COOH), that can be predicted from the electrostatic potential density maps of the xenobiotic. Copyright © 2011 SETAC.

  7. Fluorinated Vitamin B12 Analogs Are Cofactors of Corrinoid-Dependent Enzymes: a 19F-Labeled Nuclear Magnetic Resonance Probe for Identifying Corrinoid-Protein Interactions

    PubMed Central

    Stupperich, Erhard; Eisinger, Hans-Jürgen; Kerssebaum, Rainer; Nexø, Ebba

    1993-01-01

    The homoacetogenic bacterium Sporomusa ovata synthesized the vitamin B12 analog phenolyl cobamide or 4-fluorophenolyl cobamide when the methanol medium of growing cells was supplemented with 10 mM phenol or 5 mM 4-fluorophenol. Phenol and, presumably, 4-fluorophenol were specifically incorporated into these cobamides, since phenol was not metabolized significantly into amino acids or into acetic acid, the product of the catabolism. The phenol-containing cobamides contributed up to 90% of the protein-bound cobamides of the 1,300 to 1,900 nmol of corrinoid per g of dry cell material formed. Fluorine-19 nuclear magnetic resonance spectroscopy of 4-fluorophenolyl cobamide exhibited a resonance near 30 ppm. An additional signal emerged at 25 ppm when 4-fluorophenolyl cobamide was investigated as the cofactor of a corrinoid-dependent protein. The two resonances indicated distinct cofactor arrangements within the protein's active site. A 5-ppm high-field shift change suggested van der Waal's interactions between the fluorinated nucleotide of the cofactor and adjacent amino acid residues of the enzyme. Similarly, Propionibacterium freudenreichii and Methanobacterium thermoautotrophicum synthesized 5-fluorobenzimidazolyl cobamide. The human corrinoid binders intrinsic factor, transcobalamin, and haptocorrin recognized this corrinoid like vitamin B12. Hence, it is possible to use 19F-labeled nuclear magnetic resonance spectroscopy for analyses of protein-bound cobamides. PMID:16348877

  8. A bisphosphonate for 19F-magnetic resonance imaging

    PubMed Central

    Kenny, Gavin D.; Shaw, Karen P.; Sivachelvam, Saranja; White, Andrew J.P.; Botnar, Rene M.; T.M. de Rosales, Rafael

    2016-01-01

    19F-magnetic resonance imaging (MRI) is a promising technique that may allow us to measure the concentration of exogenous fluorinated imaging probes quantitatively in vivo. Here, we describe the synthesis and characterisation of a novel geminal bisphosphonate (19F-BP) that contains chemically-equivalent fluorine atoms that show a single and narrow 19F resonance and a bisphosphonate group that may be used for labelling inorganic materials based in calcium phosphates and metal oxides. The potential of 19F-BP to provide contrast was analysed in vitro and in vivo using 19F-MRI. In vitro studies demonstrated the potential of 19F-BP as an MRI contrast agent in the millimolar concentration range with signal-to-noise ratios (SNR) comparable to previously reported fluorinated probes. The preliminary in vivo MRI study reported here allowed us to visualise the biodistribution of 19F-BP, showing uptake in the liver and in the bladder/urinary system areas. However, bone uptake was not observed. In addition, 19F-BP showed undesirable toxicity effects in mice that prevent further studies with this compound at the required concentrations for MRI contrast. This study highlights the importance of developing 19F MRI probes with the highest signal intensity achievable. PMID:27110036

  9. In vitro quantitative ((1))H and ((19))F nuclear magnetic resonance spectroscopy and imaging studies of fluvastatin™ in Lescol® XL tablets in a USP-IV dissolution cell.

    PubMed

    Zhang, Qilei; Gladden, Lynn; Avalle, Paolo; Mantle, Michael

    2011-12-20

    Swellable polymeric matrices are key systems in the controlled drug release area. Currently, the vast majority of research is still focused on polymer swelling dynamics. This study represents the first quantitative multi-nuclear (((1))H and ((19))F) fast magnetic resonance imaging study of the complete dissolution process of a commercial (Lescol® XL) tablet, whose formulation is based on the hydroxypropyl methylcellulose (HPMC) polymer under in vitro conditions in a standard USP-IV (United States Pharmacopeia apparatus IV) flow-through cell that is incorporated into high field superconducting magnetic resonance spectrometer. Quantitative RARE ((1))H magnetic resonance imaging (MRI) and ((19))F nuclear magnetic resonance (NMR) spectroscopy and imaging methods have been used to give information on: (i) dissolution media uptake and hydrodynamics; (ii) active pharmaceutical ingredient (API) mobilisation and dissolution; (iii) matrix swelling and dissolution and (iv) media activity within the swelling matrix. In order to better reflect the in vivo conditions, the bio-relevant media Simulated Gastric Fluid (SGF) and Fasted State Simulated Intestinal Fluid (FaSSIF) were used. A newly developed quantitative ultra-fast MRI technique was applied and the results clearly show the transport dynamics of media penetration and hydrodynamics along with the polymer swelling processes. The drug dissolution and mobility inside the gel matrix was characterised, in parallel to the ((1))H measurements, by ((19))F NMR spectroscopy and MRI, and the drug release profile in the bulk solution was recorded offline by UV spectrometer. We found that NMR spectroscopy and 1D-MRI can be uniquely used to monitor the drug dissolution/mobilisation process within the gel layer, and the results from ((19))F NMR spectra indicate that in the gel layer, the physical mobility of the drug changes from "dissolved immobilised drug" to "dissolved mobilised drug".

  10. Site-specific solvent exposure analysis of a membrane protein using unnatural amino acids and {sup 19}F nuclear magnetic resonance

    SciTech Connect

    Shi, Pan; Li, Dong; Chen, Hongwei; Xiong, Ying; Tian, Changlin

    2011-10-22

    Highlights: {yields} Solvent isotope shift analysis of {sup 19}F-tfmF in different H{sub 2}O/D{sub 2}O molar ratio. {yields} Correlation between solvent isotope shift of {sup 19}F-spins and solvent exposure analysis. {yields} Solvent exposure analysis of membrane proteins. -- Abstract: Membrane proteins play an essential role in cellular metabolism, transportation and signal transduction across cell membranes. The scarcity of membrane protein structures has thus far prevented a full understanding of their molecular mechanisms. Preliminary topology studies and residue solvent exposure analysis have the potential to provide valuable information on membrane proteins of unknown structure. Here, a {sup 19}F-containing unnatural amino acid (trimethylfluoro-phenylalanine, tfmF) was applied to accomplish site-specific {sup 19}F spin incorporation at different sites in diacylglycerol kinase (DAGK, an Escherichia coli membrane protein) for site-specific solvent exposure analysis. Due to isotope effect on {sup 19}F spins, a standard curve for {sup 19}F-tfmF chemical shifts was drawn for varying solvent H{sub 2}O/D{sub 2}O ratios. Further site-specific {sup 19}F solvent isotope shift analysis was conducted for DAGK to distinguish residues in water-soluble loops, interfacial areas or hydrophobic membrane regions. This site-specific solvent exposure analysis method could be applied for further topological analysis of other membrane proteins.

  11. (19)F Nuclear Magnetic Resonance Spectrometric Determination of the Partition Coefficients of Flutamide and Nilutamide (Antiprostate Cancer Drugs) in a Lipid Nano-Emulsion and Prediction of Its Encapsulation Efficiency for the Drugs.

    PubMed

    Takegami, Shigehiko; Kitamura, Keisuke; Ohsugi, Mayuko; Konishi, Atsuko; Kitade, Tatsuya

    2016-12-01

    To design a useful lipid drug carrier having a high encapsulation efficiency (EE%) for the antiprostate cancer drugs flutamide (FT) and nilutamide (NT), a lipid nano-emulsion (LNE) was prepared with soybean oil (SO), phosphatidylcholine (PC), and sodium palmitate, and the partition coefficients (K ps) of the drugs for the LNE were determined by (19)F nuclear magnetic resonance (NMR) spectrometry. The (19)F NMR signal of the trifluoromethyl group of both drugs showed a downfield shift from an internal standard (trifluoroethanol) and broadening according to the increase in the lipid concentration due to their interaction with LNE particles. The difference in the chemical shift (Δδ) of each drug caused by the addition of LNE was measured under different amounts of LNE, and the K p values were calculated from the Δδ values. The results showed that FT has higher lipophilicity than NT. The total lipid concentration (SO + PC) required to encapsulate each drug into LNE with an EE% of more than 95% was calculated from the K p values as 93.3 and 189.9 mmol/L for FT and NT, respectively. For an LNE prepared with the total lipid concentration of 215 mmol/L, the predicted EE% values were 98 and 96% for FT and NT, respectively, while the experimental EE% values determined by a centrifugation method were approximately 99% for both drugs. Thus, the (19)F NMR spectrometric method is a useful technique to obtain the K p values of fluorinated drugs and thereby predict the theoretical lipid concentrations and prepare LNEs with high EE% values.

  12. Injectable hyaluronic acid hydrogel for 19F magnetic resonance imaging.

    PubMed

    Yang, Xia; Sun, Yi; Kootala, Sujit; Hilborn, Jöns; Heerschap, Arend; Ossipov, Dmitri

    2014-09-22

    We report on a 19F labeled injectable hyaluronic acid (HA) hydrogel that can be monitored by both 1H and 19F MR imaging. The HA based hydrogel formed via carbazone reaction can be obtained within a minute by simple mixing of HA-carbazate and HA-aldehyde derivatized polymers. 19F contrast agent was linked to with carbazate and thiol dually functionalized HA via orthogonal Michael addition reaction which afforded cross-linkable and 19F labeled HA. The 19F labeling of HA polymer did not affect the mechanical properties of the formed hydrogel. As a result, the shape of a hydrogel sample could be imaged very well by both 1H MRI and high resolution 19F MRI. This hydrogel has high potential in clinical applications since it is injectable, biocompatible, and can be tracked in a minimally invasive manner. The present approach can be applied in preparation of injectable 19F labeled hydrogel biomaterials from other natural biomacromolecules.

  13. Fluorinated polyurethane scaffolds for 19F magnetic resonance imaging

    PubMed Central

    Rahimi, Khosrow; Shi, Yang; Schulz, Volkmar; Kuehne, Alexander J. C.; Jockenhoevel, Stefan; Kiessling, Fabian

    2017-01-01

    Polymers are increasingly employed in implant materials. To reduce the incidence of complications, which in the case of vascular grafts include incorrect placement and restenosis, materials are needed which allow for image-guided implantation, as well as for accurate and efficient postoperative implant imaging. We here describe amorphous fluorinated polymers based on thermoplastic polyurethane (19F-TPU), and show that are useful starting materials for developing tissue-engineered vascular grafts which can be detected using 19F MRI.

  14. Probe-Specific Procedure to Estimate Sensitivity and Detection Limits for 19F Magnetic Resonance Imaging

    PubMed Central

    Taylor, Alexander J.; Granwehr, Josef; Lesbats, Clémentine; Krupa, James L.; Six, Joseph S.; Pavlovskaya, Galina E.; Thomas, Neil R.; Auer, Dorothee P.; Meersmann, Thomas; Faas, Henryk M.

    2016-01-01

    Due to low fluorine background signal in vivo, 19F is a good marker to study the fate of exogenous molecules by magnetic resonance imaging (MRI) using equilibrium nuclear spin polarization schemes. Since 19F MRI applications require high sensitivity, it can be important to assess experimental feasibility during the design stage already by estimating the minimum detectable fluorine concentration. Here we propose a simple method for the calibration of MRI hardware, providing sensitivity estimates for a given scanner and coil configuration. An experimental “calibration factor” to account for variations in coil configuration and hardware set-up is specified. Once it has been determined in a calibration experiment, the sensitivity of an experiment or, alternatively, the minimum number of required spins or the minimum marker concentration can be estimated without the need for a pilot experiment. The definition of this calibration factor is derived based on standard equations for the sensitivity in magnetic resonance, yet the method is not restricted by the limited validity of these equations, since additional instrument-dependent factors are implicitly included during calibration. The method is demonstrated using MR spectroscopy and imaging experiments with different 19F samples, both paramagnetically and susceptibility broadened, to approximate a range of realistic environments. PMID:27727294

  15. Amyloid imaging using fluorine-19 magnetic resonance imaging ((19)F-MRI).

    PubMed

    Tooyama, Ikuo; Yanagisawa, Daijiro; Taguchi, Hiroyasu; Kato, Tomoko; Hirao, Koichi; Shirai, Nobuaki; Sogabe, Takayuki; Ibrahim, Nor Faeizah; Inubushi, Toshiro; Morikawa, Shigehiro

    2016-09-01

    The formation of senile plaques followed by the deposition of amyloid-β is the earliest pathological change in Alzheimer's disease. Thus, the detection of senile plaques remains the most important early diagnostic indicator of Alzheimer's disease. Amyloid imaging is a noninvasive technique for visualizing senile plaques in the brains of Alzheimer's patients using positron emission tomography (PET) or magnetic resonance imaging (MRI). Because fluorine-19 ((19)F) displays an intense nuclear magnetic resonance signal and is almost non-existent in the body, targets are detected with a higher signal-to-noise ratio using appropriate fluorinated contrast agents. The recent introduction of high-field MRI allows us to detect amyloid depositions in the brain of living mouse using (19)F-MRI. So far, at least three probes have been reported to detect amyloid deposition in the brain of transgenic mouse models of Alzheimer's disease; (E,E)-1-fluoro-2,5-bis-(3-hydroxycarbonyl-4-hydroxy)styrylbenzene (FSB), 1,7-bis(4'-hydroxy-3'-trifluoromethoxyphenyl)-4-methoxycarbonylethyl-1,6-heptadiene3,5-dione (FMeC1, Shiga-Y5) and 6-(3',6',9',15',18',21'-heptaoxa-23',23',23'-trifluorotricosanyloxy)-2-(4'-dimethylaminostyryl)benzoxazole (XP7, Shiga-X22). This review presents the recent advances in amyloid imaging using (19)F-MRI, including our own studies. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Defect induced magnetism in highly oriented pyrolytic graphite: bulk magnetization and 19F hyperfine interaction studies.

    PubMed

    Mohanta, S K; Mishra, S N; Davane, S M; Srivastava, S K

    2012-02-29

    We have made bulk and local investigations on defect induced magnetism in highly oriented pyrolytic graphite (HOPG) irradiated with a 40 MeV carbon beam. The local magnetic response of irradiated HOPG was studied by measuring the hyperfine field of recoil implanted (19)F using γ-ray time differential perturbed angular distribution (TDPAD) measurements. While the bulk magnetic properties of the irradiated sample show features characteristic of room temperature ferromagnetism, the hyperfine field data reflect enhanced paramagnetism with no indication of long range magnetic ordering. The experimental studies are further supported by ab initio density functional calculations. We believe that the ferromagnetic response in irradiated HOPG arises mostly from defect induced magnetic moments of carbon atoms in the near surface region, while those deep inside the host matrix remain paramagnetic.

  17. 19F-magnetic resonance spectroscopy and chemical shift imaging for schizophrenic patients using haloperidol decanoate.

    PubMed

    Sassa, Takeshi; Suhara, Tetsuya; Ikehira, Hiroo; Obata, Takayuki; Girard, Franck; Tanada, Shuji; Okubo, Yoshiro

    2002-12-01

    Haloperidol decanoate is widely used in the maintenance treatment of schizophrenia and other psychotic disorders, but knowledge concerning its pharmacokinetics at the injected region is very limited. Because the chemical structure of haloperidol contains fluorine, in vivo 19F-magnetic resonance (MR) spectroscopy (repetition time (TR) = 1 s) and chemical shift imaging (CSI; TR = 1 s, pixel size = 15 x 15 mm) were performed in schizophrenic patients who were treated with haloperidol decanoate (three men and one woman) to measure its diachronic change at the injection point and visualize its local distribution after intramuscular injection. 19F signals (T1 time = 365 ms) were obtained at the haloperidol decanoate-injected region. The decrease rate of the signal-to-noise ratio (SNR) by 19F-MR spectroscopy seemed large in comparison with that of the plasma haloperidol concentration. The distribution was clearly visualized by 19F-CSI for a few days after the injection, but after 1 week could no longer be seen. Although the slow-release characteristics of depot neuroleptics have been explained by the slow diffusion of esterified neuroleptics from the oil vehicle, this result may suggest that there are other mechanisms involved in maintaining the plasma haloperidol concentration. In vivo 19F-MR spectroscopy and CSI are potentially applicable for the pharmacokinetic analysis of haloperidol and other drugs containing fluorine in their structure.

  18. Monitoring Dendritic Cell Migration using 19F / 1H Magnetic Resonance Imaging

    PubMed Central

    Waiczies, Helmar; Guenther, Martin; Skodowski, Julia; Lepore, Stefano; Pohlmann, Andreas; Niendorf, Thoralf; Waiczies, Sonia

    2013-01-01

    Continuous advancements in noninvasive imaging modalities such as magnetic resonance imaging (MRI) have greatly improved our ability to study physiological or pathological processes in living organisms. MRI is also proving to be a valuable tool for capturing transplanted cells in vivo. Initial cell labeling strategies for MRI made use of contrast agents that influence the MR relaxation times (T1, T2, T2*) and lead to an enhancement (T1) or depletion (T2*) of signal where labeled cells are present. T2* enhancement agents such as ultrasmall iron oxide agents (USPIO) have been employed to study cell migration and some have also been approved by the FDA for clinical application. A drawback of T2* agents is the difficulty to distinguish the signal extinction created by the labeled cells from other artifacts such as blood clots, micro bleeds or air bubbles. In this article, we describe an emerging technique for tracking cells in vivo that is based on labeling the cells with fluorine (19F)-rich particles. These particles are prepared by emulsifying perfluorocarbon (PFC) compounds and then used to label cells, which subsequently can be imaged by 19F MRI. Important advantages of PFCs for cell tracking in vivo include (i) the absence of carbon-bound 19F in vivo, which then yields background-free images and complete cell selectivityand(ii) the possibility to quantify the cell signal by 19F MR spectroscopy. PMID:23542739

  19. Measurement of the 19F(α,n)22Na Cross Section for Nuclear Safeguards Science

    NASA Astrophysics Data System (ADS)

    Lowe, Marcus; Smith, M. S.; Pain, S.; Febbraro, M.; Pittman, S.; Chipps, K. A.; Thompson, S. J.; Grinder, M.; Grzywacz, R.; Smith, K.; Thornsberry, C.; Thompson, P.; Peters, W. A.; Waddell, D.; Blanchard, R.; Carls, A.; Shadrick, S.; Engelhardt, A.; Hertz-Kintish, D.; Allen, N.; Sims, H.

    2015-10-01

    Enriched uranium is commonly stored in fluoride matrices such as UF6. Alpha decays of uranium in UF6 will create neutrons via the 19F(α,n)22Na reaction. An improved cross section for this reaction will enable improved nondestructive assays of uranium content in storage cylinders at material enrichment facilities. To determine this reaction cross section, we have performed experiments using both forward and inverse kinematic techniques at the University of Notre Dame (forward) and Oak Ridge National Laboratory (inverse). Both experiments utilized the Versatile Array of Neutron Detectors at Low Energy (VANDLE) for neutron detection. The ORNL experiment also used a new ionization chamber for 22Na particle identification. Gating on the 22Na nuclei detected drastically reduced the background counts in the neutron time-of-flight spectra. The latest analysis and results will be presented for 19F beam energies ranging from 20-37 MeV. This work is funded in part by the DOE Office of Nuclear Physics, the National Nuclear Security Administration's Office of Defense Nuclear Nonproliferation R&D, and the NSF.

  20. First-Principles Study of Nuclear Quadruple Interaction of ^19F* and Binding in Solid Fluorine

    NASA Astrophysics Data System (ADS)

    Mishra, D. R.; Aryal, M. M.; Adhikari, N. P.; Badu, S. R.; Pink, R. H.; Scheicher, R. H.; Chow, Lee; Das, T. P.

    2010-03-01

    We have studied the binding energy (BE) and nuclear quadrupule interaction (NQI) parameters for the ^19F* excited nuclear state in solid fluorine as part of our investigation [1] of the properties of solid halogens using the first principles Hartree-Fock Cluster procedure combined with many-body perturbation theory (MBPT), implemented by the Gaussian set of programs. Our results show that Van der Waals interaction obtained from intermolecular electron correlation effects has dominant influence on the BE but negligible effect on the NQI parameters. For the latter, ourcalculated e^2qQ is 119.0MHz using for Q(19F*), the value of 0.072 *10-28m2 [2], and η, the asymmetry parameter, is essentially zero. The influence of rotational vibrational effects on e^2qQ is being investigated using a first-principles procedure [3] to bridge the small remaining difference with experiment (127.2 MHz) for e^2qQ [4]. [1] M.M. Aryal et al., Hyperfine Interact, 176, 51 (2007). [2] K.C.Mishra et al.,Phys. Rev.B25, 3389(1982). [3] N. Sahoo et al. Phys. Rev. Lett. 50, 913(1983) [4] H. Barfuss et al., Phys. Lett. 90A, 33(1982)

  1. Cerebral blood flow in experimental ischemia assessed by sup 19 F magnetic resonance spectroscopy in cats

    SciTech Connect

    Brunetti, A.; Nagashima, G.; Bizzi, A.; DesPres, D.J. )

    1990-10-01

    We evaluated a 19F magnetic resonance spectroscopic technique that detects Freon-23 washout as a means of measuring cerebral blood flow in halothane-anesthetized adult cats during and after transient cerebral ischemia produced by vascular occlusion. The experiments were performed to test the ability of this recently developed method to detect postischemic flow deficits. Results were consistent with postischemic hypoperfusion. The method also proved valuable for measuring small residual flow during vascular occlusion. Our experiments indicate that this method provides simple, rapid, and repeatable flow measurements that can augment magnetic resonance examinations of cerebral metabolic parameters in the study of ischemia.

  2. Hexaphyrin as a Potential Theranostic Dye for Photothermal Therapy and 19F Magnetic Resonance Imaging.

    PubMed

    Higashino, Tomohiro; Nakatsuji, Hirotaka; Fukuda, Ryosuke; Okamoto, Haruki; Imai, Hirohiko; Matsuda, Tetsuya; Tochio, Hidehito; Shirakawa, Masahiro; Tkachenko, Nikolai; Hashida, Mitsuru; Murakami, Tatsuya; Imahori, Hiroshi

    2017-02-15

    meso-Aryl substituted expanded porphyrins have two potential key features suitable for theranostic agents, excellent absorption in near infrared (NIR) region and possible introduction of multiple fluorine atoms at structurally nearly equivalent positions. Herein, hexaphyrin (hexa) was synthesized using 2,6-bis(trifluoromethyl)-4-formyl benzoate and pyrrole and evaluated as a novel theranostic expanded porphyrin possessing the above key features. Under NIR light illumination hexa showed intense photothermal and weak photodynamic effects, which were most likely due to its low-lying excited states close to a singlet oxygen. This sustained photothermal effect caused the ablation of cancer cells more effectively than the photodynamic effect of indocyanine green, a clinically used dye. In addition, hexa@cpHDL revealed potential for use in visualization of tumors by 19F magnetic resonance imaging (MRI) due to the presence of the multiple fluorine atoms. These results shed light on a latent utility of expanded porphyrins as theranostic agents in both photothermal therapy and 19F MRI.

  3. (19)F spin-lattice relaxation of perfluoropolyethers: Dependence on temperature and magnetic field strength (7.0-14.1T).

    PubMed

    Kadayakkara, Deepak K; Damodaran, Krishnan; Hitchens, T Kevin; Bulte, Jeff W M; Ahrens, Eric T

    2014-05-01

    Fluorine ((19)F) MRI of perfluorocarbon-labeled cells has become a powerful technique to track the migration and accumulation of cells in living organisms. It is common to label cells for (19)F MRI with nanoemulsions of perfluoropolyethers that contain a large number of chemically equivalent fluorine atoms. Understanding the mechanisms of (19)F nuclear relaxation, and in particular the spin-lattice relaxation of these molecules, is critical to improving experimental sensitivity. To date, the temperature and magnetic field strength dependence of spin-lattice relaxation rate constant (R1) for perfluoropolyethers has not been described in detail. In this study, we evaluated the R1 of linear perfluoropolyether (PFPE) and cyclic perfluoro-15-crown-5 ether (PCE) at three magnetic field strengths (7.0, 9.4, and 14.1T) and at temperatures ranging from 256-323K. Our results show that R1 of perfluoropolyethers is dominated by dipole-dipole interactions and chemical shift anisotropy. R1 increased with magnetic field strength for both PCE and PFPE. In the temperature range studied, PCE was in the fast motion regime (ωτc<1) at all field strengths, but for PFPE, R1 passed through a maximum, from which the rotational correlation time was estimated. The importance of these measurements for the rational design of new (19)F MRI agents and methods is discussed. Copyright © 2014 Elsevier Inc. All rights reserved.

  4. Visualizing arthritic inflammation and therapeutic response by fluorine-19 magnetic resonance imaging (19F MRI)

    PubMed Central

    2012-01-01

    Background Non-invasive imaging of inflammation to measure the progression of autoimmune diseases, such as rheumatoid arthritis (RA), and to monitor responses to therapy is critically needed. V-Sense, a perfluorocarbon (PFC) contrast agent that preferentially labels inflammatory cells, which are then recruited out of systemic circulation to sites of inflammation, enables detection by 19F MRI. With no 19F background in the host, detection is highly-specific and can act as a proxy biomarker of the degree of inflammation present. Methods Collagen-induced arthritis in rats, a model with many similarities to human RA, was used to study the ability of the PFC contrast agent to reveal the accumulation of inflammation over time using 19F MRI. Disease progression in the rat hind limbs was monitored by caliper measurements and 19F MRI on days 15, 22 and 29, including the height of clinically symptomatic disease. Naïve rats served as controls. The capacity of the PFC contrast agent and 19F MRI to assess the effectiveness of therapy was studied in a cohort of rats administered oral prednisolone on days 14 to 28. Results Quantification of 19F signal measured by MRI in affected limbs was linearly correlated with disease severity. In animals with progressive disease, increases in 19F signal reflected the ongoing recruitment of inflammatory cells to the site, while no increase in 19F signal was observed in animals receiving treatment which resulted in clinical resolution of disease. Conclusion These results indicate that 19F MRI may be used to quantitatively and qualitatively evaluate longitudinal responses to a therapeutic regimen, while additionally revealing the recruitment of monocytic cells involved in the inflammatory process to the anatomical site. This study may support the use of 19F MRI to clinically quantify and monitor the severity of inflammation, and to assess the effectiveness of treatments in RA and other diseases with an inflammatory component. PMID:22721447

  5. Using magnetic coupling to implement 1H, 19F, 13C experiments in routine high resolution NMR probes

    NASA Astrophysics Data System (ADS)

    Bowyer, Paul; Finnigan, Jim; Marsden, Brian; Taber, Bob; Zens, Albert

    2015-12-01

    We report in this paper the design of 1H, 19F, 13C circuitry using magnetic coupling which can do on demand experiments where one of the three nuclei is observed and the other two are decoupled. The implementation of this circuitry in routine NMR probes is compared with capacitive coupling methods where it was found that by using magnetic coupling the performance of the routine NMR probe was not impacted by the addition of this circuitry. It is surmised that using this type of circuitry would be highly desirable for those chemists doing routine 19F NMR.

  6. Understanding of Nuclear Quadruple Interaction of ^ 19F* and Binding Energies of Solid Fluorine at the First-Principles Level

    NASA Astrophysics Data System (ADS)

    Mishra, D. R.; Aryal, M. M.; Adhikari, N. P.; Badu, S. R.; Pink, R. H.; Scheicher, R. H.; Chow, Lee; Das, T. P.

    2009-03-01

    We have studied the binding energy (BE) and nuclear quadrupole interaction (NQI) parameters for the ^19F* excited nuclear state in solid fluorine as part of our investigation [1] of the properties of solid halogens using the first principles Hartree-Fock Cluster procedure combined with many-body perturbation theory (MBPT), implemented by the Gaussian 03 set of programs. Our results show that Van der Waals interaction obtained from intermolecular electron correlation has dominant effect on the BE but negligible effect on the NQI parameters. For the latter, our e^2qQ is 117.7MHz forQ(^19F*), 0.072 *10-28 m^2 [2] and η is essentially zero.. The influence of vibrational effects on e^2qQ is being investigated using a first-principles procedure [3] to bridge the small remaining difference with experiment. [1] M.M. Aryal et al., Hyperfine Interact, 176, 51 (2007). [2] K.C.Mishra et al.,Phys. Rev.B25, 3389(1982). [3] N. Sahoo et al. Phys. Rev. Lett. 50, 913(1983) [4] H. Barfuss et al., Phys. Lett. 90A, 33(1982).

  7. Magnetism, optical absorbance, and 19F NMR spectra of nafion films with self-assembling paramagnetic networks

    SciTech Connect

    Levin, E. M.; Chen, Q.; Bud'ko, S. L.

    2012-01-15

    Magnetization, optical absorbance, and {sup 19}F NMR spectra of Nafion transparent films as received and doped with Mn{sup 2+}, Co{sup 2+}, Fe{sup 2+}, and Fe{sup 3+} ions with and without treatment in 1H-1,2,4-triazole (trz) have been studied. Doping of Nafion with Fe{sup 2+} and Co{sup 2+} and their bridging to nitrogen of triazole yields a hybrid self-assembling paramagnetic system that exhibits interesting magnetic and optical properties. These include spin crossover phenomena between high-spin (HS) and low-spin (LS) states in Nafion-Fe{sup 2+}-trz and Nafion-Co{sup 2+}-trz accompanied by thermochromic effects in the visible range induced by temperature. A large shift of the magnetization curve induced by a magnetic field in the vicinity of the HS {leftrightarrow} LS, {approx}220 K, observed for Nafion-Fe{sup 2+}-trz has a rate of {approx}6 K/kOe, which is about three orders of magnitude larger than that in bulk spin crossover Fe{sup 2+} materials. Selective response of {sup 19}F NMR signals on doping with paramagnetic ions demonstrates that NMR can be used as spatially resolved method to study Nafion film with paramagnetic network. Both chemical shift and width of {sup 19}F NMR signals show that SO groups of Nafion, Fe or Co ions, and nitrogen of triazole are bonded whereas they form a spin crossover system. Based on a model of nanosize cylinders proposed for Nafion [K. Schmidt-Rohr and Q. Chen, Nat Mater (2008), 75], we suggest that paramagnetic ions are located inside these cylinders, forming self-assembling magnetically and optically active nanoscale networks.

  8. Tumour oxygen dynamics measured simultaneously by near-infrared spectroscopy and 19F magnetic resonance imaging in rats

    NASA Astrophysics Data System (ADS)

    Xia, Mengna; Kodibagkar, Vikram; Liu, Hanli; Mason, Ralph P.

    2006-01-01

    Simultaneous near-infrared spectroscopy (NIRS) and magnetic resonance imaging (MRI) were used to investigate the correlation between tumour vascular oxygenation and tissue oxygen tension dynamics in rat breast 13762NF tumours with respect to hyperoxic gas breathing. NIRS directly detected global variations in the oxygenated haemoglobin concentration (Δ[HbO2]) within tumours and oxygen tension (pO2) maps were achieved using 19F MRI of the reporter molecule hexafluorobenzene. Multiple correlations were examined between rates and magnitudes of vascular (Δ[HbO2]) and tissue (pO2) responses. Significant correlations were found between response to oxygen and carbogen breathing using either modality. Comparison of results for the two methods showed a correlation between the vascular perfusion rate ratio and the mean pO2 values (R2 > 0.7). The initial rates of increase of Δ[HbO2] and the slope of dynamic pO2 response, d(pO2)/dt, of well-oxygenated voxels in response to hyperoxic challenge were also correlated. These results demonstrate the feasibility of simultaneous measurements using NIRS and MRI. As expected, the rate of pO2 response to oxygen is primarily dependent upon the well perfused rather than poorly perfused vasculature. Presented in part at the 12th annual meeting of the International Society of Magnetic Resonance in Medicine, Kyoto, 2004.

  9. 19F NMR study of magnetic excitations in the randomly diluted antiferromagnet Mn xZn 1- xF 2

    NASA Astrophysics Data System (ADS)

    Itoh, M.; Yasuoka, H.

    1990-12-01

    Magnetic excitations in antiferromagnetic Mn xZn 1- xF 2 have been investigated using NMR technique. The temperature dependence of the 19F resonance frequency is presented and discussed on the basis of a picture of a crossover from magnon to fracton excitations.

  10. Chitosan-coated poly(lactic-co-glycolic acid) perfluorooctyl bromide nanoparticles for cell labeling in (19)F magnetic resonance imaging.

    PubMed

    Vu-Quang, Hieu; Vinding, Mads Sloth; Xia, Dan; Nielsen, Thomas; Ullisch, Marcus Görge; Dong, MingDong; Nielsen, Niels Chr; Kjems, Jørgen

    2016-01-20

    Noninvasive therapeutic cell tracking methods in living animals are important for understanding cell function and fate in connection with cell therapy. Here we report a new particle system based on chitosan-coated poly(lactic-co-glycolic acid) perfluorooctyl bromide (PLGA PFOB) nanoparticles designed for (19)F magnetic resonance imaging (MRI) cell tracking. Chitosan was adsorbed onto the PLGA PFOB nanoparticles through electric interactions, which led to an increase in the hydrodynamic size and a surface charge proportional to the coating weight ratio. Confocal laser scanning microscopy, flow cytometry analysis and (19)F-MRI showed that to achieve the highest labeling efficiency in vitro, the optimal weight ratio of chitosan to the PLGA PFOB nanoparticles was 1:10 for human mesenchymal stem cells (hMSCs) and 1:100 for Raw 264.7 macrophages. In vivo(19)F-MRI showed that (19)F labeled hMSCs remained at the injected site 24h after injection. Thus, this study validates that chitosan-coated PLGA PFOB nanoparticles have the potential to track cell migration in vivo. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Annual Report FY2013-- A Kinematically Complete, Interdisciplinary, and Co-Institutional Measurement of the 19F(α,n) Cross-section for Nuclear Safeguards Science

    SciTech Connect

    Peters, William A; Smith, Michael Scott; Clement, Ryan; Tan, Wanpeng; Stech, Ed; Cizewski, J A; Febbraro, Michael; Madurga Flores, Miguel

    2013-10-01

    The goal of this proposal is to enable neutron detection for precision Non-Destructive Assays (NDAs) of actinide-fluoride samples. Neutrons are continuously generated from a UFx matrix in a container or sample as a result of the interaction of alpha particles from uranium-decay α particles with fluorine nuclei in the matrix. Neutrons from 19F(α,n)22Na were once considered a poorly characterized background for assays of UFx samples via 238U spontaneous fission neutron detection [SMI2010B]. However, the yield of decay-α-driven neutrons is critical for 234,235U LEU and HEU assays, as it can used to determine both the total amount of uranium and the enrichment [BER2010]. This approach can be extremely valuable in a variety of safeguard applications, such as cylinder monitoring in underground uranium storage facilities, nuclear criticality safety studies, nuclear materials accounting, and other nonproliferation applications. The success of neutron-based assays critically depends on an accurate knowledge of the cross section of the (α,n) reaction that generates the neutrons. The 40% uncertainty in the 19F(α,n)22Na cross section currently limits the precision of such assays, and has been identified as a key factor in preventing accurate enrichment determinations [CRO2003]. The need for higher quality cross section data for (α,n) reactions has been a recurring conclusion in reviews of the nuclear data needs to support safeguards. The overarching goal of this project is to enable neutron detection to be used for precision Non- Destructive Assays (NDAs) of actinide-fluoride samples. This will significantly advance safeguards verification at existing declared facilities, nuclear materials accounting, process control, nuclear criticality safety monitoring, and a variety of other nonproliferation applications. To reach this goal, Idaho National Laboratory (INL), in partnership with Oak Ridge National Laboratory (ORNL), Rutgers University (RU), and the University of Notre

  12. Design principles and theory of paramagnetic fluorine-labelled lanthanide complexes as probes for (19)F magnetic resonance: a proof-of-concept study.

    PubMed

    Chalmers, Kirsten H; De Luca, Elena; Hogg, Naomi H M; Kenwright, Alan M; Kuprov, Ilya; Parker, David; Botta, Mauro; Wilson, J Ian; Blamire, Andrew M

    2010-01-04

    The synthesis and spectroscopic properties of a series of CF(3)-labelled lanthanide(III) complexes (Ln=Gd, Tb, Dy, Ho, Er, Tm) with amide-substituted ligands based on 1,4,7,10-tetraazacyclododecane are described. The theoretical contributions of the (19)F magnetic relaxation processes in these systems are critically assessed and selected volumetric plots are presented. These plots allow an accurate estimation of the increase in the rates of longitudinal and transverse relaxation as a function of the distance between the Ln(III) ion and the fluorine nucleus, the applied magnetic field, and the re-rotational correlation time of the complex, for a given Ln(III) ion. Selected complexes exhibit pH-dependent chemical shift behaviour, and a pK(a) of 7.0 was determined in one example based on the holmium complex of an ortho-cyano DO3A-monoamide ligand, which allowed the pH to be assessed by measuring the difference in chemical shift (varying by over 14 ppm) between two (19)F resonances. Relaxation analyses of variable-temperature and variable-field (19)F, (17)O and (1)H NMR spectroscopy experiments are reported, aided by identification of salient low-energy conformers by using density functional theory. The study of fluorine relaxation rates, over a field range of 4.7 to 16.5 T allowed precise computation of the distance between the Ln(III) ion and the CF(3) reporter group by using global fitting methods. The sensitivity benefits of using such paramagnetic fluorinated probes in (19)F NMR spectroscopic studies are quantified in preliminary spectroscopic and imaging experiments with respect to a diamagnetic yttrium(III) analogue.

  13. 19F Magnetic Resonance Imaging of Perfluorocarbons for the Evaluation of Response to Antibiotic Therapy in a Staphylococcus aureus Infection Model

    PubMed Central

    Jakob, Peter; Ohlsen, Knut

    2013-01-01

    Background The emergence of antibiotic resistant bacteria in recent decades has highlighted the importance of developing new drugs to treat infections. However, in addition to the design of new drugs, the development of accurate preclinical testing methods is essential. In vivo imaging technologies such as bioluminescence imaging (BLI) or magnetic resonance imaging (MRI) are promising approaches. In a previous study, we showed the effectiveness of 19F MRI using perfluorocarbon (PFC) emulsions for detecting the site of Staphylococcus aureus infection. In the present follow-up study, we investigated the use of this method for in vivo visualization of the effects of antibiotic therapy. Methods/Principal findings Mice were infected with S. aureus Xen29 and treated with 0.9% NaCl solution, vancomycin or linezolid. Mock treatment led to the highest bioluminescence values during infection followed by vancomycin treatment. Counting the number of colony-forming units (cfu) at 7 days post-infection (p.i.) showed the highest bacterial burden for the mock group and the lowest for the linezolid group. Administration of PFCs at day 2 p.i. led to the accumulation of 19F at the rim of the abscess in all mice (in the shape of a hollow sphere), and antibiotic treatment decreased the 19F signal intensity and volume. Linezolid showed the strongest effect. The BLI, cfu, and MRI results were comparable. Conclusions 19F-MRI with PFCs is an effective non-invasive method for assessing the effects of antibiotic therapy in vivo. This method does not depend on pathogen specific markers and can therefore be used to estimate the efficacy of antibacterial therapy against a broad range of clinically relevant pathogens, and to localize sites of infection. PMID:23724049

  14. 19F single-quantum and 19F-33S heteronuclear multiple-quantum coherence NMR of SF6 in thermotropic nematogens and in the gas phase.

    PubMed

    Tervonen, Henri; Saunavaara, Jani; Ingman, L Petri; Jokisaari, Jukka

    2006-08-24

    (19)F single-quantum (SQC) and (19)F-(33)S heteronuclear multiple-quantum coherence (HMQC) NMR spectroscopy of sulfur hexafluoride (SF(6)) dissolved in thermotropic liquid crystals (TLCs) were used to investigate the properties of TLCs. On one hand, environmental effects on the NMR parameters of SF(6), (19)F nuclear shielding, (19)F-(33)S spin-spin coupling, secondary isotope effects of sulfur on (19)F shielding, and the self-diffusion coefficient in the direction of the external magnetic field were studied as well. The temperature dependence of the (19)F shielding of SF(6) in TLCs was modeled with a function that takes into account the properties of both TLC and SF(6). It appears that the TLC environment deforms the electronic system of SF(6) so that the (19)F shielding tensor becomes slightly anisotropic, with the anisotropy being from -0.5 to -1.4 ppm, depending upon the TLC solvent. On the contrary, no sign of residual dipolar coupling between (19)F and (33)S was found, meaning that the so-called deformational effects, which arise from the interaction between vibrational and reorientational motions of the molecule, on the geometry of the molecule are insignificant. Diffusion activation energies, E(a), were determined from the temperature dependence of the self-diffusion coefficients. In each TLC, E(a) increases when moving from an isotropic phase to a nematic phase. The spin-spin coupling constant, J((19)F,(33)S), increases by ca. 10 Hz when moving from the gas phase to TLC solutions. The secondary isotope shifts of (19)F shielding are practically independent of TLC solvent and temperature. For the first time, (19)F-(33)S heteronuclear multiple-quantum NMR spectra were recorded for SF(6) in the gas phase and in a liquid-crystalline solution.

  15. Absolute NMR shielding scales and nuclear spin-rotation constants in (175)LuX and (197)AuX (X = (19)F, (35)Cl, (79)Br and (127)I).

    PubMed

    Demissie, Taye B; Jaszuński, Michał; Komorovsky, Stanislav; Repisky, Michal; Ruud, Kenneth

    2015-10-28

    We present nuclear spin-rotation constants, absolute nuclear magnetic resonance (NMR) shielding constants, and shielding spans of all the nuclei in (175)LuX and (197)AuX (X = (19)F, (35)Cl, (79)Br, (127)I), calculated using coupled-cluster singles-and-doubles with a perturbative triples (CCSD(T)) correction theory, four-component relativistic density functional theory (relativistic DFT), and non-relativistic DFT. The total nuclear spin-rotation constants determined by adding the relativistic corrections obtained from DFT calculations to the CCSD(T) values are in general in agreement with available experimental data, indicating that the computational approach followed in this study allows us to predict reliable results for the unknown spin-rotation constants in these molecules. The total NMR absolute shielding constants are determined for all the nuclei following the same approach as that applied for the nuclear spin-rotation constants. In most of the molecules, relativistic effects significantly change the computed shielding constants, demonstrating that straightforward application of the non-relativistic formula relating the electronic contribution to the nuclear spin-rotation constants and the paramagnetic contribution to the shielding constants does not yield correct results. We also analyze the origin of the unusually large absolute shielding constant and its relativistic correction of gold in AuF compared to the other gold monohalides.

  16. Absolute NMR shielding scales and nuclear spin-rotation constants in 175LuX and 197AuX (X = 19F, 35Cl, 79Br and 127I)

    NASA Astrophysics Data System (ADS)

    Demissie, Taye B.; Jaszuński, Michał; Komorovsky, Stanislav; Repisky, Michal; Ruud, Kenneth

    2015-10-01

    We present nuclear spin-rotation constants, absolute nuclear magnetic resonance (NMR) shielding constants, and shielding spans of all the nuclei in 175LuX and 197AuX (X = 19F, 35Cl, 79Br, 127I), calculated using coupled-cluster singles-and-doubles with a perturbative triples (CCSD(T)) correction theory, four-component relativistic density functional theory (relativistic DFT), and non-relativistic DFT. The total nuclear spin-rotation constants determined by adding the relativistic corrections obtained from DFT calculations to the CCSD(T) values are in general in agreement with available experimental data, indicating that the computational approach followed in this study allows us to predict reliable results for the unknown spin-rotation constants in these molecules. The total NMR absolute shielding constants are determined for all the nuclei following the same approach as that applied for the nuclear spin-rotation constants. In most of the molecules, relativistic effects significantly change the computed shielding constants, demonstrating that straightforward application of the non-relativistic formula relating the electronic contribution to the nuclear spin-rotation constants and the paramagnetic contribution to the shielding constants does not yield correct results. We also analyze the origin of the unusually large absolute shielding constant and its relativistic correction of gold in AuF compared to the other gold monohalides.

  17. Absolute NMR shielding scales and nuclear spin–rotation constants in {sup 175}LuX and {sup 197}AuX (X = {sup 19}F, {sup 35}Cl, {sup 79}Br and {sup 127}I)

    SciTech Connect

    Demissie, Taye B. Komorovsky, Stanislav; Repisky, Michal; Ruud, Kenneth; Jaszuński, Michał

    2015-10-28

    We present nuclear spin–rotation constants, absolute nuclear magnetic resonance (NMR) shielding constants, and shielding spans of all the nuclei in {sup 175}LuX and {sup 197}AuX (X = {sup 19}F, {sup 35}Cl, {sup 79}Br, {sup 127}I), calculated using coupled-cluster singles-and-doubles with a perturbative triples (CCSD(T)) correction theory, four-component relativistic density functional theory (relativistic DFT), and non-relativistic DFT. The total nuclear spin–rotation constants determined by adding the relativistic corrections obtained from DFT calculations to the CCSD(T) values are in general in agreement with available experimental data, indicating that the computational approach followed in this study allows us to predict reliable results for the unknown spin–rotation constants in these molecules. The total NMR absolute shielding constants are determined for all the nuclei following the same approach as that applied for the nuclear spin–rotation constants. In most of the molecules, relativistic effects significantly change the computed shielding constants, demonstrating that straightforward application of the non-relativistic formula relating the electronic contribution to the nuclear spin–rotation constants and the paramagnetic contribution to the shielding constants does not yield correct results. We also analyze the origin of the unusually large absolute shielding constant and its relativistic correction of gold in AuF compared to the other gold monohalides.

  18. Determination of size and sign of hetero-nuclear coupling constants from 2D 19F-13C correlation spectra

    NASA Astrophysics Data System (ADS)

    Ampt, Kirsten A. M.; Aspers, Ruud L. E. G.; Dvortsak, Peter; van der Werf, Ramon M.; Wijmenga, Sybren S.; Jaeger, Martin

    2012-02-01

    Fluorinated organic compounds have become increasingly important within the polymer and the pharmaceutical industry as well as for clinical applications. For the structural elucidation of such compounds, NMR experiments with fluorine detection are of great value due to the favorable NMR properties of the fluorine nucleus. For the investigation of three fluorinated compounds, triple resonance 2D HSQC and HMBC experiments were adopted to fluorine detection with carbon and/or proton decoupling to yield F-C, F-C{H}, F-C{Cacq} and F-C{H,Cacq} variants. Analysis of E.COSY type cross-peak patterns in the F-C correlation spectra led, apart from the chemical shift assignments, to determination of size and signs of the JCH, JCF, and JHF coupling constants. In addition, the fully coupled F-C HMQC spectrum of steroid 1 was interpreted in terms of E.COSY type patterns. This example shows how coupling constants due to different nuclei can be determined together with their relative signs from a single spectrum. The analysis of cross-peak patterns, as presented here, not only provides relatively straightforward routes to the determination of size and sign of hetero-nuclear J-couplings in fluorinated compounds, it also provides new and easy ways for the determination of residual dipolar couplings and thus for structure elucidation. The examples and results presented in this study may contribute to a better interpretation and understanding of various F-C correlation experiments and thereby stimulate their utilization.

  19. Characterisation and evaluation of paramagnetic fluorine labelled glycol chitosan conjugates for (19)F and (1)H magnetic resonance imaging.

    PubMed

    De Luca, Elena; Harvey, Peter; Chalmers, Kirsten H; Mishra, Anurag; Senanayake, P Kanthi; Wilson, J Ian; Botta, Mauro; Fekete, Marianna; Blamire, Andrew M; Parker, David

    2014-02-01

    Medium molecular weight glycol chitosan conjugates have been prepared, linked by an amide bond to paramagnetic Gd(III), Ho(III) and Dy(III) macrocyclic complexes in which a trifluoromethyl reporter group is located 6.5 Å from the paramagnetic centre. The faster relaxation of the observed nucleus allows modified pulse sequences to be used with shorter acquisition times. The polydisperse materials have been characterised by gel permeation chromatography, revealing an average molecular weight on the order of 13,800 (Gd), 14,600 (Dy) and 16,200 (Ho), consistent with the presence of 8.5, 9.5 and 13 complexes, respectively. The gadolinium conjugate was prepared for both a q = 1 monoamide tricarboxylate conjugate (r1p 11.2 mM(-1) s(-1), 310 K, 1.4 T) and a q = 0 triphosphinate system, and conventional contrast-enhanced proton MRI studies at 7 T were undertaken in mice bearing an HT-29 or an HCT-116 colorectal tumour xenograft (17 μmol/kg). Enhanced contrast was observed following injection in the tail vein in tumour tissue, with uptake also evident in the liver and kidney with a tumour-to-liver ratio of 2:1 at 13 min, and large amounts in the kidney and bladder consistent with predominant renal clearance. Parallel experiments observing the (19)F resonance in the holmium conjugate complex using a surface coil did not succeed owing to its high R2 value (750 Hz, 7 T). However, the fluorine signal in the dysprosium triphosphinate chitosan conjugate [R1/R2 = 0.6 and R1 = 145 Hz (7 T)] was sharper and could be observed in vivo at -65.7 ppm, following intravenous tail vein injection of a dose of 34 μmol/kg.

  20. Using "On/Off" (19)F NMR/Magnetic Resonance Imaging Signals to Sense Tyrosine Kinase/Phosphatase Activity in Vitro and in Cell Lysates.

    PubMed

    Zheng, Zhen; Sun, Hongbin; Hu, Chen; Li, Gongyu; Liu, Xiaomei; Chen, Peiyao; Cui, Yusi; Liu, Jing; Wang, Junfeng; Liang, Gaolin

    2016-03-15

    Tyrosine kinase and phosphatase are two important, antagonistic enzymes in organisms. Development of noninvasive approach for sensing their activity with high spatial and temporal resolution remains challenging. Herein, we rationally designed a hydrogelator Nap-Phe-Phe(CF3)-Glu-Tyr-Ile-OH (1a) whose supramolecular hydrogel (i.e., Gel 1a) can be subjected to tyrosine kinase-directed disassembly, and its phosphate precursor Nap-Phe-Phe(CF3)-Glu-Tyr(H2PO3)-Ile-OH (1b), which can be subjected to alkaline phosphatase (ALP)-instructed self-assembly to form supramolecular hydrogel Gel 1b, respectively. Mechanic properties and internal fibrous networks of the hydrogels were characterized with rheology and cryo transmission electron microscopy (cryo-TEM). Disassembly/self-assembly of their corresponding supramolecular hydrogels conferring respective "On/Off" (19)F NMR/MRI signals were employed to sense the activity of these two important enzymes in vitro and in cell lysates for the first time. We anticipate that our new (19)F NMR/magnetic resonance imaging (MRI) method would facilitate pharmaceutical researchers to screen new inhibitors for these two enzymes without steric hindrance.

  1. Single-molecule magnets: structural characterization, magnetic properties, and (19)F NMR spectroscopy of a Mn(12) family spanning three oxidation levels.

    PubMed

    Chakov, Nicole E; Soler, Monica; Wernsdorfer, Wolfgang; Abboud, Khalil A; Christou, George

    2005-07-25

    The syntheses, crystal structures, and magnetic properties of [Mn(12)O(12)(O(2)CC(6)F(5))(16)(H(2)O)(4)] (2), (NMe(4))[Mn(12)O(12)(O(2)CC(6)F(5))(16)(H(2)O)(4)] (3), and (NMe(4))(2)[Mn(12)O(12)(O(2)CC(6)F(5))(16)(H(2)O)(4)] (4) are reported. Complex 2 displays quasi-reversible redox couples when examined by cyclic voltammetry in CH(2)Cl(2): one-electron reductions are observed at 0.64 and 0.30 V vs ferrocene. The reaction of complex 2 with 1 and 2 equiv of NMe(4)I yields the one- and two-electron reduced analogues, 3 and 4, respectively. Complexes 2.3CH(2)Cl(2), 3.4.5CH(2)Cl(2).(1)/(2)H(2)O, and 4.6C(7)H(8) crystallize in the triclinic P, monoclinic P2/c, and monoclinic C2/c space groups, respectively. The molecular structures are all very similar, consisting of a central [Mn(IV)O(4)] cubane surrounded by a nonplanar alternating ring of eight Mn and eight mu(3)-O(2)(-) ions. Peripheral ligation is provided by 16 bridging C(6)F(5)CO(2)(-) and 4 H(2)O ligands. Bond valence sum calculations establish that the added electrons in 3 and 4 are localized on former Mn(III) ions giving trapped-valence Mn(IV)(4)Mn(III)(7)Mn(II) and Mn(IV)(4)Mn(III)(6)Mn(II)(2) anions, respectively. (19)F NMR spectroscopy in CD(2)Cl(2) shows retention of the solid-state structure upon dissolution and detrapping of the added electrons in 3 and 4 among the outer ring of Mn ions on the (19)F NMR time scale. DC studies on dried microcrystalline samples of 2, 3, and 4.2.5C(7)H(8) restrained in eicosane in the 1.80-10.0 K and 1-70 kG ranges were fit to give S = 10, D = -0.40 cm(-)(1), g = 1.87, D/g = 0.21 cm(-)(1) for 2, S = 19/2, D = -0.34 cm(-)(1), g = 2.04, D/g = 0.17 cm(-)(1) for 3, and S = 10, D = -0.29 cm(-)(1), g = 2.05, D/g = 0.14 cm(-)(1) for 4, where D is the axial zero-field splitting parameter. The clusters exhibit out-of-phase AC susceptibility signals (chi(M)' ') indicative of slow magnetization relaxation in the 6-8 K range for 2, 4-6 K range for 3, and 2-4 K range for 4; the shift to

  2. New class of 19F pH indicators: fluoroanilines.

    PubMed Central

    Deutsch, C J; Taylor, J S

    1989-01-01

    The pH dependence of the 19F chemical shift has been characterized for a number of fluorine-substituted aniline derivatives. These compounds constitute a new class of 19F nuclear magnetic resonance (NMR) pH indicators, characterized by single 19F resonance lines with sensitivities ranging from 2 to 7 ppm/pH unit near the aniline pKa; total shifts between conjugate acid and base of 5-15 ppm; and pKas ranging from 1 to 7. One compound, N,N-(methyl-2-carboxyisopropyl)-4-fluoroaniline, has a pKa of 6.8 and a sensitivity of 5 ppm/pH unit. This compound displays significant broadening of its 19F resonance near the aniline pKa (6.8), due to a decreased rate of exchange between conjugate acid and base species. Our results are consistent with slow dissociation of an intramolecular hydrogen bond in the zwitterionic species that limits the exchange rate between protonated and unprotonated forms for N,N-(methyl-2-carboxyisopropyl)-4-fluoroaniline. PMID:2720073

  3. 19F MRI for quantitative in vivo cell tracking

    PubMed Central

    Srinivas, Mangala; Heerschap, Arend; Ahrens, Eric T.; Figdor, Carl G.; de Vries, I. Jolanda M.

    2010-01-01

    Cellular therapy, including stem cell transplants and dendritic cell vaccines, is typically monitored for dosage optimization, accurate delivery and localization using non-invasive imaging, of which magnetic resonance imaging (MRI) is a key modality. 19F MRI retains the advantages of MRI as an imaging modality, while allowing direct detection of labelled cells for unambiguous identification and quantification, unlike typical metal-based contrast agents. Recent developments in 19F MRI-based in vivo cell quantification, the existing clinical use of 19F compounds and current explosive interest in cellular therapeutics have brought 19F imaging technology closer to clinical application. We review the application of 19F MRI to cell tracking, discussing intracellular 19F labels, cell labelling and in vivo quantification, as well as the potential clinical use of 19F MRI. PMID:20427096

  4. Rapid exchange of fluoroethylamine via the Rhesus complex in human erythrocytes: 19F NMR magnetization transfer analysis showing competition by ammonia and ammonia analogues.

    PubMed

    Szekely, David; Chapman, Bogdan E; Bubb, William A; Kuchel, Philip W

    2006-08-01

    A remarkable recent discovery in red blood cell function is that the Rhesus antigen complex that for so long was considered to be simply a means of cell recognition is also the ammonia transporter. It catalyzes transmembrane exchange of ammonia on the subsecond time scale, and yet because of a lack of rapid-exchange methodology its kinetics had not been characterized. The flux of ammonia varies appreciably in diverse clinical states, and a convenient method for its characterization would be of basic and of clinical diagnostic value. Fluoroethylamine is water-soluble and when added to a suspension of human red blood cells (RBCs) displays the experimentally useful property of giving separate 19F NMR spectral peaks for the populations inside and outside the cells. By using two-site, one-dimensional magnetization exchange spectroscopy (1D-EXSY), the transmembrane exchange of fluoroethylamine was measured; it was found to occur on the subsecond time scale with an apparent first-order rate constant for efflux, under the equilibrium exchange conditions, of 3.4 s(-1). The method was used to characterize the concentration, temperature, and pH dependence of the exchange rate constant. We determined the extent of competitive inhibition exhibited by ammonia and two molecules that contain an amine group (ethylamine and methylamine). Inhibition of the exchange by incubating the suspension with anti-RhAG antibody, and no inhibition by anti-RhD antibody, suggested specificity of exchange via the RhAG protein of the Rh complex.

  5. Nickel(II) complexes of N-CH2CF3 cyclam derivatives as contrast agents for (19)F magnetic resonance imaging.

    PubMed

    Blahut, Jan; Hermann, Petr; Gálisová, Andrea; Herynek, Vít; Císařová, Ivana; Tošner, Zdeněk; Kotek, Jan

    2016-01-14

    Kinetically inert Ni(ii) complexes of N(1),N(8)-bis(2,2,2-trifluoroethyl)cyclams with hydrogen atoms or phosphonic acid groups in the N(4),N(11)-positions show significant (19)F NMR relaxation rate enhancement useful for 19-fluorine MRI imaging.

  6. New neutron cross-section measurements on {sup 19}F, {sup 39,41}K, {sup 55}Mn, and {sup 103}Rh for improved nuclear criticality safety

    SciTech Connect

    Guber, K. H.; Leal, L. C.; Sayer, R. O.; Koehler, P. E.; Wiarda, D.; Valentine, T. E.; Derrien, H.; Harvey, J. A.; Kopecky, S.; Siegler, P.; Schillebeeckx, P.; Wynants, R.; Ivanov, I.; Borella, A.

    2006-07-01

    A series of new measurements has been undertaken in response to deficiencies identified in nuclear data libraries of crucial importance to the Nuclear Criticality Safety Program as well as for burnup credit studies involving the transportation of spent nuclear fuel. New data and evaluations including covariances are required for several stable fission products as well as for materials found in mixtures with uranium. (authors)

  7. Visualization of Abscess Formation in a Murine Thigh Infection Model of Staphylococcus aureus by 19F-Magnetic Resonance Imaging (MRI)

    PubMed Central

    Kircher, Stefan; Basse-Lüsebrink, Thomas; Haddad, Daniel; Ohlsen, Knut; Jakob, Peter

    2011-01-01

    Background During the last years, 19F-MRI and perfluorocarbon nanoemulsion (PFC) emerged as a powerful contrast agent based MRI methodology to track cells and to visualize inflammation. We applied this new modality to visualize deep tissue abscesses during acute and chronic phase of inflammation caused by Staphylococcus aureus infection. Methodology and Principal Findings In this study, a murine thigh infection model was used to induce abscess formation and PFC or CLIO (cross linked ironoxides) was administered during acute or chronic phase of inflammation. 24 h after inoculation, the contrast agent accumulation was imaged at the site of infection by MRI. Measurements revealed a strong accumulation of PFC at the abscess rim at acute and chronic phase of infection. The pattern was similar to CLIO accumulation at chronic phase and formed a hollow sphere around the edema area. Histology revealed strong influx of neutrophils at the site of infection and to a smaller extend macrophages during acute phase and strong influx of macrophages at chronic phase of inflammation. Conclusion and Significance We introduce 19F-MRI in combination with PFC nanoemulsions as a new platform to visualize abscess formation in a murine thigh infection model of S. aureus. The possibility to track immune cells in vivo by this modality offers new opportunities to investigate host immune response, the efficacy of antibacterial therapies and the influence of virulence factors for pathogenesis. PMID:21455319

  8. Nuclear magnetic resonance gyroscope

    SciTech Connect

    Grover, B.C.

    1984-02-07

    A nuclear magnetic resonance gyro using two nuclear magnetic resonance gases, preferably xenon 129 and xenon 131, together with two alkaline metal vapors, preferably rubidium, potassium or cesium, one of the two alkaline metal vapors being pumped by light which has the wavelength of that alkaline metal vapor, and the other alkaline vapor being illuminated by light which has the wavelength of that other alkaline vapor.

  9. Determining the relative strengths of aromatic and aliphatic C-H⋅⋅⋅X hydrogen bonds in imidazolium ionic liquids through measurement of H/D isotope effects on (19) F nuclear shielding.

    PubMed

    Bottini, Gualberto; Moyna, Guillermo

    2017-05-29

    The relative strengths of aromatic and aliphatic C-H⋅⋅⋅X hydrogen bonds in imidazolium ionic liquids were investigated through measurement of H/D isotope effects on the (19) F nuclear shielding of deuterated isotopologues of 1-n-butyl-3-methylimidazolium hexafluorophosphate and tetrafluoroborate ([C4 mim]PF6 and [C4 mim]BF4 ). Δ(19) F(H,D) values ranging from 9.7 to 49.7 ppb were observed for [C4 mim]PF6 isotopologues, while for the [C4 mim]BF4 series these went from 26.2 to 83.8 ppb. Our findings indicate that the interactions between the fluorinated anions and protons on the C-1' and C-1″ position of the N-alkyl sidechains are comparable to, and in some cases stronger than, those involving protons on the aromatic ring, underscoring the role that these weak interionic forces have on the local ordering of imidazolium salts in the liquid state. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Nanoscale nuclear magnetic resonance with chemical resolution

    NASA Astrophysics Data System (ADS)

    Aslam, Nabeel; Pfender, Matthias; Neumann, Philipp; Reuter, Rolf; Zappe, Andrea; Fávaro de Oliveira, Felipe; Denisenko, Andrej; Sumiya, Hitoshi; Onoda, Shinobu; Isoya, Junichi; Wrachtrup, Jörg

    2017-07-01

    Nuclear magnetic resonance (NMR) spectroscopy is a key analytical technique in chemistry, biology, and medicine. However, conventional NMR spectroscopy requires an at least nanoliter-sized sample volume to achieve sufficient signal. We combined the use of a quantum memory and high magnetic fields with a dedicated quantum sensor based on nitrogen vacancy centers in diamond to achieve chemical shift resolution in 1H and 19F NMR spectroscopy of 20-zeptoliter sample volumes. We demonstrate the application of NMR pulse sequences to achieve homonuclear decoupling and spin diffusion measurements. The best measured NMR linewidth of a liquid sample was ~1 part per million, mainly limited by molecular diffusion. To mitigate the influence of diffusion, we performed high-resolution solid-state NMR by applying homonuclear decoupling and achieved a 20-fold narrowing of the NMR linewidth.

  11. Cell Labeling for 19F MRI: New and Improved Approach to Perfluorocarbon Nanoemulsion Design

    PubMed Central

    Patel, Sravan K.; Williams, Jonathan; Janjic, Jelena M.

    2013-01-01

    This report describes novel perfluorocarbon (PFC) nanoemulsions designed to improve ex vivo cell labeling for 19F magnetic resonance imaging (MRI). 19F MRI is a powerful non-invasive technique for monitoring cells of the immune system in vivo, where cells are labeled ex vivo with PFC nanoemulsions in cell culture. The quality of 19F MRI is directly affected by the quality of ex vivo PFC cell labeling. When co-cultured with cells for longer periods of time, nanoemulsions tend to settle due to high specific weight of PFC oils (1.5–2.0 g/mL). This in turn can decrease efficacy of excess nanoemulsion removal and reliability of the cell labeling in vitro. To solve this problem, novel PFC nanoemulsions are reported which demonstrate lack of sedimentation and high stability under cell labeling conditions. They are monodisperse, have small droplet size (~130 nm) and low polydispersity (<0.15), show a single peak in the 19F nuclear magnetic resonance spectrum at −71.4 ppm and possess high fluorine content. The droplet size and polydispersity remained unchanged after 160 days of follow up at three temperatures (4, 25 and 37 °C). Further, stressors such as elevated temperature in the presence of cells, and centrifugation, did not affect the nanoemulsion droplet size and polydispersity. Detailed synthetic methodology and in vitro testing for these new PFC nanoemulsions is presented. PMID:25586263

  12. (19)F NMR spectroscopic characterization of the interaction of niflumic acid with human serum albumin.

    PubMed

    Kitamura, Keisuke; Omran, Ahmed A; Takegami, Shigehiko; Tanaka, Rumi; Kitade, Tatsuya

    2007-04-01

    The interaction of a non-steroidal anti-inflammatory drug, niflumic acid (NFA), with human serum albumin (HSA) has been investigated by (19)F nuclear magnetic resonance (NMR) spectroscopy. A (19)F NMR spectrum of NFA in a buffered (pH 7.4) solution of NaCl (0.1 mol L(-1)) contained a single sharp signal of its CF(3) group 14.33 ppm from the internal reference 2,2,2-trifluoroethanol. Addition of 0.6 mmol L(-1) HSA to the NFA buffer solution caused splitting of the CF(3) signal into two broadened signals, shifted to the lower fields of 14.56 and 15.06 ppm, with an approximate intensity ratio of 1:3. Denaturation of HSA by addition of 3.0 mol L(-1) guanidine hydrochloride (GU) restored a single sharp signal of CF(3) at 14.38 ppm, indicating complete liberation of NFA from HSA as a result of its denaturation. These results suggest that the binding is reversible and occurs in at least two HSA regions. Competitive (19)F NMR experiments using warfarin, dansyl-L: -asparagine, and benzocaine (site I ligands), and L: -tryptophan and ibuprofen (site II ligands) revealed that NFA binds to site I at two different regions, Ia and Ib, in the ratio 1:3. By use of (19)F NMR with NFA as an (19)F NMR probe the nonfluorinated site I-binding drugs sulfobromophthalein and iophenoxic acid were also found to bind sites Ia and Ib, respectively. These results illustrate the usefulness and convenience of (19)F NMR for investigation of the HSA binding of both fluorinated and nonfluorinated drugs.

  13. Measurement of the extracellular pH of solid tumours in mice by magnetic resonance spectroscopy: a comparison of exogenous (19)F and (31)P probes.

    PubMed

    Ojugo, A S; McSheehy, P M; McIntyre, D J; McCoy, C; Stubbs, M; Leach, M O; Judson, I R; Griffiths, J R

    1999-12-01

    Precise measurement of pH(e) in vivo may be of clinical value for both diagnosis and selection of therapy. pH(e) measurements made by the (31)P probe 3-aminopropylphosphonate (3-APP) were compared with those made by the (19)F probe, 3-[N-(4-fluor-2-trifluoromethylphenyl)-sulphamoyl]-propionic acid (ZK-150471) in three solid tumour types, human HT29 xenografts, murine RIF-1 fibrosarcomas and Lettre tumours grown subcutaneously in mice. No significant differences were observed when probe measurements of pH(e) were compared at 20-60 min post-administration, although very low pH(e) values (ca. 6.0) were recorded in two out of eight Lettre tumours by ZK-150471. The more rapid pH(e) measurements possible using ZK-150471 showed that during the first 20 min post-administration significant increases occurred in pH(e) which were greatest in the more necrotic tumours. Since isolated cell experiments showed that ZK-150471 was non-toxic and did not enter the cells, this early increase in pH(e) may reflect gradual penetration by ZK-150471 of the reportedly alkaline necrotic space in the tumours. The wide chemical shift range, improved signal-to-noise and absence of signal overlap allowed a more rapid and precise measurement of pH(e) by ZK-150471 compared to 3-APP. These characteristics suggest that ZK-150471 is currently the preferred pH(e) probe for non-invasive MRS. Copyright 1999 John Wiley & Sons, Ltd.

  14. Nuclear Magnetic Resonance Gyroscope

    NASA Astrophysics Data System (ADS)

    Bulatowicz, Michael; Griffith, Robert; Larsen, Michael

    2014-03-01

    The navigation grade micro Nuclear Magnetic Resonance Gyroscope (micro-NMRG) being developed by the Northrop Grumman Corporation (NGC) has concluded the fourth and final phase of the DARPA Navigation Grade Integrated Micro Gyro (NGIMG) program. Traditional MEMS gyros utilize springs as an inherent part of the sensing mechanism, leading to bias and scale factor sensitivity to acceleration and vibration. As a result, they have not met performance expectations in real world environments and to date have been limited to tactical grade applications. The Nuclear Magnetic Resonance Gyroscope (NMRG) utilizes the fixed precession rate of a nuclear spin in a constant magnetic field as an inertial reference for determining rotation. The nuclear spin precession rate sensitivity to acceleration and vibration is negligible for most applications. Therefore, the application of new micro and batch fabrication methods to NMRG technology holds great promise for navigation grade performance in a low cost and compact gyro. This poster will describe the history, operational principles, design, and demonstrated performance of the NMRG including an overview of the NGC designs developed and demonstrated in the DARPA gyro development program.

  15. Nuclear Magnetic Resonance Gyroscope

    NASA Astrophysics Data System (ADS)

    Bulatowicz, Michael; Clark, Philip; Griffith, Robert; Larsen, Michael; Mirijanian, James

    2012-06-01

    The navigation grade micro Nuclear Magnetic Resonance Gyroscope (micro-NMRG) being developed by the Northrop Grumman Corporation is concluding the fourth and final phase of the DARPA Navigation Grade Integrated Micro Gyro (NGIMG) program. Traditional MEMS gyros utilize springs as an inherent part of the sensing mechanism, leading to bias and scale factor sensitivity to acceleration and vibration. As a result, they have not met performance expectations in real world environments and to date have been limited to tactical grade applications. The Nuclear Magnetic Resonance Gyroscope (NMRG) utilizes the fixed precession rate of a nuclear spin in a constant magnetic field as an inertial reference for determining rotation. The nuclear spin precession rate sensitivity to acceleration and vibration is negligible for most applications. Therefore, the application of new micro and batch fabrication methods to NMRG technology holds great promise for navigation grade performance in a low cost and compact gyro. This poster will describe the history, operational principles, and design basics of the NMRG including an overview of the NSD designs developed and demonstrated in the DARPA gyro development program. General performance results from phases 3 and 4 will also be presented.

  16. Nuclear Magnetic Resonance Gyroscope

    NASA Astrophysics Data System (ADS)

    Larsen, Michael; Griffith, Robert; Bulatowicz, Michael

    2014-03-01

    The navigation grade micro Nuclear Magnetic Resonance Gyroscope (micro-NMRG) being developed by the Northrop Grumman Corporation (NGC) has concluded the fourth and final phase of the DARPA Navigation Grade Integrated Micro Gyro (NGIMG) program. Traditional MEMS gyros utilize springs as an inherent part of the sensing mechanism, leading to bias and scale factor sensitivity to acceleration and vibration. As a result, they have not met performance expectations in real world environments and to date have been limited to tactical grade applications. The Nuclear Magnetic Resonance Gyroscope (NMRG) utilizes the fixed precession rate of a nuclear spin in a constant magnetic field as an inertial reference for determining rotation. The nuclear spin precession rate sensitivity to acceleration and vibration is negligible for most applications. Therefore, the application of new micro and batch fabrication methods to NMRG technology holds great promise for navigation grade performance in a low cost and compact gyro. This presentation will describe the operational principles, design basics, and demonstrated performance of the NMRG including an overview of the NGC designs developed and demonstrated in the DARPA gyro development program.

  17. The magnetic shielding of the /sup 19/F nuclei in crystals of ZnF/sub 2/. 4H/sub 2/O and ZnFOH

    SciTech Connect

    Avkhutskii, L.M.; Kinchakov, V.S.; Petrenko, A.N.

    1982-03-01

    Results of the calculations of the magnetic shielding of flouride in the structure of ZnF/sub 2/ . 4H/sub 2/O and ZnFOH are discussed. It is shown that the magnetic shielding constraints are equal for the nonequivalent positions of the atoms F/sub 1/ and F/sub 2/, since their chemical environments are identical. By comparison, it is shown that orthogonalization of the atomic basis is comparatively unimportant for the diamagnetic component of the shielding, and increases the absolute magnitude of the paramagmetic component by a factor of approximately 1.5. An interesting feature is that allowance in the calculation for the hydrogen bonds between flourine and neighboring ''molecules'' in the crystal produces practically no change in the paramagnetic component and increases the diamagnetic component by approximately 130 units. The diagonal components of the shieding tensor, determined in the system of crystallographic axes, for the cluster ZnF/sub 2/ . 10H/sub 2/O are sigma/sub xx/=364.15, sigma/sub yy/=430.36, sigma/sub zz/=464.25 ppm. A noteworthy feature is that the magnetic shielding constants of fluorine in the structures of ZnFOH and ZnF/sub 2/ . 4H/sub 2/O are identical, and this is not due to an identical chemical environment for the fluorine nuclei in these crystals. The immediate environment is tetrahedral in both compounds, but in ZnF/sub 2/ . 4H/sub 2/O the coordination sphere also contains three hydrogen bonds, whereas in ZnFOH it contains three zinc atoms and one hydrogen bond.

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

    PubMed Central

    Liu, Yang; Liu, Zhaoxia; Yang, Huaxin

    2016-01-01

    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. PMID:27688925

  19. A comparative study of 1H and 19F Overhauser DNP in fluorinated benzenes.

    PubMed

    Neudert, Oliver; Mattea, Carlos; Spiess, Hans Wolfgang; Stapf, Siegfried; Münnemann, Kerstin

    2013-12-21

    Hyperpolarization techniques, such as Overhauser dynamic nuclear polarization (DNP), can provide a dramatic increase in the signal obtained from nuclear magnetic resonance experiments and may therefore enable new applications where sensitivity is a limiting factor. In this contribution, studies of the (1)H and (19)F Overhauser dynamic nuclear polarization enhancements at 345 mT are presented for three different aromatic solvents with the TEMPO radical for a range of radical concentrations. Furthermore, nuclear magnetic relaxation dispersion measurements of the same solutions are analyzed, showing contributions from dipolar and scalar coupling modulated by translational diffusion and different coupling efficiency for different solvents and nuclei. Measurements of the electron paramagnetic resonance linewidth are included to support the analysis of the DNP saturation factor for varying radical concentration. The results of our study give an insight into the characteristics of nitroxide radicals as polarizing agents for (19)F Overhauser DNP of aromatic fluorinated solvents. Furthermore, we compare our results with the findings of the extensive research on Overhauser DNP that was conducted in the past for a large variety of other radicals.

  20. CHARACTERIZATION OF TANK 19F SAMPLES

    SciTech Connect

    Oji, L.; Diprete, D.; Click, D.

    2009-12-17

    The Savannah River National Laboratory (SRNL) was asked by Liquid Waste Operations to characterize Tank 19F closure samples. Tank 19F slurry samples analyzed included the liquid and solid fractions derived from the slurry materials along with the floor scrape bottom Tank 19F wet solids. These samples were taken from Tank 19F in April 2009 and made available to SRNL in the same month. Because of limited amounts of solids observed in Tank 19F samples, the samples from the north quadrants of the tank were combined into one Tank 19F North Hemisphere sample and similarly the south quadrant samples were combined into one Tank 19F South Hemisphere sample. These samples were delivered to the SRNL shielded cell. The Tank 19F samples were analyzed for radiological, chemical and elemental components. Where analytical methods yielded additional contaminants other than those requested by the customer, these results were also reported. The target detection limits for isotopes analyzed were based on detection values of 1E-04 {micro}Ci/g for most radionuclides and customer desired detection values of 1E-05 {micro}Ci/g for I-129, Pa-231, Np-237, and Ra-226. While many of the target detection limits, as specified in the technical task request and task technical and quality assurance plans were met for the species characterized for Tank 19F, some were not met. In a number of cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. SRNL, in conjunction with the plant customer, reviewed all these cases and determined that the impacts were negligible.

  1. Nuclear magnetic resonance blood flowmeter

    SciTech Connect

    Battocletti, J.H.; Halbach, R.E.; Antonich, F.J.; Sances, A. Jr.; Knox, T.A.

    1986-09-23

    An improved nuclear magnetic resonance blood flowmeter is described for non-invasively measuring blood flow in a human limb comprising; polarizing magnet means for generating a substantially uniform magnetic field; a limb receiving lumen for supporting a human limb within the field generated by the polarizing magnet means so that blood molecules within the limb are magnetically polarized thereby; transmitter means located adjacent the lumen for inducing a nuclear magnetic resonance response in the blood molecules of the human limb disposed within the lumen; scanning means including: first means for generating a first pair of opposing magnetic fields within the lumen for cancelling the nuclear magnetic resonance response induced by the transmitter means everywhere except within a first null plane along which the first opposing magnetic fields cancel each other; second means for generating a second pair of opposing magnetic fields; and control means coupled to the first and second means for generating the first and second pair of opposing magnetic fields.

  2. nuclear magnetic resonance gyroscope

    SciTech Connect

    Karwacki, F. A.; Griffin, J.

    1985-04-02

    A nuclear magnetic resonance gyroscope which derives angular rotation thereof from the phases of precessing nuclear moments utilizes a single-resonance cell situated in the center of a uniform DC magnetic field. The field is generated by current flow through a circular array of coils between parallel plates. It also utilizes a pump and read-out beam and associated electronics for signal processing and control. Encapsulated in the cell for sensing rotation are odd isotopes of Mercury Hg/sup 199/ and Hg/sup 201/. Unpolarized intensity modulated light from a pump lamp is directed by lenses to a linear polarizer, quarter wave plate combination producing circularly polarized light. The circularly polarized light is reflected by a mirror to the cell transverse to the field for optical pumping of the isotopes. Unpolarized light from a readout lamp is directed by lenses to another linear polarizer. The linearly polarized light is reflected by another mirror to the cell transverse to the field and orthogonal to the pump lamp light. The linear light after transversing the cell strikes an analyzer where it is converted to an intensity-modulated light. The modulated light is detected by a photodiode processed and utilized as feedback to control the field and pump lamp excitation and readout of angular displacement.

  3. Nuclear Magnetic Resonance Gyroscope

    NASA Astrophysics Data System (ADS)

    Larsen, Michael; Bulatowicz, Michael; Clark, Philip; Griffith, Robert; Mirijanian, James; Pavell, James

    2015-05-01

    The Nuclear Magnetic Resonance Gyroscope (NMRG) is being developed by the Northrop Grumman Corporation (NGC). Cold and hot atom interferometer based gyroscopes have suffered from Size, Weight, and Power (SWaP) challenges and limits in bandwidth, scale factor stability, dead time, high rotation rate, vibration, and acceleration. NMRG utilizes the fixed precession rate of a nuclear spin in a constant magnetic field as a reference for determining rotation, providing continuous measurement, high bandwidth, stable scale factor, high rotation rate measurement, and low sensitivity to vibration and acceleration in a low SWaP package. The sensitivity to vibration has been partially tested and demonstrates no measured sensitivity within error bars. Real time closed loop implementation of the sensor significantly decreases environmental and systematic sensitivities and supports a compact and low power digital signal processing and control system. Therefore, the NMRG technology holds great promise for navigation grade performance in a low cost SWaP package. The poster will describe the history, operation, and design of the NMRG. General performance results will also be presented along with recent vibration test results.

  4. Single Nuclear Spin Magnetic Resonance Force Microscopy

    DTIC Science & Technology

    2010-05-02

    Lab. In work not directly supported by this grant, these projects advanced MRFM detected Ferromagnetic Resonance ( FMR ) to enable studies of...directly supported by this grant, these projects advanced MRFM detected Ferromagnetic Resonance ( FMR ) to enable studies of submicron magnetic structures...our earlier NMR detection of 19F spins in CaF2 we have conducted 65Cu, 63Cu NMR stud- ies for studies of interface phenomena in multilayered magnetic

  5. Detection of site-specific binding and co-binding of ligands to macromolecules using sup 19 F NMR

    SciTech Connect

    Jenkins, B.G. )

    1991-01-01

    Study of ligand-macromolecular interactions by {sup 19}F nuclear magnetic resonance (NMR) spectroscopy affords many opportunities for obtaining molecular biochemical and pharmaceutical information. This is due to the absence of a background fluorine signal, as well as the relatively high sensitivity of {sup 19}F NMR. Use of fluorine-labeled ligands enables one to probe not only binding and co-binding phenomena to macromolecules, but also can provide data on binding constants, stoichiometries, kinetics, and conformational properties of these complexes. Under conditions of slow exchange and macromolecule-induced chemical shifts, multiple {sup 19}F NMR resonances can be observed for free and bound ligands. These shifted resonances are a direct correlate of the concentration of ligand bound in a specific state rather than the global concentrations of bound or free ligand which are usually determined using other techniques such as absorption spectroscopy or equilibrium dialysis. Examples of these interactions are demonstrated both from the literature and from interactions of 5-fluorotryptophan, 5-fluorosalicylic acid, flurbiprofen, and sulindac sulfide with human serum albumin. Other applications of {sup 19}F NMR to study of these interactions in vivo, as well for receptor binding and metabolic tracing of fluorinated drugs and proteins are discussed.

  6. 19F-MRI for monitoring human NK cells in vivo

    PubMed Central

    Bouchlaka, Myriam N.; Ludwig, Kai D.; Gordon, Jeremy W.; Kutz, Matthew P.; Bednarz, Bryan P.; Fain, Sean B.; Capitini, Christian M.

    2016-01-01

    ABSTRACT The availability of clinical-grade cytokines and artificial antigen-presenting cells has accelerated interest in using natural killer (NK) cells as adoptive cellular therapy (ACT) for cancer. One of the technological shortcomings of translating therapies from animal models to clinical application is the inability to effectively and non-invasively track these cells after infusion in patients. We have optimized the nonradioactive isotope fluorine-19 (19F) as a means to label and track NK cells in preclinical models using magnetic resonance imaging (MRI). Human NK cells were expanded with interleukin (IL)-2 and labeled in vitro with increasing concentrations of 19F. Doses as low as 2 mg/mL 19F were detected by MRI. NK cell viability was only decreased at 8 mg/mL 19F. No effects on NK cell cytotoxicity against K562 leukemia cells were observed with 2, 4 or 8 mg/mL 19F. Higher doses of 19F, 4 mg/mL and 8 mg/mL, led to an improved 19F signal by MRI with 3 × 1011 19F atoms per NK cell. The 4 mg/mL 19F labeling had no effect on NK cell function via secretion of granzyme B or interferon gamma (IFNγ), compared to NK cells exposed to vehicle alone. 19F-labeled NK cells were detectable immediately by MRI after intratumoral injection in NSG mice and up to day 8. When 19F-labeled NK cells were injected subcutaneously, we observed a loss of signal through time at the site of injection suggesting NK cell migration to distant organs. The 19F perfluorocarbon is a safe and effective reagent for monitoring the persistence and trafficking of NK cell infusions in vivo, and may have potential for developing novel imaging techniques to monitor ACT for cancer. PMID:27467963

  7. Introduction to nuclear magnetic resonance.

    PubMed

    Mlynárik, Vladimír

    2016-05-19

    Nuclear magnetic resonance spectroscopy is a useful tool for studying normal and pathological biochemical processes in tissues. In this review, the principles of nuclear magnetic resonance and methods of obtaining nuclear magnetic resonance spectra are briefly outlined. The origin of the most important spectroscopic parameters-chemical shifts, coupling constants, longitudinal and transverse relaxation times, and spectroscopic line intensities-is explained, and the role of these parameters in interpretation of spectra is addressed. Basic methodological concepts of localized spectroscopy and spectroscopic imaging for the study of tissue metabolism in vivo are also described.

  8. Nuclear Magnetic Resonance

    NASA Astrophysics Data System (ADS)

    Reuhs, Bradley L.; Simsek, Senay

    Nuclear magnetic resonance (NMR) spectroscopy is a powerful analytical technique with a wide variety of applications. It may be used for complex structural studies, for protocol or process development, or as a simple quality assay for which structural information is important. It is nondestructive, and high-quality data may be obtained from milligram, even microgram, quantities of sample. Whereas other spectroscopy techniques may be used to determine the nature of the functional groups present in a sample, only NMR spectroscopy can provide the data necessary to determine the complete structure of a molecule. The applicability of NMR to food analysis has increased over the last three decades. In addition to improved instrumentation and much lower costs, very complex and specialized NMR techniques can now be routinely performed by a student or technician. These experiments can be set up with the click of a button/icon, as all the basic parameters are embedded into default experiment files listed in the data/work station software, and the results are obtained in a short time.

  9. Bioluminescence and 19F magnetic resonance imaging visualize the efficacy of lysostaphin alone and in combination with oxacillin against Staphylococcus aureus in murine thigh and catheter-associated infection models.

    PubMed

    Hertlein, Tobias; Sturm, Volker; Lorenz, Udo; Sumathy, K; Jakob, Peter; Ohlsen, Knut

    2014-01-01

    Staphylococci are the leading cause of hospital-acquired infections worldwide. Increasingly, they resist antibiotic treatment owing to the development of multiple antibiotic resistance mechanisms in most strains. Therefore, the activity and efficacy of recombinant lysostaphin as a drug against this pathogen have been evaluated. Lysostaphin exerts high levels of activity against antibiotic-resistant strains of Staphylococcus aureus, including methicillin-resistant S. aureus (MRSA). The therapeutic value of lysostaphin has been analyzed in two different clinically relevant in vivo models, a catheter-associated infection model and a thigh infection model. We infected mice with luciferase-expressing S. aureus Xen 29, and the efficacies of lysostaphin, vancomycin, oxacillin, and combined lysostaphin-oxacillin were investigated by determining numbers of CFU, detecting bioluminescent signals, and measuring the accumulation of perfluorocarbon emulsion at the site of infection by (19)F magnetic resonance imaging. Lysostaphin treatment significantly reduced the bacterial burden in infected thigh muscles and, after systemic spreading from the catheter, in inner organs. The efficiency of lysostaphin treatment was even more pronounced in combinatorial therapy with oxacillin. These results suggest that recombinant lysostaphin may have potential as an anti-S. aureus drug worthy of further clinical development. In addition, both imaging technologies demonstrated efficacy patterns similar to that of CFU determination, although they proved to be less sensitive. Nonetheless, they served as powerful tools to provide additional information about the course and gravity of infection in a noninvasive manner, possibly allowing a reduction in the number of animals needed for research evaluation of new antibiotics in future studies.

  10. Bioluminescence and 19F Magnetic Resonance Imaging Visualize the Efficacy of Lysostaphin Alone and in Combination with Oxacillin against Staphylococcus aureus in Murine Thigh and Catheter-Associated Infection Models

    PubMed Central

    Hertlein, Tobias; Sturm, Volker; Lorenz, Udo; Sumathy, K.; Jakob, Peter

    2014-01-01

    Staphylococci are the leading cause of hospital-acquired infections worldwide. Increasingly, they resist antibiotic treatment owing to the development of multiple antibiotic resistance mechanisms in most strains. Therefore, the activity and efficacy of recombinant lysostaphin as a drug against this pathogen have been evaluated. Lysostaphin exerts high levels of activity against antibiotic-resistant strains of Staphylococcus aureus, including methicillin-resistant S. aureus (MRSA). The therapeutic value of lysostaphin has been analyzed in two different clinically relevant in vivo models, a catheter-associated infection model and a thigh infection model. We infected mice with luciferase-expressing S. aureus Xen 29, and the efficacies of lysostaphin, vancomycin, oxacillin, and combined lysostaphin-oxacillin were investigated by determining numbers of CFU, detecting bioluminescent signals, and measuring the accumulation of perfluorocarbon emulsion at the site of infection by 19F magnetic resonance imaging. Lysostaphin treatment significantly reduced the bacterial burden in infected thigh muscles and, after systemic spreading from the catheter, in inner organs. The efficiency of lysostaphin treatment was even more pronounced in combinatorial therapy with oxacillin. These results suggest that recombinant lysostaphin may have potential as an anti-S. aureus drug worthy of further clinical development. In addition, both imaging technologies demonstrated efficacy patterns similar to that of CFU determination, although they proved to be less sensitive. Nonetheless, they served as powerful tools to provide additional information about the course and gravity of infection in a noninvasive manner, possibly allowing a reduction in the number of animals needed for research evaluation of new antibiotics in future studies. PMID:24366730

  11. Nuclear magnetic resonance imaging with 90-nm resolution.

    PubMed

    Mamin, H J; Poggio, M; Degen, C L; Rugar, D

    2007-05-01

    Magnetic resonance imaging (MRI) is a powerful imaging technique that typically operates on the scale of millimetres to micrometres. Conventional MRI is based on the manipulation of nuclear spins with radio-frequency fields, and the subsequent detection of spins with induction-based techniques. An alternative approach, magnetic resonance force microscopy (MRFM), uses force detection to overcome the sensitivity limitations of conventional MRI. Here, we show that the two-dimensional imaging of nuclear spins can be extended to a spatial resolution better than 100 nm using MRFM. The imaging of 19F nuclei in a patterned CaF(2) test object was enabled by a detection sensitivity of roughly 1,200 nuclear spins at a temperature of 600 mK. To achieve this sensitivity, we developed high-moment magnetic tips that produced field gradients up to 1.4 x 10(6) T m(-1), and implemented a measurement protocol based on force-gradient detection of naturally occurring spin fluctuations. The resulting detection volume was less than 650 zeptolitres. This is 60,000 times smaller than the previous smallest volume for nuclear magnetic resonance microscopy, and demonstrates the feasibility of pushing MRI into the nanoscale regime.

  12. 19F solid-state NMR spectroscopic investigation of crystalline and amorphous forms of a selective muscarinic M3 receptor antagonist, in both bulk and pharmaceutical dosage form samples.

    PubMed

    Wenslow, Robert M

    2002-05-01

    The purpose of the following investigation was to display the utility of 19F solid-state nuclear magnetic resonance (NMR) in both distinguishing between solid forms of a selective muscarinic M3 receptor antagonist and characterizing the active pharmaceutical ingredient in low-dose tablets. Ambient- and elevated-temperature solid-state 19F fast (15 kHz) magic-angle spinning (MAS) NMR experiments were employed to obtain desired spectral resolution in this system. Ambient sample temperature combined with rotor frequencies of 15 kHz provided adequate 19F peak resolution to successfully distinguish crystalline and amorphous forms in this system. Additionally, elevated-temperature 19F MAS NMR further characterized solid forms through 19F resonance narrowing brought about by the phenomenon of solvent escape. Similar solvent dynamics at elevated temperatures were utilized in combination with ambient-temperature 19F MAS NMR analysis to provide excipient-free spectra to unambiguously identify the active pharmaceutical ingredient (API) conversion from crystalline Form I to the amorphous form in low-dose tablets. It is shown that 19F solid-state NMR is exceptionally powerful in distinguishing amorphous and crystalline forms in both bulk and formulation samples.

  13. GHz nuclear magnetic resonance

    SciTech Connect

    Cross, T.A.; Drobny, G.; Trewhella, J.

    1994-12-01

    For the past dozen years, 500- and 600-MHz spectrometers have become available in many laboratories. The first 600-MHz NMR spectrometer (at Carnegie Mellon University) was commissioned more than 15 years ago and, until 1994, represented the highest field available for high-resolution NMR. This year, we have witnessed unprecedented progress in the development of very high field magnets for NMR spectroscopy, including the delivery of the first commercial 750-MHz NMR spectrometers. In addition, NMR signals have been obtained from 20-Tesla magnets (850 MHz for {sup 1}H`s) at both Los Alamos National Laboratory and Florida State University in the NHMFL (National High Magnetic Field Laboratory). These preliminary experiments have been performed in magnets with 100-ppm homogeneity, but a 20-Tesla magnet developed for the NHMFL will be brought to field this year with a projected homogeneity of 0.1 ppm over a 1-cm-diam spherical volume.

  14. Dual 19F/1H MR gene reporter molecules for in vivo detection of β-galactosidase

    PubMed Central

    Yu, Jian-Xin; Kodibagkar, Vikram D.; Hallac, Rami R.; Liu, Li; Mason, Ralph P.

    2012-01-01

    Increased emphasis on personalized medicine and novel therapies require the development of non-invasive strategies for assessing biochemistry in vivo. The detection of enzyme activity and gene expression in vivo is potentially important for the characterization of diseases and gene therapy. Magnetic resonance imaging (MRI) is a particularly promising tool since it is non-invasive, and has no associated radioactivity, yet penetrates deep tissue. We now demonstrate a novel class of dual 1H/19F nuclear magnetic resonance (NMR) lacZ gene reporter molecule to specifically reveal enzyme activity in human tumor xenografts growing in mice. We report the design, synthesis, and characterization of six novel molecules and evaluation of the most effective reporter in mice in vivo. Substrates show a single 19F NMR signal and exposure to β-galactosidase induces a large 19F NMR chemical shift response. In the presence of ferric ions the liberated aglycone generates intense proton MRI T2 contrast. The dual modality approach allows both the detection of substrate and imaging of product enhancing the confidence in enzyme detection. PMID:22352428

  15. Nuclear magnetic resonance scanners

    SciTech Connect

    Danby, G.T.; Hsieh, H.C.H.; Jackson, J.W.; Damadian, R.V.

    1988-08-23

    This patent describes a medical NMR scanner comprising a primary field magnet assembly including: (a) a ferromagnetic frame defining a patient-receiving space adapted to receive a human body, the frame having a pair of opposed polar regions aligned on a polar axis and disposed on opposite sides of the patient-receiving space, and the frame including a substantially continuous ferro-magnetic flux return path extending between the polar regions remote from the patient-receiving space; (b) flux-generating means including superconductive windings and cryostat means for maintaining the windings at superconducting temperatures; and (c) support means for maintaining the windings in proximity to the frame so that when a current passes through the windings magnetic flux emanating from the windings produces a magnetic field within the patient-receiving space and at least a portion of the flux passes into the patient-receiving space by way of the polar regions.

  16. (19)F Oximetry with semifluorinated alkanes.

    PubMed

    Kegel, Stefan; Chacon-Caldera, Jorge; Tsagogiorgas, Charalambos; Theisinger, Bastian; Glatting, Gerhard; Schad, Lothar R

    2016-12-01

    This work examines the variation of longitudinal relaxation rate R1(= 1/T1) of the (19)F-CF3-resonance of semifluorinated alkanes (SFAs) with oxygen tension (pO2), temperature (T) and pH in vitro. Contrary to their related perfluorocarbons (PFCs), SFA are amphiphilic and facilitate stable emulsions, a prerequisite for clinical use. A linear relationship between R1 and pO2 was confirmed for the observed SFAs at different temperatures. Using a standard saturation recovery sequence, T1 has been successfully measured using fluorine (19)F-MRI with a self-constructed birdcage resonator at 9.4 T. A calibration curve to calculate pO2 depending on T and R1 was found for each SFA used. In contrast to the commonly used PFC, SFAs are less sensitive to changes in pO2, but more sensitive to changes in temperature. The influence of pH to R1 was found to be negligible.

  17. Implementation of a modified birdcage resonator for 19F/1H MRI at low fields (0.14 T).

    PubMed

    Samaratunga, R C; Pratt, R G; Zhu, Y; Massoth, R J; Thomas, S R

    1994-05-01

    Fluorine-19 nuclear magnetic resonance of perfluorinated blood substitute materials provides a method for determination of oxygen tension (pO2) in vivo. Use of a double resonant 19F/1H radio frequency coil allows convenient correlation between the high resolution anatomic presentation of proton images and the fluorine distribution. However, quantitative 19F measurements require an RF coil with good H1 field homogeneity over the image volume and a high quality factor (Q) to minimize errors caused by the low signal-to-noise levels available in in vivo imaging and image nonuniformities introduced by the large chemical shift of fluorocarbons. The birdcage coil design provides a high Q structure with optimum H1 field uniformity and fill factor. However, at low resonance frequencies, the inherently low inductance of the birdcage geometry requires the use of a large number of chip capacitors giving rise to unwieldy coil fabrication and increased cost. This communication describes a modification to the birdcage design that reduces the chip capacitor requirement by at least a factor of 4 for a given dimension, yet retains the essential characteristics of the birdcage design. The modified structure was tuned for double resonance at 5.7/6.0 MHz for 19F/1H magnetic resonance imaging at 0.14 T. For a coil with a length to diameter ratio of 1.67, an H1 uniformity of +/- 2% for the 19F resonance was obtained over a cylindrical region with radius approximately 0.6r (r = radius of coil) and length approximately 1.8r within the coil.

  18. Theory of nuclear magnetic relaxation

    NASA Technical Reports Server (NTRS)

    Mcconnell, J.

    1983-01-01

    A theory of nuclear magnetic interaction is based on the study of the stochastic rotation operator. The theory is applied explicitly to relaxation by anisotropic chemical shift and to spin-rotational interactions. It is applicable also to dipole-dipole and quadrupole interactions.

  19. Simultaneous 19F-1H medium resolution NMR spectroscopy for online reaction monitoring

    NASA Astrophysics Data System (ADS)

    Zientek, Nicolai; Laurain, Clément; Meyer, Klas; Kraume, Matthias; Guthausen, Gisela; Maiwald, Michael

    2014-12-01

    Medium resolution nuclear magnetic resonance (MR-NMR) spectroscopy is currently a fast developing field, which has an enormous potential to become an important analytical tool for reaction monitoring, in hyphenated techniques, and for systematic investigations of complex mixtures. The recent developments of innovative MR-NMR spectrometers are therefore remarkable due to their possible applications in quality control, education, and process monitoring. MR-NMR spectroscopy can beneficially be applied for fast, non-invasive, and volume integrating analyses under rough environmental conditions. Within this study, a simple 1/16″ fluorinated ethylene propylene (FEP) tube with an ID of 0.04″ (1.02 mm) was used as a flow cell in combination with a 5 mm glass Dewar tube inserted into a benchtop MR-NMR spectrometer with a 1H Larmor frequency of 43.32 MHz and 40.68 MHz for 19F. For the first time, quasi-simultaneous proton and fluorine NMR spectra were recorded with a series of alternating 19F and 1H single scan spectra along the reaction time coordinate of a homogeneously catalysed esterification model reaction containing fluorinated compounds. The results were compared to quantitative NMR spectra from a hyphenated 500 MHz online NMR instrument for validation. Automation of handling, pre-processing, and analysis of NMR data becomes increasingly important for process monitoring applications of online NMR spectroscopy and for its technical and practical acceptance. Thus, NMR spectra were automatically baseline corrected and phased using the minimum entropy method. Data analysis schemes were designed such that they are based on simple direct integration or first principle line fitting, with the aim that the analysis directly revealed molar concentrations from the spectra. Finally, the performance of 1/16″ FEP tube set-up with an ID of 1.02 mm was characterised regarding the limit of detection (LOQ (1H) = 0.335 mol L-1 and LOQ (19F) = 0.130 mol L-1 for trifluoroethanol in

  20. (1)H and (19)F spin-lattice relaxation and CH3 or CF3 reorientation in molecular solids containing both H and F atoms.

    PubMed

    Beckmann, Peter A; Rheingold, Arnold L

    2016-04-21

    The dynamics of methyl (CH3) and fluoromethyl (CF3) groups in organic molecular (van der Waals) solids can be exploited to survey their local environments. We report solid state (1)H and (19)F spin-lattice relaxationexperiments in polycrystalline 3-trifluoromethoxycinnamic acid, along with an X-ray diffraction determination of the molecular and crystal structure, to investigate the intramolecular and intermolecular interactions that determine the properties that characterize the CF3 reorientation. The molecule is of no particular interest; it simply provides a motionless backbone (on the nuclear magnetic resonance(NMR) time scale) to investigate CF3 reorientation occurring on the NMR time scale. The effects of (19)F-(19)F and (19)F-(1)H spin-spin dipolar interactions on the complicated nonexponential NMRrelaxation provide independent inputs into determining a model for CF3 reorientation. As such, these experiments provide much more information than when only one spin species (usually (1)H) is present. In Sec. IV, which can be read immediately after the Introduction without reading the rest of the paper, we compare the barrier to CH3 and CF3 reorientation in seven organic solids and separate this barrier into intramolecular and intermolecular components.

  1. Wide-range nuclear magnetic resonance detector

    NASA Technical Reports Server (NTRS)

    Sturman, J. C.; Jirberg, R. J.

    1972-01-01

    Compact and easy to use solid state nuclear magnetic resonance detector is designed for measuring field strength to 20 teslas in cryogenically cooled magnets. Extremely low noise and high sensitivity make detector applicable to nearly all types of analytical nuclear magnetic resonance measurements and can be used in high temperature and radiation environments.

  2. Evidence of a structural phase transition in superconducting SmFeAsO1-xFx from 19F NMR

    NASA Astrophysics Data System (ADS)

    Majumder, M.; Ghoshray, K.; Mazumdar, C.; Poddar, A.; Ghoshray, A.; Berardan, D.; Dragoe, N.

    2013-01-01

    We report resistivity, magnetization and 19F NMR results in a polycrystalline sample of SmFeAsO0.86F0.14. The resistivity and magnetization data show a sharp drop at 48 K indicating a superconducting transition. The nuclear spin-lattice rate (1/T1) and spin-spin relaxation rate (1/T2) clearly show the existence of a structural phase transition near 163 K in the sample, which also undergoes a superconducting transition. This finding creates interest in exploring whether this is unique for Sm based systems or is also present in other rare-earth based 1111 superconductors.

  3. NUCLEAR MAGNETIC RELAXATION IN LIQUID METALS, ALLOYS, AND SALTS.

    DTIC Science & Technology

    NUCLEAR MAGNETIC RESONANCE, *ALKALI METAL ALLOYS, *LIQUID METALS, * SALTS , NUCLEAR MAGNETIC RESONANCE, NUCLEAR MAGNETIC RESONANCE, RELAXATION TIME... SODIUM , GALLIUM, SODIUM ALLOYS, THALLIUM, THALLIUM COMPOUNDS, MELTING, NUCLEAR SPINS, QUANTUM THEORY, OPERATORS(MATHEMATICS), BIBLIOGRAPHIES, INTEGRAL EQUATIONS, TEST EQUIPMENT, MATHEMATICAL ANALYSIS.

  4. Shiftless nuclear magnetic resonance spectroscopy.

    PubMed

    Wu, Chin H; Opella, Stanley J

    2008-02-07

    The acquisition and analysis of high resolution one- and two-dimensional solid-state nuclear magnetic resonance (NMR) spectra without chemical shift frequencies are described. Many variations of shiftless NMR spectroscopy are feasible. A two-dimensional experiment that correlates the dipole-dipole and dipole-dipole couplings in the model peptide , (15)N labeled N-acetyl-leucine is demonstrated. In addition to the resolution of resonances from individual sites in a single crystal sample, the bond lengths and angles are characterized by the two-dimensional powder pattern obtained from a polycrystalline sample.

  5. Evanescent Waves Nuclear Magnetic Resonance

    PubMed Central

    Halidi, El Mohamed; Nativel, Eric; Akel, Mohamad; Kenouche, Samir; Coillot, Christophe; Alibert, Eric; Jabakhanji, Bilal; Schimpf, Remy; Zanca, Michel; Stein, Paul; Goze-Bac, Christophe

    2016-01-01

    Nuclear Magnetic Resonance spectroscopy and imaging can be classified as inductive techniques working in the near- to far-field regimes. We investigate an alternative capacitive detection with the use of micrometer sized probes positioned at sub wavelength distances of the sample in order to characterize and model evanescent electromagnetic fields originating from NMR phenomenon. We report that in this experimental configuration the available NMR signal is one order of magnitude larger and follows an exponential decay inversely proportional to the size of the emitters. Those investigations open a new road to a better understanding of the evanescent waves component in NMR with the opportunity to perform localized spectroscopy and imaging. PMID:26751800

  6. Introduction to Nuclear Magnetic Resonance

    NASA Technical Reports Server (NTRS)

    Manatt, Stanley L.

    1985-01-01

    The purpose of this paper is to try to give a short overview of what the status is on nuclear magnetic resonance (NMR). It's a subject where one really has to spend some time to look at the physics in detail to develop a proper working understanding. I feel it's not appropriate to present to you density matrices, Hamiltonians of all sorts, and differential equations representing the motion of spins. I'm really going to present some history and status, and show a few very simple concepts involved in NMR. It is a form of radio frequency spectroscopy and there are a great number of nuclei that can be studied very usefully with the technique. NMR requires a magnet, a r.f. transmitter/receiver system, and a data acquisition system.

  7. 3-FG as substrate for investigating flux through the polyol pathway in dog lens by 19F-NMR spectroscopy.

    PubMed

    Lizak, M J; Secchi, E F; Lee, J W; Sato, S; Kubo, E; Akagi, Y; Kador, P F

    1998-12-01

    To investigate flux through the polyol pathway in the dog lens by 19F-nuclear magnetic resonance (19F-NMR) spectroscopy, using 3-fluoro-3-deoxy-D-glucose (3-FG) as a substrate. 3-FG metabolism was monitored by 19F-NMR analysis. Dog lenses were incubated in Dulbecco's modified Eagle's medium containing 10 mM 3-FG. Enzymatic reductase and dehydrogenase activities were spectrophotometrically determined, whereas the analyses of 3-FG metabolites were conducted by 19F-NMR analysis. Aldose reductase (AR) was immunohistochemically localized in dog lens with antibodies raised against dog kidney AR. 19F-NMR spectra indicate that incubation of purified dog lenses AR with 3-FG results in the formation of 3-fluoro-3-deoxy-D-sorbitol (3-FS) and that incubation of dog liver sorbitol dehydrogenase (SDH) with 3-FS results in the formation of 3-fluoro-3-deoxy-D-fructose (3-FF). This confirms that 3-FG is metabolized to 3-FF by the polyol pathway enzymes. The affinity (Km) of AR for 3-FG is approximately 20-fold better than that for D-glucose, whereas the Km of SDH for 3-FS was fourfold less than for D-sorbitol. 3-FG in cultured dog lenses is metabolized primarily to 3-FS; however, small amounts of 3-FF and 3-fluoro-3-deoxy-D-gluconic acid (3-FGA) are also formed. 3-FS formation was reduced by the AR inhibitor AL 1576, and 3-FF formation was eliminated by the SDH inhibitor CP-166,572. In dog lens epithelial cells cultured with 3-FG, only 3-FS is formed. Similarly, only 3-FS is formed when lens capsule containing primarily epithelial lens contaminated with superficial epithelial cells was incubated in 3-FG. Similar incubation of the remaining cortex resulted primarily in the formation of 3-FS and 3-FGA. This enzymatic distribution was confirmed by spectrophotometric activity analysis and the immunohistochemical localization of AR. The data confirm that flux through the polyol pathway primarily results in sorbitol accumulation. The absence of fructose and gluconic acid from cultured

  8. (19) F DOSY diffusion-NMR spectroscopy of fluoropolymers.

    PubMed

    Xu, Chenglong; Wan, Yingbo; Chen, Dongxue; Gao, Chun; Yin, Hongnan; Fetherston, Daniel; Kupce, Eriks; Lopez, Gerald; Ameduri, Bruno; Twum, Eric B; Wyzgoski, Faith J; Li, Xiaohong; McCord, Elizabeth F; Rinaldi, Peter L

    2017-05-01

    A new pulse sequence for obtaining (19) F detected DOSY (diffusion ordered spectroscopy) spectra of fluorinated molecules is presented and used to study fluoropolymers based on vinylidene fluoride and chlorotrifluoroethylene. The performance of (19) F DOSY NMR experiments (and in general any type of NMR experiment) on fluoropolymers creates some unique complications that very often prevent detection of important signals. Factors that create these complications include: (1) the presence of many scalar couplings among (1) H, (19) F and (13) C; (2) the large magnitudes of many (19) F homonuclear couplings (especially (2) JFF ); (3) the large (19) F chemical shift range; and (4) the low solubility of these materials (which requires that experiments be performed at high temperatures). A systematic study of the various methods for collecting DOSY NMR data, and the adaptation of these methods to obtain (19) F detected DOSY data, has been performed using a mixture of low molecular weight, fluorinated model compounds. The best pulse sequences and optimal experimental conditions have been determined for obtaining (19) F DOSY spectra. The optimum pulse sequences for acquiring (19) F DOSY NMR data have been determined for various circumstances taking into account the spectral dispersion, number and magnitude of couplings present, and experimental temperature. Pulse sequences and experimental parameters for optimizing these experiments for the study of fluoropolymers have been studied. Copyright © 2016 John Wiley & Sons, Ltd.

  9. Polarization quantum beat spectroscopy of HCF(A1A"). I. 19F and 1H hyperfine structure and Zeeman effect.

    PubMed

    Fan, Haiyan; Ionescu, Ionela; Xin, Ju; Reid, Scott A

    2004-11-08

    To further investigate the (19)F and (1)H nuclear hyperfine structure and Zeeman effect in the simplest singlet carbene, HCF, we recorded polarization quantum beat spectra (QBS) of the pure bending levels 2(0) (n) with n = 0-7 and combination bands 1(0) (1)2(0) (n) with n = 1-6 and 2(0) (n)3(0) (1) with n = 0-3 in the HCF A(1)A(")<--X(1)A(') system. The spectra were measured under jet-cooled conditions using a pulsed discharge source, both at zero field and under application of a weak magnetic field (<30 G). Analysis yielded the nuclear spin-rotation constants C(aa) and weak field Lande g(aa) factors. Consistent with a two-state model, the majority of observed vibrational levels exhibit a linear correlation of C(aa) and g(aa), and our analysis yielded effective (a) hyperfine constants for the (19)F and (1)H nuclei (in MHz) of 728(23) and 55(2), respectively. The latter was determined here owing to the high resolving power of QBS. The vibrational state selectivity of the (19)F hyperfine constants is discussed, and we suggest that the underlying Renner-Teller interaction may play an important role. Copyright 2004 American Institute of Physics.

  10. Microcoil nuclear magnetic resonance spectroscopy.

    PubMed

    Webb, A G

    2005-08-10

    In comparison with most analytical chemistry techniques, nuclear magnetic resonance has an intrinsically low sensitivity, and many potential applications are therefore precluded by the limited available quantity of certain types of sample. In recent years, there has been a trend, both commercial and academic, towards miniaturization of the receiver coil in order to increase the mass sensitivity of NMR measurements. These small coils have also proved very useful in coupling NMR detection with commonly used microseparation techniques. A further development enabled by small detectors is parallel data acquisition from many samples simultaneously, made possible by incorporating multiple receiver coils into a single NMR probehead. This review article summarizes recent developments and applications of "microcoil" NMR spectroscopy.

  11. Double-tuned radiofrequency coil for (19)F and (1)H imaging.

    PubMed

    Otake, Yosuke; Soutome, Yoshihisa; Hirata, Koji; Ochi, Hisaaki; Bito, Yoshitaka

    2014-01-01

    We developed a double-tuned radiofrequency (RF) coil using a novel circuit method to double tune for fluorine-19 (19F) and 1H magnetic resonance imaging, whose frequencies are very close to each other. The RF coil consists of 3 parallel-connected series inductor capacitor circuits. A computer simulation for our double-tuned RF coil with a phantom demonstrated that the coil has tuned resonant frequency and high sensitivity for both 19F and 1H. Drug distribution was visualized at 7 tesla using this RF coil and a rat administered perfluoro 15-crown-5-ether emulsion. The double-tune RF coil we developed may be a powerful tool for 19F and 1H imaging.

  12. NMR shielding and spin–rotation constants of {sup 175}LuX (X = {sup 19}F, {sup 35}Cl, {sup 79}Br, {sup 127}I) molecules

    SciTech Connect

    Demissie, Taye B.

    2015-12-31

    This presentation demonstrates the relativistic effects on the spin-rotation constants, absolute nuclear magnetic resonance (NMR) shielding constants and shielding spans of {sup 175}LuX (X = {sup 19}F, {sup 35}Cl, {sup 79}Br, {sup 127}I) molecules. The results are obtained from calculations performed using density functional theory (non-relativistic and four-component relativistic) and coupled-cluster calculations. The spin-rotation constants are compared with available experimental values. In most of the molecules studied, relativistic effects make an order of magnitude difference on the NMR absolute shielding constants.

  13. Different distribution of fluorinated anesthetics and nonanesthetics in model membrane: a 19F NMR study.

    PubMed Central

    Tang, P; Yan, B; Xu, Y

    1997-01-01

    Despite their structural resemblance, a pair of cyclic halogenated compounds, 1-chloro-1,2,2-trifluorocyclobutane (F3) and 1,2-dichlorohexafluorocyclobutane (F6), exhibit completely different anesthetic properties. Whereas the former is a potent general anesthetic, the latter produces no anesthesia. Two linear compounds, isoflurane and 2,3-dichlorooctofluorobutane (F8), although not a structural pair, also show the same anesthetic discrepancy. Using 19F nuclear magnetic spectroscopy, we investigated the time-averaged submolecular distribution of these compounds in a vesicle suspension of phosphatidylcholine lipids. A two-site exchange model was used to interpret the observed changes in resonance frequencies as a function of the solubilization of these compounds in membrane and in water. At clinically relevant concentrations, the anesthetics F3 and isoflurane distributed preferentially to regions of the membrane that permit easy contact with water. The frequency changes of these two anesthetics can be well characterized by the two-site exchange model. In contrast, the nonanesthetics F6 and F8 solubilized deeply into the lipid core, and their frequency change significantly deviated from the prediction of the model. It is concluded that although anesthetics and nonanesthetics may show similar hydrophobicity in bulk solvents such as olive oil, their distributions in various regions in biomembranes, and hence their effective concentrations at different submolecular sites, may differ significantly. PMID:9083671

  14. 19F-lanthanide complexes with increased sensitivity for 19F-MRI: optimization of the MR acquisition.

    PubMed

    Chalmers, Kirsten H; Kenwright, Alan M; Parker, David; Blamire, Andrew M

    2011-10-01

    Fluorine-19 magnetic resonance methods offer advantages for molecular or cellular imaging in vivo due to the absence of radioactivity, lack of naturally occurring background signal, and the ability to easily combine measurements with anatomical MRI. Previous studies have shown that (19) F-MRI sensitivity is limited to millimolar concentrations by slow longitudinal relaxation. In this study, a new class of macrocyclic fluorinated lanthanide complexes is investigated where relaxation rates are significantly shortened by proximity of the fluorine group to a paramagnetic lanthanide ion located within the same molecule. Longitudinal and transverse relaxation rates are field dependent and in the range 50-150 s(-1) and 70-200 s(-1), respectively, at 7 T. Relaxation rates in these complexes are a function of the molecular structure and are independent of concentration at biologically relevant levels, so can be used as criteria to optimize imaging acquisition. Phantom experiments at 7 T indicate a lower limit for detection by imaging of 20 μM.

  15. Development of (19)F-NMR chemical shift detection of DNA B-Z equilibrium using (19)F-NMR.

    PubMed

    Nakamura, S; Yang, H; Hirata, C; Kersaudy, F; Fujimoto, K

    2017-06-28

    Various DNA conformational changes are in correlation with biological events. In particular, DNA B-Z equilibrium showed a high correlation with translation and transcription. In this study, we developed a DNA probe containing 5-trifluoromethylcytidine or 5-trifluoromethylthymidine to detect DNA B-Z equilibrium using (19)F-NMR. Its probe enabled the quantitative detection of B-, Z-, and ss-DNA based on (19)F-NMR chemical shift change.

  16. Through-space (19)F-(19)F spin-spin coupling in ortho-fluoro Z-azobenzene.

    PubMed

    Rastogi, Shiva K; Rogers, Robert A; Shi, Justin; Brown, Christopher T; Salinas, Cindy; Martin, Katherine M; Armitage, Jacob; Dorsey, Christopher; Chun, Gao; Rinaldi, Peter; Brittain, William J

    2016-02-01

    We report through-space (TS) (19)F-(19)F coupling for ortho-fluoro-substituted Z-azobenzenes. The magnitude of the TS-coupling constant ((TS) JFF ) ranged from 2.2-5.9 Hz. Using empirical formulas reported in the literature, these coupling constants correspond to non-bonded F-F distances (dFF) of 3.0-3.5 Å. These non-bonded distances are significantly smaller than those determined by X-ray crystallography or density functional theory, which argues that simple models of (19)F-(19)F TS spin-spin coupling solely based dFF are not applicable. (1)H, (13)C and (19)F data are reported for both the E and Z isomers of ten fluorinated azobenzenes. Density functional theory [B3YLP/6-311++G(d,p)] was used to calculate (19) F chemical shifts, and the calculated values deviated 0.3-10.0 ppm compared with experimental values. Copyright © 2015 John Wiley & Sons, Ltd.

  17. An improved nuclear magnetic resonance spectrometer

    NASA Technical Reports Server (NTRS)

    Elleman, D. D.; Manatt, S. L.

    1967-01-01

    Cylindrical sample container provides a high degree of nuclear stabilization to a nuclear magnetic resonance /nmr/ spectrometer. It is placed coaxially about the nmr insert and contains reference sample that gives a signal suitable for locking the field and frequency of an nmr spectrometer with a simple audio modulation system.

  18. Nuclear Magnetic Resonance Technology for Medical Studies

    NASA Astrophysics Data System (ADS)

    Budinger, Thomas F.; Lauterbur, Paul C.

    1984-10-01

    Nuclear magnetic resonance proton imaging provides anatomical definition of normal and abnormal tissues with a contrast and detection sensitivity superior to those of x-ray computed tomography in the human head and pelvis and parts of the cardiovascular and musculoskeletal systems. Recent improvements in technology should lead to advances in diagnostic imaging of the breast and regions of the abdomen. Selected-region nuclear magnetic resonance spectroscopy of protons, carbon-13, and phosphorus-31 has developed into a basic science tool for in vivo studies on man and a unique tool for clinical diagnoses of metabolic disorders. At present, nuclear magnetic resonance is considered safe if access to the magnet environment is controlled. Technological advances employing field strengths over 2 teslas will require biophysical studies of heating and static field effects.

  19. Solid-state 19F-NMR analysis of 19F-labeled tryptophan in gramicidin A in oriented membranes.

    PubMed Central

    Grage, Stephan L; Wang, Junfeng; Cross, Timothy A; Ulrich, Anne S

    2002-01-01

    The response of membrane-associated peptides toward the lipid environment or other binding partners can be monitored by solid-state NMR of suitably labeled side chains. Tryptophan is a prominent amino acid in transmembrane helices, and its (19)F-labeled analogues are generally biocompatible and cause little structural perturbation. Hence, we use 5F-Trp as a highly sensitive NMR probe to monitor the conformation and dynamics of the indole ring. To establish this (19)F-NMR strategy, gramicidin A was labeled with 5F-Trp in position 13 or 15, whose chi(1)/chi(2) torsion angles are known from previous (2)H-NMR studies. First, the alignment of the (19)F chemical shift anisotropy tensor within the membrane was deduced by lineshape analysis of oriented samples. Next, the three principal axes of the (19)F chemical shift anisotropy tensor were assigned within the molecular frame of the indole ring. Finally, determination of chi(1)/chi(2) for 5F-Trp in the lipid gel phase showed that the side chain alignment differs by up to 20 degrees from its known conformation in the liquid crystalline state. The sensitivity gain of (19)F-NMR and the reduction in the amount of material was at least 10-fold compared with previous (2)H-NMR studies on the same system and 100-fold compared with (15)N-NMR. PMID:12496101

  20. Nuclear magnetic resonance contrast agents

    DOEpatents

    Smith, P.H.; Brainard, J.R.; Jarvinen, G.D.; Ryan, R.R.

    1997-12-30

    A family of contrast agents for use in magnetic resonance imaging and a method of enhancing the contrast of magnetic resonance images of an object by incorporating a contrast agent of this invention into the object prior to forming the images or during formation of the images. A contrast agent of this invention is a paramagnetic lanthanide hexaazamacrocyclic molecule, where a basic example has the formula LnC{sub 16}H{sub 14}N{sub 6}. Important applications of the invention are in medical diagnosis, treatment, and research, where images of portions of a human body are formed by means of magnetic resonance techniques. 10 figs.

  1. Nuclear magnetic resonance contrast agents

    DOEpatents

    Smith, Paul H.; Brainard, James R.; Jarvinen, Gordon D.; Ryan, Robert R.

    1997-01-01

    A family of contrast agents for use in magnetic resonance imaging and a method of enhancing the contrast of magnetic resonance images of an object by incorporating a contrast agent of this invention into the object prior to forming the images or during formation of the images. A contrast agent of this invention is a paramagnetic lanthanide hexaazamacrocyclic molecule, where a basic example has the formula LnC.sub.16 H.sub.14 N.sub.6. Important applications of the invention are in medical diagnosis, treatment, and research, where images of portions of a human body are formed by means of magnetic resonance techniques.

  2. Clonal distribution of pneumococcal serotype 19F isolates from Ghana.

    PubMed

    Sparding, Nadja; Dayie, Nicholas T K D; Mills, Richael O; Newman, Mercy J; Dalsgaard, Anders; Frimodt-Møller, Niels; Slotved, Hans-Christian

    2015-04-01

    Streptococcus pneumoniae is a major cause of morbidity and mortality worldwide. Pneumococcal strains are classified according to their capsular polysaccharide and more than 90 different serotypes are currently known. In this project, three distinct groups of pneumococcal carriage isolates from Ghana were investigated; isolates from healthy children in Tamale and isolates from both healthy and children attending the outpatient department at a hospital in Accra. The isolates were previously identified and characterized by Gram staining, serotyping and susceptibility to penicillin. In this study, isolates of the common serotype 19F were further investigated by Multi-Locus Sequence Typing (MLST). Overall, 14 different Sequence Types (STs) were identified by MLST, of which nine were novel based on the international MLST database. Two clones within serotype 19F seem to circulate in Ghana, a known ST (ST 4194) and a novel ST (ST 9090). ST 9090 was only found in healthy children in Accra, whereas ST 4194 was found equally in all children studied. In the MLST database, other isolates of ST 4194 were also associated with serotype 19F, and these isolates came from other West African countries. The majority of isolates were penicillin intermediate resistant. In conclusion, two clones within serotype 19F were found to be dominating in pneumococcal carriage in Accra and Tamale in Ghana. Furthermore, it seems as though the clonal distribution of serotype 19F may be different from what is currently known in Ghana in that many new clones were identified. This supports the importance of continued monitoring of pneumococcal carriage in Ghana and elsewhere when vaccines, e.g., PCV-13, have been introduced to monitor the possible future spread of antimicrobial resistant clones.

  3. Magnetic fusion driventransmutation of nuclear waste (FTW)

    SciTech Connect

    Peng, Yueng Kay Martin; Cheng, E.T.

    1993-01-01

    The possibility of magnetic Fusion driven Transmutation of Waste (FTW) was revisted and discussed recently. Nuclear wastes include all transuranium elements: Pu isotopes, minor actinides separated from the spent fission fuel, and fissile products. Elimination of thse long-life nuclear wastes is necessary for the long-term viability of fission power. A Small Business Innovative Research program has been initiated under the leadership of TSI Research to examine the efficacy of fusion transmutation of waste utilizing small fusion drivers.

  4. Novel fluorinated ligands for gold nanoparticle labelling with applications in (19)F-MRI.

    PubMed

    Michelena, Olatz; Padro, Daniel; Carrillo-Carrión, Carolina; Del Pino, Pablo; Blanco, Jorge; Arnaiz, Blanca; Parak, Wolfgang J; Carril, Mónica

    2017-02-21

    Novel fluorinated ligands for gold nanoparticle labelling have been designed and synthesised. Several types of gold nanoparticles have been prepared in the presence of these fluorinated ligands alone, or in combination with non-fluorinated ligands. Their colloidal stability in water and other solvents was tested and the magnetic resonance properties of the so-obtained nanoparticles were also assessed in detail. (1)H and (19)F-NMR spectra were evaluated and MRI phantoms of the most promising nanoparticles were successfully measured in (19)F-MRI. The MRI signal to noise ratio was related to the fluorine concentration and compared with ICP-MS data to correlate the real concentration of fluorine grafted onto the nanoparticles with the actually active fluorine in MRI.

  5. Determining diffusion coefficients of ionic liquids by means of field cycling nuclear magnetic resonance relaxometry.

    PubMed

    Kruk, D; Meier, R; Rachocki, A; Korpała, A; Singh, R K; Rössler, E A

    2014-06-28

    Field Cycling Nuclear Magnetic Resonance (FC NMR) relaxation studies are reported for three ionic liquids: 1-ethyl-3- methylimidazolium thiocyanate (EMIM-SCN, 220-258 K), 1-butyl-3-methylimidazolium tetrafluoroborate (BMIM-BF4, 243-318 K), and 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF6, 258-323 K). The dispersion of (1)H spin-lattice relaxation rate R1(ω) is measured in the frequency range of 10 kHz-20 MHz, and the studies are complemented by (19)F spin-lattice relaxation measurements on BMIM-PF6 in the corresponding frequency range. From the (1)H relaxation results self-diffusion coefficients for the cation in EMIM-SCN, BMIM-BF4, and BMIM-PF6 are determined. This is done by performing an analysis considering all relevant intra- and intermolecular relaxation contributions to the (1)H spin-lattice relaxation as well as by benefiting from the universal low-frequency dispersion law characteristic of Fickian diffusion which yields, at low frequencies, a linear dependence of R1 on square root of frequency. From the (19)F relaxation both anion and cation diffusion coefficients are determined for BMIM-PF6. The diffusion coefficients obtained from FC NMR relaxometry are in good agreement with results reported from pulsed- field-gradient NMR. This shows that NMR relaxometry can be considered as an alternative route of determining diffusion coefficients of both cations and anions in ionic liquids.

  6. Fluorine-19 nuclear magnetic resonance and biochemical characterization of fluorotyrosine-labeled-thymidylate-synthetase

    NASA Astrophysics Data System (ADS)

    Rosson, Dan; Lewis, Charles A.; Ellis, Paul D.; Dunlap, R. Bruce

    1994-03-01

    Fluorotyrosine has been incorporated into thymidylate synthetase from Lactobacillus casei by growth of the bacterium in media containing 3-fluorotyrosine. The enzyme exhibited a specific activity 70% of that of the normal enzyme and formed a covalent binary complex with pyrimidine nucleotides, as well as a covalent ternary complex with 5-fluorodeoxyuridylate and 5,10-methylenetetrahydrofolate. 19F nuclear magnetic resonance spectroscopy has been used to follow the formation of these complexes. 5-Fluorodeoxyuridylate, dUMP, dTMP and dCMP produced identical conformational changes in the enzyme as monitored by the fluorotyrosyl resonances. Ternary complex formation of the fluorotyrosine-containing enzyme with 5-fluorodeoxyuridylate and 5,10-methylenetetrahydrofolate resulted in further spectral changes.

  7. Nuclear Magnetic Resonance Technology for Medical Studies.

    ERIC Educational Resources Information Center

    Budinger, Thomas F.; Lauterbur, Paul C.

    1984-01-01

    Reports on the status of nuclear magnetic resonance (NMR) from theoretical and clinical perspectives, reviewing NMR theory and relaxation parameters relevant to NMR imaging. Also reviews literature related to modern imaging strategies, signal-to-noise ratio, contrast agents, in vivo spectroscopy, spectroscopic imaging, clinical applications, and…

  8. Sample spinner for nuclear magnetic resonance spectrometer

    SciTech Connect

    Stejskal, E.O.

    1984-05-01

    A sample spinner for a nuclear magnetic resonance spectrometer having improved operating characteristics is described comprising a rotor supported at both ends by support gas bearings and positioned by a thrust gas bearing. Improved support gas bearings are also described which result in a spinner exhibiting long-term stable operation characteristics.

  9. Nuclear Magnetic Resonance Technology for Medical Studies.

    ERIC Educational Resources Information Center

    Budinger, Thomas F.; Lauterbur, Paul C.

    1984-01-01

    Reports on the status of nuclear magnetic resonance (NMR) from theoretical and clinical perspectives, reviewing NMR theory and relaxation parameters relevant to NMR imaging. Also reviews literature related to modern imaging strategies, signal-to-noise ratio, contrast agents, in vivo spectroscopy, spectroscopic imaging, clinical applications, and…

  10. Nuclear Magnetic Resonance Imaging. South Carolina Health Service Area 2

    SciTech Connect

    Not Available

    1984-12-01

    Contents include: Nuclear Magnetic Resonance Imaging (NMRI); (Clinical applications, Magnet types, Comparisons with other systems, Manpower, Manufacturers, Contraindications); Analysis of systems; (Availability, Accessibility, Cost, Quality, Continuity, Acceptability).

  11. Using fluorine nuclear magnetic resonance to probe the interaction of membrane-active peptides with the lipid bilayer.

    PubMed

    Buer, Benjamin C; Chugh, Jeetender; Al-Hashimi, Hashim M; Marsh, E Neil G

    2010-07-13

    A variety of biologically active peptides exert their function through direct interactions with the lipid membrane of the cell. These surface interactions are generally transient and highly dynamic, making them hard to study. Here we have examined the feasibility of using solution phase (19)F nuclear magnetic resonance (NMR) to study peptide-membrane interactions. Using the antimicrobial peptide MSI-78 as a model system, we demonstrate that peptide binding to either small unilamellar vesicles (SUVs) or bicelles can readily be detected by simple one-dimensional (19)F NMR experiments with peptides labeled with l-4,4,4-trifluoroethylglycine. The (19)F chemical shift associated with the peptide-membrane complex is sensitive both to the position of the trifluoromethyl reporter group (whether in the hydrophobic face or positively charged face of the amphipathic peptide) and to the curvature of the lipid bilayer (whether the peptide is bound to SUVs or bicelles). (19)F spin echo experiments using the Carr-Purcell-Meiboom-Gill pulse sequence were used to measure the transverse relaxation (T(2)) of the nucleus and thereby examine the local mobility of the MSI-78 analogues bound to bicelles. The fluorine probe positioned in the hydrophobic face of the peptide relaxes at a rate that correlates with the tumbling of the bicelle, suggesting that it is relatively immobile, whereas the probe at the positively charged face relaxes more slowly, indicating this position is much more dynamic. These results are in accord with structural models of MSI-78 bound to lipids and point to the feasibility of using fluorine-labeled peptides to monitor peptide-membrane interactions in living cells.

  12. Fluorine (19F) MRS and MRI in biomedicine

    PubMed Central

    Ruiz-Cabello, Jesús; Barnett, Brad P.; Bottomley, Paul A.; Bulte, Jeff W.M.

    2011-01-01

    Shortly after the introduction of 1H MRI, fluorinated molecules were tested as MR-detectable tracers or contrast agents. Many fluorinated compounds, which are nontoxic and chemically inert, are now being used in a broad range of biomedical applications, including anesthetics, chemotherapeutic agents, and molecules with high oxygen solubility for respiration and blood substitution. These compounds can be monitored by fluorine (19F) MRI and/or MRS, providing a noninvasive means to interrogate associated functions in biological systems. As a result of the lack of endogenous fluorine in living organisms, 19F MRI of ‘hotspots’ of targeted fluorinated contrast agents has recently opened up new research avenues in molecular and cellular imaging. This includes the specific targeting and imaging of cellular surface epitopes, as well as MRI cell tracking of endogenous macrophages, injected immune cells and stem cell transplants. PMID:20842758

  13. Calculation of optimal parameters for 19F MRI

    NASA Astrophysics Data System (ADS)

    Anisimov, N.; Gulaev, M.; Pavlova, O.; Fomina, D.; Glukhova, V.; Batova, S.; Pirogov, Yu

    2017-08-01

    This paper presents a method for optimizing the parameters of the scanning pulse sequences for MRI in relation to objects with a wide NMR spectrum. In this case, a broadband excitation of the spin system is difficult because of hardware limitations. It is proposed to apply the selective excitation, the optimum parameters of which are calculated by an algorithm that uses information concerning the NMR spectrum. The method is especially useful for 19F MRI of fluorocarbons.

  14. Nuclear magnetic resonance studies of lens transparency

    SciTech Connect

    Beaulieu, C.F.

    1989-01-01

    Transparency of normal lens cytoplasm and loss of transparency in cataract were studied by nuclear magnetic resonance (NMR) methods. Phosphorus ({sup 31}P) NMR spectroscopy was used to measure the {sup 31}P constituents and pH of calf lens cortical and nuclear homogenates and intact lenses as a function of time after lens enucleation and in opacification produced by calcium. Transparency was measured with laser spectroscopy. Despite complete loss of adenosine triphosphate (ATP) within 18 hrs of enucleation, the homogenates and lenses remained 100% transparent. Additions of calcium to ATP-depleted cortical homogenates produced opacification as well as concentration-dependent changes in inorganic phosphate, sugar phosphates, glycerol phosphorylcholine and pH. {sup 1}H relaxation measurements of lens water at 200 MHz proton Larmor frequency studied temperature-dependent phase separation of lens nuclear homogenates. Preliminary measurements of T{sub 1} and T{sub 2} with non-equilibrium temperature changes showed a change in the slope of the temperature dependence of T{sub 1} and T{sub 2} at the phase separation temperature. Subsequent studies with equilibrium temperature changes showed no effect of phase separation on T{sub 1} or T{sub 2}, consistent with the phase separation being a low-energy process. {sup 1}H nuclear magnetic relaxation dispersion (NMRD) studies (measurements of the magnetic field dependence of the water proton 1/T{sub 1} relaxation rates) were performed on (1) calf lens nuclear and cortical homogenates (2) chicken lens homogenates, (3) native and heat-denatured egg white and (4) pure proteins including bovine {gamma}-II crystallin bovine serum albumin (BSA) and myoglobin. The NMRD profiles of all samples exhibited decreases in 1/T{sub 1} with increasing magnetic field.

  15. Optically pumped nuclear magnetic resonance of semiconductors.

    PubMed

    Hayes, Sophia E; Mui, Stacy; Ramaswamy, Kannan

    2008-02-07

    Optically pumped NMR (OPNMR) of direct gap and indirect gap semiconductors has been an area of active research interest, motivated by both basic science and technological perspectives. Proposals to enhance and to spatially localize nuclear polarization have stimulated interest in this area. Recent progress in OPNMR has focused on exploring the experimental parameter space in order to elucidate details of the underlying photophysics of optical pumping phenomena. The focus of this review is on recent studies of bulk samples of GaAs and InP, namely, the photon energy dependence, the magnetic field dependence, and the phase dependence of OPNMR resonances. Models for the development of nuclear polarization are discussed.

  16. Conformational isomerism in solid state of AMG 853--structure studies using solid-state nuclear magnetic resonance and X-ray diffraction.

    PubMed

    Kiang, Y-H; Nagapudi, Karthik; Wu, Tian; Peterson, Matthew L; Jona, Janan; Staples, Richard J; Stephens, Peter W

    2015-07-01

    Investigation of an additional resonance peak in the (19) F solid-state nuclear magnetic resonance (NMR) spectrum of AMG 853, a dual antagonist of DP and CRTH2 previously in clinical development for asthma, has led to the identification of two conformational isomers coexisting in the crystal lattice in a continuous composition range between 89.7%:10.3% and 96.5%:3.5%. These two isomers differ in the chloro-flurorophenyl moiety orientation-the aromatic ring is flipped by 180° in these two isomers. The level of the minor isomer is directly measured through integration of the two peaks in the (19) F solid-state NMR spectrum. The values obtained from the NMR data are in excellent agreement with the degree of disorder of the fluorine atom in the crystal structure, refined using both single-crystal and high-resolution powder X-ray diffraction data.

  17. [Nuclear magnetic resonance in psychiatry].

    PubMed

    Hamad, H

    1993-01-01

    Magnetic Resonance Imaging (MRI) is a more recent technique than computerized tomography (CT), with which morphological, high quality, three-dimensional images can be obtained, it is capable of differentiating gray/white matter without patients' exposure to radiation. Clinical investigation studies demonstrate the following findings: In Schizophrenics: Enlargement of lateral ventricles volume in 67-73%, in naive patients 21-33%. The increase of the third ventricle varies from 19 to 73%, whose patients have significant flat affect. The temporal lobe gray matter is reduced, including amygdala-hippocampal complex, and parahippocampal gyrus. No specific corpus callosum results are concluded. There is cortical atrophy, specially of bilateral prefrontal regions. Basal ganglia (lenticular and caudate nuclei) are increased. The prefrontal, temporal and limbic dysfunction supports the abnormal connection hypothesis in schizophrenics. Basal ganglia also are involved in the pathogenesis of the disease. Clinical cortical atrophy symptoms are demonstrated by neuropsychological tests, although some cognitive deficits are remediable. Perinatal complications are more frequent, in children who will be schizophrenics, than their siblings (23.6% vs 12.8%); those of special interest are: toxemia, prematurity, long labor, jaundice and bleeding during pregnancy. In affective Bipolar Disorders: There is increase (19-50%) in the number of focal signal hyperintensities at the lateral limits of ventricles and in both hemispheres, and a trend towards larger ventricular size. The temporal lobe is smaller bilaterally, but the right side is 15% larger; its volume correlates negatively with long-term illness in males. In Unipolar Disorder an increase of frontal white matter T1 values is registered.(ABSTRACT TRUNCATED AT 250 WORDS)

  18. Magnetic nuclear core restraint and control

    DOEpatents

    Cooper, Martin H.

    1979-01-01

    A lateral restraint and control system for a nuclear reactor core adaptable to provide an inherent decrease of core reactivity in response to abnormally high reactor coolant fluid temperatures. An electromagnet is associated with structure for radially compressing the core during normal reactor conditions. A portion of the structures forming a magnetic circuit are composed of ferromagnetic material having a curie temperature corresponding to a selected coolant fluid temperature. Upon a selected signal, or inherently upon a preselected rise in coolant temperature, the magnetic force is decreased a given amount sufficient to relieve the compression force so as to allow core radial expansion. The expanded core configuration provides a decreased reactivity, tending to shut down the nuclear reaction.

  19. Magnetic nuclear core restraint and control

    DOEpatents

    Cooper, Martin H.

    1978-01-01

    A lateral restraint and control system for a nuclear reactor core adaptable to provide an inherent decrease of core reactivity in response to abnormally high reactor coolant fluid temperatures. An electromagnet is associated with structure for radially compressing the core during normal reactor conditions. A portion of the structures forming a magnetic circuit are composed of ferromagnetic material having a curie temperature corresponding to a selected coolant fluid temperature. Upon a selected signal, or inherently upon a preselected rise in coolant temperature, the magnetic force is decreased a given amount sufficient to relieve the compression force so as to allow core radial expansion. The expanded core configuration provides a decreased reactivity, tending to shut down the nuclear reaction.

  20. Magnetic-field cycling instrumentation for dynamic nuclear polarization-nuclear magnetic resonance using photoexcited triplets.

    PubMed

    Kagawa, Akinori; Negoro, Makoto; Takeda, Kazuyuki; Kitagawa, Masahiro

    2009-04-01

    To advance static solid-state NMR with hyperpolarized nuclear spins, a system has been developed enabling dynamic nuclear polarization (DNP) using electron spins in the photoexcited triplet state with X-band microwave apparatus, followed by static solid-state nuclear magnetic resonance (NMR) experiments using the polarized nuclear-spin system with a goniometer. In order to perform the DNP and NMR procedures in different magnetic fields, the DNP system and the NMR system are spatially separated, between which the sample can be shuttled while its orientation is controlled in a reproducible fashion. We demonstrate that the system developed in this work is operational for solid-state NMR with hyperpolarized nuclear-spin systems in static organic materials, and also discuss the application of our system.

  1. Nuclear magnetic moments and related sum rules

    SciTech Connect

    Bentz, Wolfgang; Arima, Akito

    2011-05-06

    We first review the history and our present understanding of nuclear magnetic moments and Gamow-Teller transitions, with emphasis on the roles of configuration mixing and meson exchange currents. Then we discuss the renormalization of the orbital g-factor in nuclei, and its relation to the E1 sum rule for photoabsorption and the M1 sum rule for the scissors mode of deformed nuclei.

  2. Hot magnetized nuclear matter: Thermodynamic and saturation properties

    NASA Astrophysics Data System (ADS)

    Rezaei, Z.; Bordbar, G. H.

    2017-03-01

    We have used a realistic nuclear potential, AV_{18}, and a many-body technique, the lowest-order constraint variational (LOCV) approach, to calculate the properties of hot magnetized nuclear matter. By investigating the free energy, spin polarization parameter, and symmetry energy, we have studied the temperature and magnetic field dependence of the saturation properties of magnetized nuclear matter. In addition, we have calculated the equation of state of magnetized nuclear matter at different temperatures and magnetic fields. It was found that the flashing temperature of nuclear matter decreases by increasing the magnetic field. In addition, we have studied the effect of the magnetic field on liquid gas phase transition of nuclear matter. The liquid gas coexistence curves, the order parameter of the liquid gas phase transition, and the properties of critical point at different magnetic fields have been calculated.

  3. Nuclear magnetic resonance properties of lunar samples.

    NASA Technical Reports Server (NTRS)

    Kline, D.; Weeks, R. A.

    1972-01-01

    Nuclear magnetic resonance spectra of Na-23, Al-27, and P-31 in fines samples 10084,60 and 14163,168 and in crystalline rock samples 12021,55 and 14321,166, have been recorded over a range of frequencies up to 20 MHz. A shift in the field at which maximum absorption occurs for all of the spectra relative to the field at which maximum absorption occurs for terrestrial analogues is attributed to a sample-dependent magnetic field at the Na, Al, and P sites opposing the laboratory field. The magnitude of these fields internal to the samples is sample dependent and varies from 5 to 10 G. These fields do not correlate with the iron content of the samples. However, the presence of single-domain particles of iron distributed throughout the plagioclase fraction that contains the principal fraction of Na and Al is inferred from electron magnetic resonance spectra shapes.

  4. Mapping phosphorylation rate of fluoro-deoxy-glucose in rat brain by (19)F chemical shift imaging.

    PubMed

    Coman, Daniel; Sanganahalli, Basavaraju G; Cheng, David; McCarthy, Timothy; Rothman, Douglas L; Hyder, Fahmeed

    2014-05-01

    (19)F magnetic resonance spectroscopy (MRS) studies of 2-fluoro-2-deoxy-d-glucose (FDG) and 2-fluoro-2-deoxy-d-glucose-6-phosphate (FDG-6P) can be used for directly assessing total glucose metabolism in vivo. To date, (19)F MRS measurements of FDG phosphorylation in the brain have either been achieved ex vivo from extracted tissue or in vivo by unusually long acquisition times. Electrophysiological and functional magnetic resonance imaging (fMRI) measurements indicate that FDG doses up to 500 mg/kg can be tolerated with minimal side effects on cerebral physiology and evoked fMRI-BOLD responses to forepaw stimulation. In halothane-anesthetized rats, we report localized in vivo detection and separation of FDG and FDG-6P MRS signals with (19)F 2D chemical shift imaging (CSI) at 11.7 T. A metabolic model based on reversible transport between plasma and brain tissue, which included a non-saturable plasma to tissue component, was used to calculate spatial distribution of FDG and FDG-6P concentrations in rat brain. In addition, spatial distribution of rate constants and metabolic fluxes of FDG to FDG-6P conversion were estimated. Mapping the rate of FDG to FDG-6P conversion by (19)F CSI provides an MR methodology that could impact other in vivo applications such as characterization of tumor pathophysiology. Copyright © 2014 Elsevier Inc. All rights reserved.

  5. STATISTICAL ANALYSIS OF TANK 19F FLOOR SAMPLE RESULTS

    SciTech Connect

    Harris, S.

    2010-09-02

    Representative sampling has been completed for characterization of the residual material on the floor of Tank 19F as per the statistical sampling plan developed by Harris and Shine. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples results to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL95%) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current scrape sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 19F. The uncertainty is quantified in this report by an UCL95% on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL95% was based entirely on the six current scrape sample results (each averaged across three analytical determinations).

  6. Nuclear magnetic resonance imaging of liver hemangiomas

    SciTech Connect

    Sigal, R.; Lanir, A.; Atlan, H.; Naschitz, J.E.; Simon, J.S.; Enat, R.; Front, D.; Israel, O.; Chisin, R.; Krausz, Y.

    1985-10-01

    Nine patients with cavernous hemangioma of the liver were examined by nuclear magnetic resonance imaging (MRI) with a 0.5 T superconductive magnet. Spin-echo technique was used with varying time to echo (TE) and repetition times (TR). Results were compared with /sup 99m/Tc red blood cell (RBC) scintigraphy, computed tomography (CT), echography, and arteriography. Four illustrated cases are reported. It was possible to establish a pattern for MRI characteristics of cavernous hemangiomas; rounded or smooth lobulated shape, marked increase in T1 and T2 values as compared with normal liver values. It is concluded that, although more experience is necessary to compare the specificity with that of ultrasound and CT, MRI proved to be very sensitive for the diagnosis of liver hemangioma, especially in the case of small ones which may be missed by /sup 99m/Tc-labeled RBC scintigraphy.

  7. QED theory of the nuclear magnetic shielding in hydrogenlike ions.

    PubMed

    Yerokhin, V A; Pachucki, K; Harman, Z; Keitel, C H

    2011-07-22

    The shielding of the nuclear magnetic moment by the bound electron in hydrogenlike ions is calculated ab initio with inclusion of relativistic, nuclear, and quantum electrodynamics (QED) effects. The QED correction is evaluated to all orders in the nuclear binding strength parameter and, independently, to the first order in the expansion in this parameter. The results obtained lay the basis for the high-precision determination of nuclear magnetic dipole moments from measurements of the g factor of hydrogenlike ions.

  8. High resolution ¹⁹F{¹H} nuclear magnetic resonance spectroscopy and liquid chromatography-solid phase extraction-offline ¹H nuclear magnetic resonance spectroscopy for conclusive detection and identification of cyanide in water samples.

    PubMed

    Mazumder, Avik; Kumar, Ajeet; Dubey, Devendra K

    2013-04-05

    We report herein a new, sensitive and efficient method for detection, identification and quantification of cyanide in water samples. Cyanide was converted (>95% yield) to its versatile and stable derivative, 1-cyano-2,2,2-trifluoro-1-phenylethyl acetate (CTPA).The crude reaction mixture was directly subjected to high resolution fluorine-19 nuclear magnetic resonance ((19)F{(1)H} NMR) spectroscopy. In order to do away with signal overlap and dynamic range problems associated with (1)H NMR spectroscopy, liquid chromatography with UV detection hyphenated to online solid phase extraction (LC-UV-SPE) was performed. The trapped and enriched CTPA was thereafter subjected to offline (1)H NMR spectroscopy. In this way the δ(1)H, δ(19)F spectral signatures and LC-UV retention time were used for specific detection and identification and quantification of cyanide. The three techniques (viz. LC-UV and LC-UV-SPE followed by offline (1)H NMR and (19)F{(1)H} NMR spectroscopy) demonstrated good linearity (r(2)>0.99), reproducibility (inter-day RSD: 1.43-1.89%, 2.60-2.80%, 1.42-1.60; intra-day: RSD 1.20-1.38%, 3.21-3.25%, 1.00-1.19%), accuracy (recoveries: 95.1-97.2%, 77.5-82.8%, 96.8-98.9%) and LODs (1.31 μg/mL, 4.24 μg/mL, and 2.14 μg/mL) respectively. Total time required for the analysis was ∼3 h. Utility of the method was demonstrated by the detection and identification of spiked water samples. Since the derivative CTPA was volatile, could also be analyzed by GC-MS and GC-FTIR instruments. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Determining diffusion coefficients of ionic liquids by means of field cycling nuclear magnetic resonance relaxometry

    SciTech Connect

    Kruk, D.; Meier, R.; Rössler, E. A.; Rachocki, A.; Korpała, A.; Singh, R. K.

    2014-06-28

    Field Cycling Nuclear Magnetic Resonance (FC NMR) relaxation studies are reported for three ionic liquids: 1-ethyl-3- methylimidazolium thiocyanate (EMIM-SCN, 220–258 K), 1-butyl-3-methylimidazolium tetrafluoroborate (BMIM-BF{sub 4}, 243–318 K), and 1-butyl-3-methylimidazolium hexafluorophosphate (BMIM-PF{sub 6}, 258–323 K). The dispersion of {sup 1}H spin-lattice relaxation rate R{sub 1}(ω) is measured in the frequency range of 10 kHz–20 MHz, and the studies are complemented by {sup 19}F spin-lattice relaxation measurements on BMIM-PF{sub 6} in the corresponding frequency range. From the {sup 1}H relaxation results self-diffusion coefficients for the cation in EMIM-SCN, BMIM-BF{sub 4}, and BMIM-PF{sub 6} are determined. This is done by performing an analysis considering all relevant intra- and intermolecular relaxation contributions to the {sup 1}H spin-lattice relaxation as well as by benefiting from the universal low-frequency dispersion law characteristic of Fickian diffusion which yields, at low frequencies, a linear dependence of R{sub 1} on square root of frequency. From the {sup 19}F relaxation both anion and cation diffusion coefficients are determined for BMIM-PF{sub 6}. The diffusion coefficients obtained from FC NMR relaxometry are in good agreement with results reported from pulsed- field-gradient NMR. This shows that NMR relaxometry can be considered as an alternative route of determining diffusion coefficients of both cations and anions in ionic liquids.

  10. An introduction to nuclear magnetic resonance in biomedicine.

    PubMed

    Andrew, E R

    1990-02-01

    In this paper the author illustrates the historical aspects of the development, first, of the fundamental principles of nuclear magnetic resonance and, second, the extension of these principles to magnetic resonance imaging and in vivo spectroscopy.

  11. Tracking Perfluorocarbon Nanoemulsion Delivery by 19F MRI for Precise High Intensity Focused Ultrasound Tumor Ablation

    PubMed Central

    Shin, Soo Hyun; Park, Eun-Joo; Min, Changki; Choi, Sun Il; Jeon, Soyeon; Kim, Yun-Hee; Kim, Daehong

    2017-01-01

    Perfluorocarbon nanoemulsions (PFCNEs) have recently been undergoing rigorous study to investigate their ability to improve the therapeutic efficacy of tumor ablation by high intensity focused ultrasound (HIFU). For precise control of PFCNE delivery and thermal ablation, their accumulation and distribution in a tumor should be quantitatively analyzed. Here, we used fluorine-19 (19F) magnetic resonance imaging (MRI) to quantitatively track PFCNE accumulation in a tumor, and analyzed how intra-tumoral PFCNE quantities affect the therapeutic efficacy of HIFU treatment. Ablation outcomes were assessed by intra-voxel incoherent motion analysis and bioluminescent imaging up to 14 days after the procedure. Assessment of PFCNE delivery and treatment outcomes showed that 2-3 mg/mL of PFCNE in a tumor produces the largest ablation volume under the same HIFU insonation conditions. Histology showed varying degrees of necrosis depending on the amount of PFCNE delivered. 19F MRI promises to be a valuable platform for precisely guiding PFCNE-enhanced HIFU ablation of tumors. PMID:28255351

  12. Simple and Inexpensive Classroom Demonstrations of Nuclear Magnetic Resonance and Magnetic Resonance Imaging.

    ERIC Educational Resources Information Center

    Olson, Joel A.; Nordell, Karen J.; Chesnik, Marla A.; Landis, Clark R.; Ellis, Arthur B.; Rzchowski, M. S.; Condren, S. Michael; Lisensky, George C.

    2000-01-01

    Describes a set of simple, inexpensive, classical demonstrations of nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) principles that illustrate the resonance condition associated with magnetic dipoles and the dependence of the resonance frequency on environment. (WRM)

  13. Simple and Inexpensive Classroom Demonstrations of Nuclear Magnetic Resonance and Magnetic Resonance Imaging.

    ERIC Educational Resources Information Center

    Olson, Joel A.; Nordell, Karen J.; Chesnik, Marla A.; Landis, Clark R.; Ellis, Arthur B.; Rzchowski, M. S.; Condren, S. Michael; Lisensky, George C.

    2000-01-01

    Describes a set of simple, inexpensive, classical demonstrations of nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) principles that illustrate the resonance condition associated with magnetic dipoles and the dependence of the resonance frequency on environment. (WRM)

  14. Spatial localization in nuclear magnetic resonance spectroscopy.

    PubMed

    Keevil, Stephen F

    2006-08-21

    The ability to select a discrete region within the body for signal acquisition is a fundamental requirement of in vivo NMR spectroscopy. Ideally, it should be possible to tailor the selected volume to coincide exactly with the lesion or tissue of interest, without loss of signal from within this volume or contamination with extraneous signals. Many techniques have been developed over the past 25 years employing a combination of RF coil properties, static magnetic field gradients and pulse sequence design in an attempt to meet these goals. This review presents a comprehensive survey of these techniques, their various advantages and disadvantages, and implications for clinical applications. Particular emphasis is placed on the reliability of the techniques in terms of signal loss, contamination and the effect of nuclear relaxation and J-coupling. The survey includes techniques based on RF coil and pulse design alone, those using static magnetic field gradients, and magnetic resonance spectroscopic imaging. Although there is an emphasis on techniques currently in widespread use (PRESS, STEAM, ISIS and MRSI), the review also includes earlier techniques, in order to provide historical context, and techniques that are promising for future use in clinical and biomedical applications.

  15. Pharmaceutical Applications of Relaxation Filter-Selective Signal Excitation Methods for ¹⁹F Solid-State Nuclear Magnetic Resonance: Case Study With Atorvastatin in Dosage Formulation.

    PubMed

    Asada, Mamiko Nasu; Nemoto, Takayuki; Mimura, Hisashi

    2016-03-01

    We recently developed several new relaxation filter-selective signal excitation (RFS) methods for (13)C solid-state nuclear magnetic resonance (NMR) that allow (13)C signal extraction of the target components from pharmaceuticals. These methods were successful in not only qualification but also quantitation over the wide range of 5% to 100%. Here, we aimed to improve the sensitivity of these methods and initially applied them to (19)F solid-state NMR, on the basis that the fluorine atom is one of the most sensitive NMR-active nuclei. For testing, we selected atorvastatin calcium (ATC), an antilipid BCS class II drug that inhibits 3-hydroxy-3-methylglutaryl-coenzyme A reductase and is marketed in crystalline and amorphous forms. Tablets were obtained from 2 generic drug suppliers, and the ATC content occurred mainly as an amorphous form. Using the RFS method with (19)F solid-state NMR, we succeeded in qualifying trace amounts (less than 0.5% w/w level) of crystalline phase (Form I) of ATC in the tablets. RFS methods with (19)F solid-state NMR are practical and time efficient and can contribute not only to the study of pharmaceutical drugs, including those with small amounts of a highly potent active ingredient within a formulated product, but also to the study of fluoropolymers in material sciences. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  16. In vivo 19F MRI for cell tracking.

    PubMed

    Srinivas, Mangala; Boehm-Sturm, Philipp; Aswendt, Markus; Pracht, Eberhard D; Figdor, Carl G; de Vries, I Jolanda; Hoehn, Mathias

    2013-11-25

    In vivo (19)F MRI allows quantitative cell tracking without the use of ionizing radiation. It is a noninvasive technique that can be applied to humans. Here, we describe a general protocol for cell labeling, imaging, and image processing. The technique is applicable to various cell types and animal models, although here we focus on a typical mouse model for tracking murine immune cells. The most important issues for cell labeling are described, as these are relevant to all models. Similarly, key imaging parameters are listed, although the details will vary depending on the MRI system and the individual setup. Finally, we include an image processing protocol for quantification. Variations for this, and other parts of the protocol, are assessed in the Discussion section. Based on the detailed procedure described here, the user will need to adapt the protocol for each specific cell type, cell label, animal model, and imaging setup. Note that the protocol can also be adapted for human use, as long as clinical restrictions are met.

  17. Small-Volume Nuclear Magnetic Resonance Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fratila, Raluca M.; Velders, Aldrik H.

    2011-07-01

    Nuclear magnetic resonance (NMR) spectroscopy is one of the most information-rich analytical techniques available. However, it is also inherently insensitive, and this drawback precludes the application of NMR spectroscopy to mass- and volume-limited samples. We review a particular approach to increase the sensitivity of NMR experiments, namely the use of miniaturized coils. When the size of the coil is reduced, the sample volume can be brought down to the nanoliter range. We compare the main coil geometries (solenoidal, planar, and microslot/stripline) and discuss their applications to the analysis of mass-limited samples. We also provide an overview of the hyphenation of microcoil NMR spectroscopy to separation techniques and of the integration with lab-on-a-chip devices and microreactors.

  18. In vivo nuclear magnetic resonance imaging

    NASA Technical Reports Server (NTRS)

    Leblanc, A.; Evans, H.; Bryan, R. N.; Johnson, P.; Schonfeld, E.; Jhingran, S. G.

    1984-01-01

    A number of physiological changes have been demonstrated in bone, muscle and blood after exposure of humans and animals to microgravity. Determining mechanisms and the development of effective countermeasures for long duration space missions is an important NASA goal. The advent of tomographic nuclear magnetic resonance imaging (NMR or MRI) gives NASA a way to greatly extend early studies of this phenomena in ways not previously possible; NMR is also noninvasive and safe. NMR provides both superb anatomical images for volume assessments of individual organs and quantification of chemical/physical changes induced in the examined tissues. The feasibility of NMR as a tool for human physiological research as it is affected by microgravity is demonstrated. The animal studies employed the rear limb suspended rat as a model of mucle atrophy that results from microgravity. And bedrest of normal male subjects was used to simulate the effects of microgravity on bone and muscle.

  19. Nuclear magnetic resonance imaging of the spine

    SciTech Connect

    Modic, M.T.; Weinstein, M.A.; Pavlicek, W.; Starnes, D.L.; Duchesneau, P.M.; Boumphrey, F.; Hardy, R.J. Jr.

    1984-01-01

    Forty subjects were examined to determine the accuracy and clinical usefulness of nuclear magnetic resonance (NMR) examination of the spine. The NMR images were compared with plain radiographs, high-resolution computed tomograms, and myelograms. The study included 15 patients with normal spinal cord anatomy and 25 patients whose pathological conditions included canal stenosis, herniated discs, metastatic tumors, primary cord tumor, trauma, Chiari malformations, syringomyelia, and developmental disorders. Saturation recovery images were best in differentiating between soft tissue and cerebrospinal fluid. NMR was excellent for the evaluation of the foramen magnum region and is presently the modality of choice for the diagnosis of syringomyelia and Chiari malformation. NMR was accurate in diagnosing spinal cord trauma and spinal canal block.

  20. Nuclear magnetic resonance spectrometer and method

    SciTech Connect

    Peterson, P.E.; Vidrine, D.W.

    1981-08-18

    A nuclear magnetic resonance techniis described that allows simultaneous temperature determination and spectral acquisition. The technique employs a modification of the lock circuit of a varian xl-100 spectrometer which permits accurate measurement of the difference in resonance frequency between a primary lock nucleus and another , secondary, nucleus. The field stabilization function of the main lock circuit is not compromised. A feedback signal having a frequency equal to the frequency difference is substituted for the normal power supply in the spectrometer's existing radio frequency transmitter to modulate that transmitter. Thus, the transmitter's radio frequency signal is enhanced in a frequency corresponding to the resonance peak of the secondary nucleus. Determination of the frequency difference allows the determination of temperature without interference with the observed spectrum. The feedback character of the circuit and the presence of noise make the circuit self-activating.

  1. Geochemical Controls on Nuclear Magnetic Resonance Measurements

    SciTech Connect

    Knight, Rosemary; Prasad, Manika; Keating, Kristina

    2003-11-11

    OAK-B135 Our research objectives are to determine, through an extensive set of laboratory experiments, the effect of the specific mineralogic form of iron and the effect of the distribution of iron on proton nuclear magnetic resonance (NMR) relaxation mechanisms. In the first nine months of this project, we have refined the experimental procedures to be used in the acquisition of the laboratory NMR data; have ordered, and conducted preliminary measurements on, the sand samples to be used in the experimental work; and have revised and completed the theoretical model to use in this project. Over the next year, our focus will be on completing the first phase of the experimental work where the form and distribution of the iron in the sands in varied.

  2. Nuclear magnetic resonance imaging in medicine

    PubMed Central

    McKinstry, C S

    1986-01-01

    Using the technique of nuclear magnetic resonance (NMR, MR, MRI), the first images displaying pathology in humans were published in 1980.1 Since then, there has been a rapid extension in the use of the technique, with an estimated 225 machines in use in the USA at the end of 1985.2 Considerable enthusiasm has been expressed for this new imaging technique,3 although awareness of its high cost in the present economic climate has led to reservations being expressed in other quarters.2 The aim of this article is to give an outline of the present state of NMR, and indicate some possible future developments. ImagesFig 1Fig 2Fig 3(a)Fig 3 (b)Fig 4Fig 5Fig 6Fig 7 (a)Fig 7 (b)Fig 8Fig 9Fig 10 PMID:3811023

  3. (13)C and (19)F solid-state NMR and X-ray crystallographic study of halogen-bonded frameworks featuring nitrogen-containing heterocycles.

    PubMed

    Szell, Patrick M J; Gabriel, Shaina A; Gill, Russell D D; Wan, Shirley Y H; Gabidullin, Bulat; Bryce, David L

    2017-03-01

    Halogen bonding is a noncovalent interaction between the electrophilic region of a halogen (σ-hole) and an electron donor. We report a crystallographic and structural analysis of halogen-bonded compounds by applying a combined X-ray diffraction (XRD) and solid-state nuclear magnetic resonance (SSNMR) approach. Single-crystal XRD was first used to characterize the halogen-bonded cocrystals formed between two fluorinated halogen-bond donors (1,4-diiodotetrafluorobenzene and 1,3,5-trifluoro-2,4,6-triiodobenzene) and several nitrogen-containing heterocycles (acridine, 1,10-phenanthroline, 2,3,5,6-tetramethylpyrazine, and hexamethylenetetramine). New structures are reported for the following three cocrystals, all in the P21/c space group: acridine-1,3,5-trifluoro-2,4,6-triiodobenzene (1/1), C6F3I3·C13H9N, 1,10-phenanthroline-1,3,5-trifluoro-2,4,6-triiodobenzene (1/1), C6F3I3·C12H8N2, and 2,3,5,6-tetramethylpyrazine-1,3,5-trifluoro-2,4,6-triiodobenzene (1/1), C6F3I3·C8H12N2. (13)C and (19)F solid-state magic-angle spinning (MAS) NMR is shown to be a convenient method to characterize the structural features of the halogen-bond donor and acceptor, with chemical shifts attributable to cocrystal formation observed in the spectra of both nuclides. Cross polarization (CP) from (19)F to (13)C results in improved spectral sensitivity in characterizing the perfluorinated halogen-bond donor when compared to conventional (1)H CP. Gauge-including projector-augmented wave density functional theory (GIPAW DFT) calculations of magnetic shielding constants, along with optimization of the XRD structures, provide a final set of structures in best agreement with the experimental (13)C and (19)F chemical shifts. Data for carbons bonded to iodine remain outliers due to well-known relativistic effects.

  4. 31P and 19F NMR studies of glycophorin-reconstituted membranes: preferential interaction of glycophorin with phosphatidylserine

    SciTech Connect

    Ong, R.L.

    1984-01-01

    Glycophorin A, a major glycoprotein of the erythrocyte membrane, has been incorporated into small unilamellar vesicles composed of a variety of pure and mixed phospholipids. Nuclear spin labels including 31P and 19F have been used at natural abundance or have been synthetically incorporated in lipids to act as probes of lipid-protein interaction. Interactions produce broadening of resonances in several cases and it can be used to demonstrate preferential interaction of certain lipids with glycophorin. 31P and 19F probes show a strong preferential interaction of glycophorin with phosphatidylserine over phosphatidylcholine. There is some evidence that interactions are more pronounced at the inner surface of the bilayer and these results are rationalized in terms of the asymmetric distribution of protein and lipid.

  5. Nuclear magnetic resonance techniques in medicine.

    PubMed

    Bradbury, E M; Radda, G K; Allen, P S

    1983-04-01

    Nuclear magnetic resonance (NMR) techniques are now finding exciting new noninvasive applications in medicine. There are two major approaches. The first is as an analytical technique using 31P NMR spectroscopy for the identification and quantitation of the more abundant phosphate metabolites in various tissues. Changes in the levels of these metabolites and in intracellular cytoplasmic pH can be followed in various ischemic and hypoxic conditions to monitor metabolic response to stress situations and to diagnose inborn errors of metabolism. The second major approach is an entirely different application of NMR techniques and uses 1H, the nucleus most abundant in biological tissues, largely in water and fats, to produce NMR images of any section of the body. By applying non-uniform magnetic fields across a section of the body, hydrogen nuclei in different elemental volumes in the section are tagged with different frequencies and their signals can be processed to give an image of the section. In contrast to computed tomographic scanning, NMR has particularly powerful application in the imaging of soft tissues.

  6. 19F NMR study of the equilibria and dynamics of the Al3+/F- system.

    PubMed

    Bodor, A; Tóth, I; Bányai, I; Szabó, Z; Hefter, G T

    2000-06-12

    A careful reinvestigation by high-field 19F NMR (470 MHz) spectroscopy has been made of the Al3+/F- system in aqueous solution under carefully controlled conditions of pH, concentration, ionic strength (I), and temperature. The 19F NMR spectra show five distinct signals at 278 K and I = 0.6 M (TMACl) which have been attributed to the complexes AlFi(3-i)+(aq) with i < or = 5. There was no need to invoke AlFi(OH)j(3-i-j)+ mixed complexes in the model under our experimental conditions (pH < or = 6.5), nor was any evidence obtained for the formation of AlF6(3-)(aq) at very high ratios of F-/Al3+. The stepwise equilibrium constants obtained for the complexes by integration of the 19F signals are in good agreement with literature data given the differences in medium and temperature. In I = 0.6 M TMACl at 278 K and in I = 3 M KCl at 298 K the log Ki values are 6.42, 5.41, 3.99, 2.50, and 0.84 (for species i = 1-5) and 6.35, 5.25, and 4.11 (for species i = 1-3), respectively. Disappearance of the 19F NMR signals under certain conditions was shown to be due to precipitation. Certain 19F NMR signals exhibit temperature- and concentration-dependent exchange broadening. Detailed line shape analysis of the spectra and magnetization transfer measurements indicate that the kinetics are dominated by F- exchange rather than complex formation. The detected reactions and their rate constants are AlF2(2+) + *F- reversible AlF*F2+ + F- (k02 = (1.8 +/- 0.3) x 10(6) M-1 s-1), AlF3(0) + *F- reversible AlF2*F0 + F- (k03 = (3.9 +/- 0.9) x 10(6) M-1 s-1), and AlF3(0) + H*F reversible AlF2*F0 + HF (kH03 = (6.6 +/- 0.5) x 10(4) M-1 s-1). The rates of these exchange reactions increase markedly with increasing F- substitution. Thus, the reactions of AlF2+(aq) were too inert to be detected even on the T1 NMR time scale, while some of the reactions of AlF3(0)(aq) were fast, causing large line broadening. The ligand exchange appears to follow an associative interchange mechanism. The cis

  7. Dynamic nuclear polarization at high magnetic fields

    PubMed Central

    Maly, Thorsten; Debelouchina, Galia T.; Bajaj, Vikram S.; Hu, Kan-Nian; Joo, Chan-Gyu; Mak–Jurkauskas, Melody L.; Sirigiri, Jagadishwar R.; van der Wel, Patrick C. A.; Herzfeld, Judith; Temkin, Richard J.; Griffin, Robert G.

    2009-01-01

    Dynamic nuclear polarization (DNP) is a method that permits NMR signal intensities of solids and liquids to be enhanced significantly, and is therefore potentially an important tool in structural and mechanistic studies of biologically relevant molecules. During a DNP experiment, the large polarization of an exogeneous or endogeneous unpaired electron is transferred to the nuclei of interest (I) by microwave (μw) irradiation of the sample. The maximum theoretical enhancement achievable is given by the gyromagnetic ratios (γe/γl), being ∼660 for protons. In the early 1950s, the DNP phenomenon was demonstrated experimentally, and intensively investigated in the following four decades, primarily at low magnetic fields. This review focuses on recent developments in the field of DNP with a special emphasis on work done at high magnetic fields (≥5 T), the regime where contemporary NMR experiments are performed. After a brief historical survey, we present a review of the classical continuous wave (cw) DNP mechanisms—the Overhauser effect, the solid effect, the cross effect, and thermal mixing. A special section is devoted to the theory of coherent polarization transfer mechanisms, since they are potentially more efficient at high fields than classical polarization schemes. The implementation of DNP at high magnetic fields has required the development and improvement of new and existing instrumentation. Therefore, we also review some recent developments in μw and probe technology, followed by an overview of DNP applications in biological solids and liquids. Finally, we outline some possible areas for future developments. PMID:18266416

  8. BROADBAND EXCITATION IN NUCLEAR MAGNETIC RESONANCE

    SciTech Connect

    Tycko, R.

    1984-10-01

    Theoretical methods for designing sequences of radio frequency (rf) radiation pulses for broadband excitation of spin systems in nuclear magnetic resonance (NMR) are described. The sequences excite spins uniformly over large ranges of resonant frequencies arising from static magnetic field inhomogeneity, chemical shift differences, or spin couplings, or over large ranges of rf field amplitudes. Specific sequences for creating a population inversion or transverse magnetization are derived and demonstrated experimentally in liquid and solid state NMR. One approach to broadband excitation is based on principles of coherent averaging theory. A general formalism for deriving pulse sequences is given, along with computational methods for specific cases. This approach leads to sequences that produce strictly constant transformations of a spin system. The importance of this feature in NMR applications is discussed. A second approach to broadband excitation makes use of iterative schemes, i.e. sets of operations that are applied repetitively to a given initial pulse sequences, generating a series of increasingly complex sequences with increasingly desirable properties. A general mathematical framework for analyzing iterative schemes is developed. An iterative scheme is treated as a function that acts on a space of operators corresponding to the transformations produced by all possible pulse sequences. The fixed points of the function and the stability of the fixed points are shown to determine the essential behavior of the scheme. Iterative schemes for broadband population inversion are treated in detail. Algebraic and numerical methods for performing the mathematical analysis are presented. Two additional topics are treated. The first is the construction of sequences for uniform excitation of double-quantum coherence and for uniform polarization transfer over a range of spin couplings. Double-quantum excitation sequences are demonstrated in a liquid crystal system. The

  9. (1) H-(19) F REDOR-filtered NMR spin diffusion measurements of domain size in heterogeneous polymers.

    PubMed

    Sorte, Eric G; Alam, Todd M

    2017-06-02

    Solid state NMR spectroscopy is inherently sensitive to chemical structure and composition and thus makes an ideal method to probe the heterogeneity of multicomponent polymers. Specifically, NMR spin diffusion experiments can be used to extract reliable information about spatial domain sizes on multiple length scales, provided that magnetization selection of one domain can be achieved. In this paper, we demonstrate the preferential filtering of protons in fluorinated domains during NMR spin diffusion experiments using (1) H-(19) F heteronuclear dipolar dephasing based on rotational echo double resonance (REDOR) MAS NMR techniques. Three pulse sequence variations are demonstrated based on the different nuclei detected: direct (1) H detection, plus both (1) H➔(13) C cross polarization and (1) H➔(19) F cross polarization detection schemes. This (1) H-(19) F REDOR-filtered spin diffusion method was used to measure fluorinated domain sizes for a complex polymer blend. The efficacy of the REDOR-based spin filter does not rely on spin relaxation behavior or chemical shift differences and thus is applicable for performing NMR spin diffusion experiments in samples where traditional magnetization filters may prove unsuccessful. This REDOR-filtered NMR spin diffusion method can also be extended to other samples where a heteronuclear spin pair exists that is unique to the domain of interest. Copyright © 2017 John Wiley & Sons, Ltd.

  10. Combining insights from solid-state NMR and first principles calculation: applications to the 19F NMR of octafluoronaphthalene.

    PubMed

    Robbins, Andrew J; Ng, William T K; Jochym, Dominik; Keal, Thomas W; Clark, Stewart J; Tozer, David J; Hodgkinson, Paul

    2007-05-21

    Advances in solid-state NMR methodology and computational chemistry are applied to the (19)F NMR of solid octafluoronaphthalene. It is demonstrated experimentally, and confirmed by density functional theory (DFT) calculations, that the spectral resolution in the magic-angle spinning spectrum is limited by the anisotropy of the bulk magnetic susceptibility (ABMS). This leads to the unusual observation that the resolution improves as the sample is diluted. DFT calculations provide assignments of each of the peaks in the (19)F spectrum, but the predictions are close to the limits of accuracy and correlation information from 2-D NMR is invaluable in confirming the assignments. The effects of non-Gaussian lineshapes on the use of 2-D NMR for mapping correlations of spectral frequencies (e.g. due to the ABMS) are also discussed.

  11. (19)F MRSI of capecitabine in the liver at 7 T using broadband transmit-receive antennas and dual-band RF pulses.

    PubMed

    van Gorp, Jetse S; Seevinck, Peter R; Andreychenko, Anna; Raaijmakers, Alexander J E; Luijten, Peter R; Viergever, Max A; Koopman, Miriam; Boer, Vincent O; Klomp, Dennis W J

    2015-11-01

    Capecitabine (Cap) is an often prescribed chemotherapeutic agent, successfully used to cure some patients from cancer or reduce tumor burden for palliative care. However, the efficacy of the drug is limited, it is not known in advance who will respond to the drug and it can come with severe toxicity. (19)F Magnetic Resonance Spectroscopy (MRS) and Magnetic Resonance Spectroscopic Imaging (MRSI) have been used to non-invasively study Cap metabolism in vivo to find a marker for personalized treatment. In vivo detection, however, is hampered by low concentrations and the use of radiofrequency (RF) surface coils limiting spatial coverage. In this work, the use of a 7T MR system with radiative multi-channel transmit-receive antennas was investigated with the aim of maximizing the sensitivity and spatial coverage of (19)F detection protocols. The antennas were broadband optimized to facilitate both the (1)H (298 MHz) and (19)F (280 MHz) frequencies for accurate shimming, imaging and signal combination. B1(+) simulations, phantom and noise measurements showed that more than 90% of the theoretical maximum sensitivity could be obtained when using B1(+) and B1(-) information provided at the (1)H frequency for the optimization of B1(+) and B1(-) at the (19)F frequency. Furthermore, to overcome the limits in maximum available RF power, whilst ensuring simultaneous excitation of all detectable conversion products of Cap, a dual-band RF pulse was designed and evaluated. Finally, (19)F MRS(I) measurements were performed to detect (19)F metabolites in vitro and in vivo. In two patients, at 10 h (patient 1) and 1 h (patient 2) after Cap intake, (19)F metabolites were detected in the liver and the surrounding organs, illustrating the potential of the set-up for in vivo detection of metabolic rates and drug distribution in the body.

  12. Chiral discrimination in nuclear magnetic resonance spectroscopy.

    PubMed

    Lazzeretti, Paolo

    2017-08-08

    Chirality is a fundamental property of molecules whose spatial symmetry is characterized by the absence of improper rotations, making them not superimposable to their mirror image. Chiral molecules constitute the elementary building blocks of living species and one enantiomer is in general favoured (e.g., L-aminoacids and D-sugars pervade terrestrial homochiral biochemistry), because most chemical reactions producing natural substances are enantioselective. Since the effect of chiral chemicals and drugs on living beings can be markedly different between enantiomers, the quest for practical spectroscopical methods to scrutinize chirality is an issue of great importance and interest. Nuclear magnetic resonance (NMR) is a topmost analytical technique, but spectrometers currently used are ``blind'' to chirality, i.e., %%In fact, spectrometers presently used in NMR are unable to discriminate the two mirror-image forms of a chiral molecule, because, in the absence of a chiral solvent, the spectral parameters, chemical shifts and spin-spin coupling constants, are identical for enantiomers. Therefore, the development of new procedures for routine chiral recognition would offer basic support to scientists. However, in the presence of magnetic fields, a distinction between {\\em true} and {\\em false} chirality is mandatory. The former epitomizes natural optical activity, which is rationalized by a time-even pseudoscalar, i.e., the trace of a second-rank tensor, the mixed electric dipole/mag\\-net\\-ic dipole polarizability. The Faraday effect, magnetic circular dichroism and magnetic optical activity are instead related to a time-odd axial vector. The present review summarizes recent theoretical and experimental efforts to discriminate enantiomers via NMR spectroscopy, with the focus on the deep connection between chirality

  13. Through-space (19) F-(15) N couplings for the assignment of stereochemistry in flubenzimine.

    PubMed

    Ghiviriga, Ion; Rubinski, Miles A; Dolbier, William R

    2016-07-01

    Through-space (19) F-(15) N couplings revealed the configuration of flubenzimine, with the CF3 group on N4 pointing towards the lone pair of N5. The (19) F-(15) N coupling constants were measured at natural abundance using a spin-state selective indirect-detection pulse sequence. As (15) N-labelled proteins are routinely synthesized for NMR studies, through-space (19) F-(15) N couplings have the potential to probe the stereochemistry of these proteins by (19) F labelling of some amino acids or can reveal the site of docking of fluorine-containing drugs. Copyright © 2016 John Wiley & Sons, Ltd.

  14. Dynamic nuclear polarization in a magnetic resonance force microscope experiment.

    PubMed

    Issac, Corinne E; Gleave, Christine M; Nasr, Paméla T; Nguyen, Hoang L; Curley, Elizabeth A; Yoder, Jonilyn L; Moore, Eric W; Chen, Lei; Marohn, John A

    2016-04-07

    We report achieving enhanced nuclear magnetization in a magnetic resonance force microscope experiment at 0.6 tesla and 4.2 kelvin using the dynamic nuclear polarization (DNP) effect. In our experiments a microwire coplanar waveguide delivered radiowaves to excite nuclear spins and microwaves to excite electron spins in a 250 nm thick nitroxide-doped polystyrene sample. Both electron and proton spin resonance were observed as a change in the mechanical resonance frequency of a nearby cantilever having a micron-scale nickel tip. NMR signal, not observable from Curie-law magnetization at 0.6 T, became observable when microwave irradiation was applied to saturate the electron spins. The resulting NMR signal's size, buildup time, dependence on microwave power, and dependence on irradiation frequency was consistent with a transfer of magnetization from electron spins to nuclear spins. Due to the presence of an inhomogeneous magnetic field introduced by the cantilever's magnetic tip, the electron spins in the sample were saturated in a microwave-resonant slice 10's of nm thick. The spatial distribution of the nuclear polarization enhancement factor ε was mapped by varying the frequency of the applied radiowaves. The observed enhancement factor was zero for spins in the center of the resonant slice, was ε = +10 to +20 for spins proximal to the magnet, and was ε = -10 to -20 for spins distal to the magnet. We show that this bipolar nuclear magnetization profile is consistent with cross-effect DNP in a ∼10(5) T m(-1) magnetic field gradient. Potential challenges associated with generating and using DNP-enhanced nuclear magnetization in a nanometer-resolution magnetic resonance imaging experiment are elucidated and discussed.

  15. Automated data evaluation and modelling of simultaneous (19) F-(1) H medium-resolution NMR spectra for online reaction monitoring.

    PubMed

    Zientek, Nicolai; Laurain, Clément; Meyer, Klas; Paul, Andrea; Engel, Dirk; Guthausen, Gisela; Kraume, Matthias; Maiwald, Michael

    2016-06-01

    Medium-resolution nuclear magnetic resonance spectroscopy (MR-NMR) currently develops to an important analytical tool for both quality control and process monitoring. In contrast to high-resolution online NMR (HR-NMR), MR-NMR can be operated under rough environmental conditions. A continuous re-circulating stream of reaction mixture from the reaction vessel to the NMR spectrometer enables a non-invasive, volume integrating online analysis of reactants and products. Here, we investigate the esterification of 2,2,2-trifluoroethanol with acetic acid to 2,2,2-trifluoroethyl acetate both by (1) H HR-NMR (500 MHz) and (1) H and (19) F MR-NMR (43 MHz) as a model system. The parallel online measurement is realised by splitting the flow, which allows the adjustment of quantitative and independent flow rates, both in the HR-NMR probe as well as in the MR-NMR probe, in addition to a fast bypass line back to the reactor. One of the fundamental acceptance criteria for online MR-MNR spectroscopy is a robust data treatment and evaluation strategy with the potential for automation. The MR-NMR spectra are treated by an automated baseline and phase correction using the minimum entropy method. The evaluation strategies comprise (i) direct integration, (ii) automated line fitting, (iii) indirect hard modelling (IHM) and (iv) partial least squares regression (PLS-R). To assess the potential of these evaluation strategies for MR-NMR, prediction results are compared with the line fitting data derived from the quantitative HR-NMR spectroscopy. Although, superior results are obtained from both IHM and PLS-R for (1) H MR-NMR, especially the latter demands for elaborate data pretreatment, whereas IHM models needed no previous alignment. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

  16. Nuclear magnetic resonance for cultural heritage.

    PubMed

    Brai, Maria; Camaiti, Mara; Casieri, Cinzia; De Luca, Francesco; Fantazzini, Paola

    2007-05-01

    Nuclear magnetic resonance (NMR) portable devices are now being used for nondestructive in situ analysis of water content, pore space structure and protective treatment performance in porous media in the field of cultural heritage. It is a standard procedure to invert T(1) and T(2) relaxation data of fully water-saturated samples to get "pore size" distributions, but the use of T(2) requires great caution. It is well known that dephasing effects due to water molecule diffusion in a magnetic field gradient can affect transverse relaxation data, even if the smallest experimentally available half echo time tau is used in Carr-Purcell-Meiboom-Gill experiments. When a portable single-sided NMR apparatus is used, large field gradients due to the instrument, at the scale of the sample, are thought to be the dominant dephasing cause. In this paper, T(1) and T(2) (at different tau values) distributions were measured in natural (Lecce stone) and artificial (brick samples coming from the Greek-Roman Theatre of Taormina) porous media of interest for cultural heritage by a standard laboratory instrument and a portable device. While T(1) distributions do not show any appreciable effect from inhomogeneous fields, T(2) distributions can show strong effects, and a procedure is presented based on the dependence of 1/T(2) on tau to separate pore-scale gradient effects from sample-scale gradient effects. Unexpectedly, the gradient at the pore scale can be, in some cases, strong enough to make negligible the effects of gradients at the sample scale of the single-sided device.

  17. Burn injury by nuclear magnetic resonance imaging.

    PubMed

    Eising, Ernst G; Hughes, Justin; Nolte, Frank; Jentzen, Walter; Bockisch, Andreas

    2010-01-01

    Nuclear magnetic resonance imaging has become a standard diagnostic procedure in clinical medicine and is well known to have hazards for patients with pacemaker or metallic foreign bodies. Compared to CT, the frequency of MRI examinations is increasing due to the missing exposure of the patients by X-rays. Furthermore, high-field magnetic resonance tomograph (MRT) with 3 T has entered clinical practice, and 7-T systems are installed in multiple scientific institutions. On the other hand, the possibility of burn injuries has been reported only in very few cases. Based on a clinical finding of a burn injury in a 31-year-old male patient during a routine MRI of the lumbar spine with standard protocol, the MR scanner was checked and the examination was simulated in an animal model. The patient received a third-degree burn injury of the skin of the right hand and pelvis in a small region of skin contact. The subsequent control of the MRI scanner indicated no abnormal values for radiofrequency (RF) and power. In the subsequent animal experiment, comparable injuries could only be obtained by high RF power in a microwave stove. It is concluded that 'tissue loops' resulting from a contact between hand and pelvis must be avoided. With regard to forensic aspects, the need to inform patients of such a minimal risk can be avoided if the patients are adequately positioned using an isolating material between the hands and pelvis. These facts must be emphasized more in the future, if high-field MRI with stronger RF gradients is available in routine imaging. Copyright 2010 Elsevier Inc. All rights reserved.

  18. Selectivity in multiple quantum nuclear magnetic resonance

    SciTech Connect

    Warren, W.S.

    1980-11-01

    The observation of multiple-quantum nuclear magnetic resonance transitions in isotropic or anisotropic liquids is shown to give readily interpretable information on molecular configurations, rates of motional processes, and intramolecular interactions. However, the observed intensity of high multiple-quantum transitions falls off dramatically as the number of coupled spins increases. The theory of multiple-quantum NMR is developed through the density matrix formalism, and exact intensities are derived for several cases (isotropic first-order systems and anisotropic systems with high symmetry) to shown that this intensity decrease is expected if standard multiple-quantum pulse sequences are used. New pulse sequences are developed which excite coherences and produce population inversions only between selected states, even though other transitions are simultaneously resonant. One type of selective excitation presented only allows molecules to absorb and emit photons in groups of n. Coherent averaging theory is extended to describe these selective sequences, and to design sequences which are selective to arbitrarily high order in the Magnus expansion. This theory and computer calculations both show that extremely good selectivity and large signal enhancements are possible.

  19. Nuclear magnetic resonance data of C10H15

    NASA Astrophysics Data System (ADS)

    Kalinowski, H.-O.; Kumar, M.; Gupta, V.; Gupta, R.

    This document is part of Part 1 `Aliphatic Compounds' of Subvolume D 'Chemical Shifts and Coupling Constants for Carbon-13' of Landolt-Börnstein III/35 'Nuclear Magnetic Resonance Data', Group III 'Condensed Matter'.

  20. Nuclear magnetic resonance data of C9H20OSi

    NASA Astrophysics Data System (ADS)

    Mikhova, B. M.

    This document is part of Part 6 `Organic Metalloid Compounds' of Subvolume D 'Chemical Shifts and Coupling Constants for Carbon-13' of Landolt-Börnstein III/35 'Nuclear Magnetic Resonance Data', Group III 'Condensed Matter'.

  1. Nuclear magnetic resonance data of C8H18OSi

    NASA Astrophysics Data System (ADS)

    Mikhova, B. M.

    This document is part of Part 6 `Organic Metalloid Compounds' of Subvolume D 'Chemical Shifts and Coupling Constants for Carbon-13' of Landolt-Börnstein III/35 'Nuclear Magnetic Resonance Data', Group III 'Condensed Matter'.

  2. Nuclear Magnetic Double Resonance Using Weak Perturbing RF Fields

    ERIC Educational Resources Information Center

    Reynolds, G. Fredric

    1977-01-01

    Describes a nuclear magnetic resonance experimental example of spin tickling; also discusses a direct approach for verifying the relative signs of coupling constants in three-spin cyclopropyl systems. (SL)

  3. Nuclear Magnetic Double Resonance Using Weak Perturbing RF Fields

    ERIC Educational Resources Information Center

    Reynolds, G. Fredric

    1977-01-01

    Describes a nuclear magnetic resonance experimental example of spin tickling; also discusses a direct approach for verifying the relative signs of coupling constants in three-spin cyclopropyl systems. (SL)

  4. Nuclear magnetic resonance spectroscopy with single spin sensitivity

    PubMed Central

    Müller, C.; Kong, X.; Cai, J.-M.; Melentijević, K.; Stacey, A.; Markham, M.; Twitchen, D.; Isoya, J.; Pezzagna, S.; Meijer, J.; Du, J. F.; Plenio, M. B.; Naydenov, B.; McGuinness, L. P.; Jelezko, F.

    2014-01-01

    Nuclear magnetic resonance spectroscopy and magnetic resonance imaging at the ultimate sensitivity limit of single molecules or single nuclear spins requires fundamentally new detection strategies. The strong coupling regime, when interaction between sensor and sample spins dominates all other interactions, is one such strategy. In this regime, classically forbidden detection of completely unpolarized nuclei is allowed, going beyond statistical fluctuations in magnetization. Here we realize strong coupling between an atomic (nitrogen–vacancy) sensor and sample nuclei to perform nuclear magnetic resonance on four 29Si spins. We exploit the field gradient created by the diamond atomic sensor, in concert with compressed sensing, to realize imaging protocols, enabling individual nuclei to be located with Angstrom precision. The achieved signal-to-noise ratio under ambient conditions allows single nuclear spin sensitivity to be achieved within seconds. PMID:25146503

  5. /sup 1/H, /sup 19/F and /sup 11/B nuclear magnetic resonance characterization of BF/sub 3/:amine catalysts used in the cure of C fiber-epoxy prepregs

    SciTech Connect

    Happe, J.A.; Morgan, R.J.; Walkup, C.M.

    1983-12-01

    The chemical composition of commercial BF/sub 3/:amine complexes are variable and contain BF/sub 4//sup -/ and BF/sub 3/(OH)/sup -/ salts together with other unidentified highly reactive species. The BF/sub 3/:amine complexes, which are susceptible to hydrolysis, also partially convert to the BF/sub 4//sup -/ salt (i.e. BF/sub 4//sup -/NH/sub 3//sup +/C/sub 2/H/sub 5/) upon heating. This salt formation is accelerated in dimethyl sulfoxide solution and in the presence of the epoxides that are present in commercial prepregs. Commercial C fiber-epoxy prepregs are shown to contain either BF/sub 3/:NH/sub 2/C/sub 2/H/sub 5/ or BF/sub 3/:NHC/sub 5/H/sub 10/ species together with their BF/sub 4//sup -/ salts and a variety of boron-fluorine or carbon-fluorine prepreg species. Considerable variation in the relative quantities of BF/sub 3/:amine to its BF/sub 4//sup -/ salt was observed from prepreg lot to lot, which will cause variable viscosity-time-temperature prepreg cure profiles. It is concluded that the chemically stable and mobile BF/sub 4//sup -/ salt is the pre-dominant catalytic species, acting as a cationic catalyst for the prepreg cure reactions. During the early stages of cure the BF/sub 3/:amine catalyst converts to the BF/sub 4//sup -/ salt in the presence of epoxides, whereas the BF/sub 3/-prepreg species are susceptible to catalytic deactivation and immobilization.

  6. (19)F labelled glycosaminoglycan probes for solution NMR and non-linear (CARS) microscopy.

    PubMed

    Lima, Marcelo A; Cavalheiro, Renan P; M Viana, Gustavo; Meneghetti, Maria C Z; Rudd, Timothy R; Skidmore, Mark A; Powell, Andrew K; Yates, Edwin A

    2016-08-15

    Studying polysaccharide-protein interactions under physiological conditions by conventional techniques is challenging. Ideally, macromolecules could be followed by both in vitro spectroscopy experiments as well as in tissues using microscopy, to enable a proper comparison of results over these different scales but, often, this is not feasible. The cell surface and extracellular matrix polysaccharides, glycosaminoglycans (GAGs) lack groups that can be detected selectively in the biological milieu. The introduction of (19)F labels into GAG polysaccharides is explored and the interaction of a labelled GAG with the heparin-binding protein, antithrombin, employing (19)F NMR spectroscopy is followed. Furthermore, the ability of (19)F labelled GAGs to be imaged using CARS microscopy is demonstrated. (19)F labelled GAGs enable both (19)F NMR protein-GAG binding studies in solution at the molecular level and non-linear microscopy at a microscopic scale to be conducted on the same material, essentially free of background signals.

  7. Comparison of nuclear electric resonance and nuclear magnetic resonance in integer and fractional quantum Hall states

    SciTech Connect

    Tomimatsu, Toru Shirai, Shota; Hashimoto, Katsushi Sato, Ken; Hirayama, Yoshiro

    2015-08-15

    Electric-field-induced nuclear resonance (NER: nuclear electric resonance) involving quantum Hall states (QHSs) was studied at various filling factors by exploiting changes in nuclear spins polarized at quantum Hall breakdown. Distinct from the magnetic dipole interaction in nuclear magnetic resonance, the interaction of the electric-field gradient with the electric quadrupole moment plays the dominant role in the NER mechanism. The magnitude of the NER signal strongly depends on whether electronic states are localized or extended. This indicates that NER is sensitive to the screening capability of the electric field associated with QHSs.

  8. Nuclear magnetization in gallium arsenide quantum dots at zero magnetic field

    PubMed Central

    Sallen, G.; Kunz, S.; Amand, T.; Bouet, L.; Kuroda, T.; Mano, T.; Paget, D.; Krebs, O.; Marie, X.; Sakoda, K.; Urbaszek, B.

    2014-01-01

    Optical and electrical control of the nuclear spin system allows enhancing the sensitivity of NMR applications and spin-based information storage and processing. Dynamic nuclear polarization in semiconductors is commonly achieved in the presence of a stabilizing external magnetic field. Here we report efficient optical pumping of nuclear spins at zero magnetic field in strain-free GaAs quantum dots. The strong interaction of a single, optically injected electron spin with the nuclear spins acts as a stabilizing, effective magnetic field (Knight field) on the nuclei. We optically tune the Knight field amplitude and direction. In combination with a small transverse magnetic field, we are able to control the longitudinal and transverse components of the nuclear spin polarization in the absence of lattice strain—that is, in dots with strongly reduced static nuclear quadrupole effects, as reproduced by our model calculations. PMID:24500329

  9. Nuclear magnetization in gallium arsenide quantum dots at zero magnetic field.

    PubMed

    Sallen, G; Kunz, S; Amand, T; Bouet, L; Kuroda, T; Mano, T; Paget, D; Krebs, O; Marie, X; Sakoda, K; Urbaszek, B

    2014-01-01

    Optical and electrical control of the nuclear spin system allows enhancing the sensitivity of NMR applications and spin-based information storage and processing. Dynamic nuclear polarization in semiconductors is commonly achieved in the presence of a stabilizing external magnetic field. Here we report efficient optical pumping of nuclear spins at zero magnetic field in strain-free GaAs quantum dots. The strong interaction of a single, optically injected electron spin with the nuclear spins acts as a stabilizing, effective magnetic field (Knight field) on the nuclei. We optically tune the Knight field amplitude and direction. In combination with a small transverse magnetic field, we are able to control the longitudinal and transverse components of the nuclear spin polarization in the absence of lattice strain--that is, in dots with strongly reduced static nuclear quadrupole effects, as reproduced by our model calculations.

  10. High-Resolution Nuclear Magnetic Resonance of Solids.

    ERIC Educational Resources Information Center

    Maciel, Gary E.

    1984-01-01

    Examines recent developments in techniques for obtaining high-resolution nuclear magnetic resonance (NMR) spectra on solid samples, discussing the kinds of applications for which these techniques are well suited. Also discusses the characteristics of NMR of solids and generating magnetization for NMR in solids. (JN)

  11. High-Resolution Nuclear Magnetic Resonance of Solids.

    ERIC Educational Resources Information Center

    Maciel, Gary E.

    1984-01-01

    Examines recent developments in techniques for obtaining high-resolution nuclear magnetic resonance (NMR) spectra on solid samples, discussing the kinds of applications for which these techniques are well suited. Also discusses the characteristics of NMR of solids and generating magnetization for NMR in solids. (JN)

  12. Electron transport through nuclear pasta in magnetized neutron stars

    NASA Astrophysics Data System (ADS)

    Yakovlev, D. G.

    2015-10-01

    We present a simple model for electron transport in a possible layer of exotic nuclear clusters (in the so-called nuclear pasta layer) between the crust and liquid core of a strongly magnetized neutron star. The electron transport there can be strongly anisotropic and gyrotropic. The anisotropy is produced by different electron effective collision frequencies along and across local symmetry axis in domains of exotic ordered nuclear clusters and by complicated effects of the magnetic field. We also calculate averaged kinetic coefficients in case local domains are freely oriented. Possible applications of the obtained results and open problems are outlined.

  13. Electron paramagnetic resonance study of 14N and 19F superhyperfine interaction in VO 2+ doped propylenediammonium hexafluorozirconate

    NASA Astrophysics Data System (ADS)

    Lakshmi^Kasturi, T.; Krishnan, V. G.

    1998-05-01

    Electron paramagnetic resonance spectra have been recorded at X-band frequencies at room temperature on VO 2+ molecular ion in propylenediammonium hexafluorozirconate, [H 3N(CH 2) 3NH 3]ZrF 6, single crystals. The superhyperfine structure caused by 14N and 19F has been clearly observed in the spectra. The two sets of spectra observed are related to each other by the symmetry operations of the host crystals and represent vanadyl ion at two magnetically distinguishable interstitial sites in the unit cell.

  14. Need for remeasurements of nuclear magnetic dipole moments

    NASA Astrophysics Data System (ADS)

    Gustavsson, Martin G.; Mårtensson-Pendrill, Ann-Marie

    1998-11-01

    The need for a reassessment of nuclear magnetic dipole moments is prompted by recent experiments on the ground-state hyperfine structure in highly charged hydrogenlike systems which are sufficiently sensitive to probe QED effects. This work gives an overview of the magnetic dipole moments for the nuclei of interest, i.e., 165Ho, 185,187Re, 203,205Tl, 207Pb, and 209Bi. It is found that the present uncertainties in the nuclear magnetic dipole moment limit the interpretation of the accurate experimental hyperfine structures for these systems.

  15. The Fourier Transform in Chemistry. Part 1. Nuclear Magnetic Resonance: Introduction.

    ERIC Educational Resources Information Center

    King, Roy W.; Williams, Kathryn R.

    1989-01-01

    Using fourier transformation methods in nuclear magnetic resonance has made possible increased sensitivity in chemical analysis. This article describes these methods as they relate to magnetization, the RF magnetic field, nuclear relaxation, the RF pulse, and free induction decay. (CW)

  16. The Fourier Transform in Chemistry. Part 1. Nuclear Magnetic Resonance: Introduction.

    ERIC Educational Resources Information Center

    King, Roy W.; Williams, Kathryn R.

    1989-01-01

    Using fourier transformation methods in nuclear magnetic resonance has made possible increased sensitivity in chemical analysis. This article describes these methods as they relate to magnetization, the RF magnetic field, nuclear relaxation, the RF pulse, and free induction decay. (CW)

  17. Thick target neutron yield from 145 MeV 19F+27Al system

    NASA Astrophysics Data System (ADS)

    Sunil, C.; Bandyopadhyay, T.; Nandy, M.; Suman, Vitisha; Paul, S.; Nanal, V.; Pillay, R. G.; Sarkar, P. K.

    2013-09-01

    The double differential neutron energy distribution has been measured for the 19F+27Al system at 145 MeV projectile energy. The time of flight technique was used to measure the energy while pulse shape discrimination has been used to separate the neutrons from photons. The results are compared with the statistical nuclear reaction model codes PACE and EMPIRE. The PACE code appears to predict the slope and the end point energy of the experimental spectra fairly well but over predicts the values. The slope obtained from the EMPIRE calculations appears to be harder while the values being closer to the experimental results. The yield from the Hauser-Feshbach based compound nucleus model calculations agree reasonably well with the experimental results at the backward angles but not in the forward directions. The energy integrated angular distribution from 145 MeV projectiles show an enhanced emission in the forward angles compared to the similar results from 110 MeV projectiles. This analysis suggests some contribution from the pre-equilibrium emissions from the system at the higher projectile energy.

  18. Least Squares Magnetic-Field Optimization for Portable Nuclear Magnetic Resonance Magnet Design

    SciTech Connect

    Paulsen, Jeffrey L; Franck, John; Demas, Vasiliki; Bouchard, Louis-S.

    2008-03-27

    Single-sided and mobile nuclear magnetic resonance (NMR) sensors have the advantages of portability, low cost, and low power consumption compared to conventional high-field NMR and magnetic resonance imaging (MRI) systems. We present fast, flexible, and easy-to-implement target field algorithms for mobile NMR and MRI magnet design. The optimization finds a global optimum ina cost function that minimizes the error in the target magnetic field in the sense of least squares. When the technique is tested on a ring array of permanent-magnet elements, the solution matches the classical dipole Halbach solution. For a single-sided handheld NMR sensor, the algorithm yields a 640 G field homogeneous to 16 100 ppm across a 1.9 cc volume located 1.5 cm above the top of the magnets and homogeneous to 32 200 ppm over a 7.6 cc volume. This regime is adequate for MRI applications. We demonstrate that the homogeneous region can be continuously moved away from the sensor by rotating magnet rod elements, opening the way for NMR sensors with adjustable"sensitive volumes."

  19. High-Tc Superconductivity with Tc = 52 K under Antiferromagnetic Order in Five-Layered Cuprate Ba2Ca4Cu5O10(F,O)2 with TN = 175 K: 19F- and Cu-NMR Studies

    NASA Astrophysics Data System (ADS)

    Shimizu, Sunao; Tabata, Shin-ichiro; Mukuda, Hidekazu; Kitaoka, Yoshio; Shirage, Parasharam M.; Kito, Hijiri; Iyo, Akira

    2011-04-01

    We report on the observation of high-Tc superconductivity (SC) emerging with the background of an antiferro magnetic (AFM) order in the five-layered cuprate Ba2Ca4Cu5O10(F,O)2 through 19F-NMR and zero-field Cu-NMR studies. The measurements of spectrum and nuclear spin--lattice relaxation rates 19 of 19F-NMR give convincing evidence for the AFM order taking place below TN = 175 K and for the onset of SC below Tc = 52 K, hence both coexisting. The zero-field Cu-NMR study has revealed that AFM moments at Cu sites are 0.14 μB at outer CuO2 layers and 0.20 μB at inner ones. We remark that an intimate coupling exists between the AFM state and the SC order parameter below Tc = 52 K; the spin alignment in the AFM state is presumably changed in the SC-AFM mixed state.

  20. T-maze performance after developmental exposure to 19F tagged 5-HTP in chicks.

    PubMed

    Dingman, Sherry; Nash, Laurie; Hogan, Jeremy; Branch, Craig

    2004-12-01

    Chicks were used as a model to investigate behavioral effects of administering a new compound intended for use with magnetic resonance. The compound has multiple 19F atom tags covalently bonded to the indole ring of 5-hydroxytryptophan (PF-5HTP), the immediate precursor to the neurotransmitter serotonin. On incubation Day 17, 5 microg of PF-5-HTP, an equivalent amount of 5-HTP, or just 200 microL of the weak phosphate buffered saline (PBS) vehicle was injected into the airsac of each egg. Three days after hatching, chicks were isolated at the top of a simple T-Maze which, when traversed correctly, enabled them to return to their brood mates. A second trial in the T-Maze was conducted about three hours later. The brief period of isolation at the start of a trial causes social distress in chicks who are reinforced by returning to the brood. The task was selected as being sensitive to functioning of the serotonin pathways whose development might be altered by administering the compound during brain development. Repeated-measures analysis of variance yielded a statistically significant main effect for trial within groups, but no significant difference between injection groups. Administering a low dose of the fluorine tagged compound during development did not impair performance on this T-maze task.

  1. Nuclear Magnetic Resonance and the BCS Theory

    NASA Astrophysics Data System (ADS)

    Slichter, Charles P.

    The author describes the inspiration for the experiment by Hebel and Slichter to measure the nuclear spin-lattice relaxation time in super-conductors, the design considerations for the experiment, the surprising experimental results, their theoretical treatment using the Bardeen-Cooper-Schrieffer theory, and how comparing the nuclear relaxation results with those for ultrasound absorption confirmed the central idea of the BCS theory, the BCS pair wave function.

  2. Capacitor-based detection of nuclear magnetization: nuclear quadrupole resonance of surfaces.

    PubMed

    Gregorovič, Alan; Apih, Tomaž; Kvasić, Ivan; Lužnik, Janko; Pirnat, Janez; Trontelj, Zvonko; Strle, Drago; Muševič, Igor

    2011-03-01

    We demonstrate excitation and detection of nuclear magnetization in a nuclear quadrupole resonance (NQR) experiment with a parallel plate capacitor, where the sample is located between the two capacitor plates and not in a coil as usually. While the sensitivity of this capacitor-based detection is found lower compared to an optimal coil-based detection of the same amount of sample, it becomes comparable in the case of very thin samples and even advantageous in the proximity of conducting bodies. This capacitor-based setup may find its application in acquisition of NQR signals from the surface layers on conducting bodies or in a portable tightly integrated nuclear magnetic resonance sensor.

  3. Effective Giromagnetic Ratios in Artifical Nuclear Magnetization Pumping of the Noble Gases Mix

    NASA Astrophysics Data System (ADS)

    Popov, E. N.; Barantsev, K. A.; Litvinov, A. N.

    2015-09-01

    Dynamic of the nuclear magnetization of the two noble gases mix was studied in this research. Nuclear magnetization pumped along the induction of external magnetic field. Vector of nuclear magnetization is given a tilt by the week rotational magnetic field, which makes NMR for noble gases. Interaction between the nuclear magnetic moments of the different noble gases adducted to shifts at the frequency of nuclear moments precession in external magnetic field. Effective gyromagnetic ratios of the nuclear of noble gases is defined and it different from the tabulated value. There is theoretical calculation of effective gyromagnetic ratios in this research.

  4. Invited Review Article: Instrumentation for nuclear magnetic resonance in zero and ultralow magnetic field.

    PubMed

    Tayler, Michael C D; Theis, Thomas; Sjolander, Tobias F; Blanchard, John W; Kentner, Arne; Pustelny, Szymon; Pines, Alexander; Budker, Dmitry

    2017-09-01

    We review experimental techniques in our laboratory for nuclear magnetic resonance (NMR) in zero and ultralow magnetic field (below 0.1 μT) where detection is based on a low-cost, non-cryogenic, spin-exchange relaxation free (87)Rb atomic magnetometer. The typical sensitivity is 20-30 fT/Hz(1/2) for signal frequencies below 1 kHz and NMR linewidths range from Hz all the way down to tens of mHz. These features enable precision measurements of chemically informative nuclear spin-spin couplings as well as nuclear spin precession in ultralow magnetic fields.

  5. Detection of targeted perfluorocarbon nanoparticle binding using 19F diffusion weighted MR spectroscopy.

    PubMed

    Waters, Emily A; Chen, Junjie; Yang, Xiaoxia; Zhang, Huiying; Neumann, Robert; Santeford, Andrea; Arbeit, Jeffrey; Lanza, Gregory M; Wickline, Samuel A

    2008-11-01

    Real-time detection of targeted contrast agent binding is challenging due to background signal from unbound agent. (19)F diffusion weighted MR spectroscopy (DWS) could selectively detect binding of angiogenesis-targeted perfluorocarbon nanoparticles in vivo. Transgenic K14-HPV16 mice with epidermal squamous carcinomas exhibiting up-regulated neovasculature were used, with nontransgenic littermates as controls. Mice were treated with alpha(v)beta(3)-integrin targeted perfluorocarbon nanoparticles. (19)F DWS (b-values from 0 to 16,000 s/mm(2)) was performed on mouse ears in vivo at 11.74 Tesla. Progressive decay of (19)F signal with increased diffusion weighting at low b-values (< 1500 s/mm(2)) was observed in ears of both K14-HPV16 and control mice, demonstrating suppression of background (19)F signal from unbound nanoparticles in the blood. Much of the (19)F signal from ears of K14-HPV16 mice persisted at high b-values, indicating a stationary signal source, reflecting abundant nanoparticle binding to angiogenesis. (19)F signal in controls decayed completely at high b-values (> 1500 s/mm(2)), reflecting a moving signal source due to absence of angiogenesis (no binding sites). Estimated ADCs of nanoparticles in K14-HPV16 and control mice were 33.1 +/- 12.9 microm(2)/s and 19563 +/- 5858 microm(2)/s (p < 0.01). In vivo (19)F DWS can be used for specific detection of bound perfluorocarbon nanoparticles by selectively suppressing background (19)F signal from nanoparticles flowing in blood.

  6. Polywater: proton nuclear magnetic resonance spectrum.

    PubMed

    Page, T F; Jakobsen, R J; Lippincott, E R

    1970-01-02

    In the presence of water, the resonance of the strongly hydrogenbonded protons characteristic of polywater appears at 5 parts per million lower applied magnetic field than water. Polywater made by a new method confirms the infrared spectrum reported originally.

  7. Quantitative Component Analysis of Solid Mixtures by Analyzing Time Domain (1)H and (19)F T1 Saturation Recovery Curves (qSRC).

    PubMed

    Stueber, Dirk; Jehle, Stefan

    2017-07-01

    Prevalent polymorphism and complicated phase behavior of active pharmaceutical ingredients (APIs) often result in remarkable differences in the respective biochemical and physical API properties. Consequently, API form characterization and quantification play a central role in the pharmaceutical industry from early drug development to manufacturing. Here we present a novel and proficient quantification protocol for solid mixtures (qSRC) based on the measurement and mathematical fitting of T1 nuclear magnetic resonance (NMR) saturation recovery curves collected on a bench top time-domain NMR instrument. The saturation recovery curves of the relevant pure components are used as fingerprints. Employing a bench top NMR instrument possesses clear benefits. These instruments exhibit a small footprint, do not present any special requirements on lab space, and required sample handling is simple and fast. The qSRC analysis can easily be conducted in a conventional laboratory setting as well as in an industrial production environment, making it a versatile tool with the potential for widespread application. The accuracy and efficiency of the qSRC method is illustrated using (1)H and (19)F T1 data of selected pharmaceutical model compounds, as well as utilizing (1)H T1 data of an actual binary API anhydrous polymorph system of a Merck & Co., Inc. compound formerly developed as a hepatitis C virus drug. Copyright © 2017 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  8. Magnet design considerations for Fusion Nuclear Science Facility

    SciTech Connect

    Zhai, Yuhu; Kessel, Chuck; El-guebaly, Laila; Titus, Peter

    2016-02-25

    The Fusion Nuclear Science Facility (FNSF) is a nuclear confinement facility to provide a fusion environment with components of the reactor integrated together to bridge the technical gaps of burning plasma and nuclear science between ITER and the demonstration power plant (DEMO). Compared to ITER, the FNSF is smaller in size but generates much higher magnetic field, 30 times higher neutron fluence with 3 orders of magnitude longer plasma operation at higher operating temperatures for structures surrounding the plasma. Input parameters to the magnet design from system code analysis include magnetic field of 7.5 T at the plasma center with plasma major radius of 4.8 m and minor radius of 1.2 m, and a peak field of 15.5 T on the TF coils for FNSF. Both low temperature superconductor (LTS) and high temperature superconductor (HTS) are considered for the FNSF magnet design based on the state-of-the-art fusion magnet technology. The higher magnetic field can be achieved by using the high performance ternary Restack Rod Process (RRP) Nb3Sn strands for toroidal field (TF) magnets. The circular cable-in-conduit conductor (CICC) design similar to ITER magnets and a high aspect ratio rectangular CICC design are evaluated for FNSF magnets but low activation jacket materials may need to be selected. The conductor design concept and TF coil winding pack composition and dimension based on the horizontal maintenance schemes are discussed. Neutron radiation limits for the LTS and HTS superconductors and electrical insulation materials are also reviewed based on the available materials previously tested. As a result, the material radiation limits for FNSF magnets are defined as part of the conceptual design studies for FNSF magnets.

  9. Magnet Design Considerations for Fusion Nuclear Science Facility

    SciTech Connect

    Zhai, Y.; Kessel, C.; El-Guebaly, L.; Titus, P.

    2016-06-01

    The Fusion Nuclear Science Facility (FNSF) is a nuclear confinement facility that provides a fusion environment with components of the reactor integrated together to bridge the technical gaps of burning plasma and nuclear science between the International Thermonuclear Experimental Reactor (ITER) and the demonstration power plant (DEMO). Compared with ITER, the FNSF is smaller in size but generates much higher magnetic field, i.e., 30 times higher neutron fluence with three orders of magnitude longer plasma operation at higher operating temperatures for structures surrounding the plasma. Input parameters to the magnet design from system code analysis include magnetic field of 7.5 T at the plasma center with a plasma major radius of 4.8 m and a minor radius of 1.2 m and a peak field of 15.5 T on the toroidal field (TF) coils for the FNSF. Both low-temperature superconductors (LTS) and high-temperature superconductors (HTS) are considered for the FNSF magnet design based on the state-of-the-art fusion magnet technology. The higher magnetic field can be achieved by using the high-performance ternary restacked-rod process Nb3Sn strands for TF magnets. The circular cable-in-conduit conductor (CICC) design similar to ITER magnets and a high-aspect-ratio rectangular CICC design are evaluated for FNSF magnets, but low-activation-jacket materials may need to be selected. The conductor design concept and TF coil winding pack composition and dimension based on the horizontal maintenance schemes are discussed. Neutron radiation limits for the LTS and HTS superconductors and electrical insulation materials are also reviewed based on the available materials previously tested. The material radiation limits for FNSF magnets are defined as part of the conceptual design studies for FNSF magnets.

  10. Magnet design considerations for Fusion Nuclear Science Facility

    DOE PAGES

    Zhai, Yuhu; Kessel, Chuck; El-guebaly, Laila; ...

    2016-02-25

    The Fusion Nuclear Science Facility (FNSF) is a nuclear confinement facility to provide a fusion environment with components of the reactor integrated together to bridge the technical gaps of burning plasma and nuclear science between ITER and the demonstration power plant (DEMO). Compared to ITER, the FNSF is smaller in size but generates much higher magnetic field, 30 times higher neutron fluence with 3 orders of magnitude longer plasma operation at higher operating temperatures for structures surrounding the plasma. Input parameters to the magnet design from system code analysis include magnetic field of 7.5 T at the plasma center withmore » plasma major radius of 4.8 m and minor radius of 1.2 m, and a peak field of 15.5 T on the TF coils for FNSF. Both low temperature superconductor (LTS) and high temperature superconductor (HTS) are considered for the FNSF magnet design based on the state-of-the-art fusion magnet technology. The higher magnetic field can be achieved by using the high performance ternary Restack Rod Process (RRP) Nb3Sn strands for toroidal field (TF) magnets. The circular cable-in-conduit conductor (CICC) design similar to ITER magnets and a high aspect ratio rectangular CICC design are evaluated for FNSF magnets but low activation jacket materials may need to be selected. The conductor design concept and TF coil winding pack composition and dimension based on the horizontal maintenance schemes are discussed. Neutron radiation limits for the LTS and HTS superconductors and electrical insulation materials are also reviewed based on the available materials previously tested. As a result, the material radiation limits for FNSF magnets are defined as part of the conceptual design studies for FNSF magnets.« less

  11. In Vivo 19F MR Imaging Cell Tracking of Inflammatory Macrophages and Site-specific Development of Colitis-associated Dysplasia

    PubMed Central

    Shin, Soo Hyun; Kadayakkara, Deepak K.; Bulte, Jeff W. M.

    2017-01-01

    Purpose To investigate whether the magnitude of in vivo fluorine 19 (19F) magnetic resonance (MR) imaging signal is associated with subsequent development of colitis-associated dysplasia after in situ fluorination of inflammatory macrophages in a mouse model of inflammatory bowel disease (IBD). Materials and Methods Experiments were approved by the institutional animal care and use committee. Mice in the experimental group (n = 10) were administered azoxymethane and dextran sulfate sodium to induce colitis-associated dysplasia. Five mice were in the noninduced control group. Animals were injected with a commercially available perfluorocarbon and were examined in vivo with an 11.7-T MR imager for up to 110 days. Colons were then harvested followed by high-spatial-resolution ex vivo MR imaging. Multiple colon segments with or without 19F signal were histologically graded and were correlated with 19F signal intensity by using a Spearman correlation test. The signal intensity in mice with colitis-associated dysplasia was compared with that in control mice with a two-tailed Mann-Whitney U test. Results Patchy distributions of 19F signal intensity in the colon wall were seen on in vivo and ex vivo images, representing chronic inflammation as shown by immunohistochemistry. Histologic scores of inflammation and site-specific development of colitis-associated dysplasia in the descending colon showed good correlation with normalized 19F signal intensity (r = 0.88, P = .033 for the ascending colon; r = 0.82, P = .006 for the descending colon). A significantly (P = .002) higher normalized 19F signal-to-noise ratio was found at sites that developed dysplasia (mean, 0.58 ± 0.09 [standard deviation]) as compared with sites that did not (mean, 0.17 ± 0.22). Conclusion 19F MR imaging cell tracking of macrophages can be used to assess local inflammation in a mouse model of IBD. The resulting local 19F signal intensity, representing the magnitude of inflammation, has a positive

  12. Method and apparatus for measuring nuclear magnetic properties

    DOEpatents

    Weitekamp, D.P.; Bielecki, A.; Zax, D.B.; Zilm, K.W.; Pines, A.

    1987-12-01

    A method for studying the chemical and structural characteristics of materials is disclosed. The method includes placement of a sample material in a high strength polarizing magnetic field to order the sample nuclei. The condition used to order the sample is then removed abruptly and the ordering of the sample allowed to evolve for a time interval. At the end of the time interval, the ordering of the sample is measured by conventional nuclear magnetic resonance techniques. 5 figs.

  13. Nuclear magnetic resonance in environmental engineering: principles and applications.

    PubMed

    Lens, P N; Hemminga, M A

    1998-01-01

    This paper gives an introduction to nuclear magnetic resonance spectroscopy (NMR) and magnetic resonance imaging (MRI) in relation to applications in the field of environmental science and engineering. The underlying principles of high resolution solution and solid state NMR, relaxation time measurements and imaging are presented. Then, the use of NMR is illustrated and reviewed in studies of biodegradation and biotransformation of soluble and solid organic matter, removal of nutrients and xenobiotics, fate of heavy metal ions, and transport processes in bioreactor systems.

  14. Method and apparatus for measuring nuclear magnetic properties

    DOEpatents

    Weitekamp, Daniel P.; Bielecki, Anthony; Zax, David B.; Zilm, Kurt W.; Pines, Alexander

    1987-01-01

    A method for studying the chemical and structural characteristics of materials is disclosed. The method includes placement of a sample material in a high strength polarizing magnetic field to order the sample nucleii. The condition used to order the sample is then removed abruptly and the ordering of the sample allowed to evolve for a time interval. At the end of the time interval, the ordering of the sample is measured by conventional nuclear magnetic resonance techniques.

  15. Nuclear Magnetic Resonance in the Earth's Magnetic Field

    NASA Astrophysics Data System (ADS)

    Hollos, Stefan; Hollos, Richard

    2002-10-01

    We will address the challenges of doing NMR in the Earth's magnetic field. The design of an Earth's field proton precession magnetometer will be presented along with some preliminary attempts to do spectroscopy with this device.

  16. Saturated symmetric nuclear matter in strong magnetic fields

    NASA Astrophysics Data System (ADS)

    Diener, J. P. W.; Scholtz, F. G.

    2013-06-01

    Strongly magnetized symmetric nuclear matter is investigated within the context of effective baryon-meson exchange models. The magnetic field is coupled to the charge as well as the dipole moment of the baryons by including the appropriate terms in the Lagrangian density. The saturation density of magnetized, symmetric nuclear matter ρ0(B) was calculated for magnetic fields of the order of 1017 gauss. For the calculated range of ρ0(B) the binding energy, symmetry energy coefficient a4, and compressibility K of nuclear matter were also calculated. It is found that with an increasing magnetic field ρ0(B) increases, while the system becomes less bound. Furthermore, the depopulation of proton Landau levels leaves a distinct fluctuating imprint on K and a4. The calculations were also performed for increased values of the baryon magnetic dipole moment. By increasing the dipole moment strength ρ0(B) is found to decrease, but the system becomes more tightly bound while the fluctuations in K and a4 persist.

  17. Self-Assembly of Peptide Amphiphiles Designed as Imaging Probes for 19F and Relaxation-Enhanced 1H imaging

    NASA Astrophysics Data System (ADS)

    Preslar, Adam Truett

    This work incorporates whole-body imaging functionality into peptide amphiphile (PA) nanostructures used for regenerative medicine to facilitate magnetic resonance imaging (MRI). Two strategies were employed: 1. Conjugation of gadolinium chelates to peptide nanostructures to monitor biomaterial degradation in vivo with MRI and inductively-coupled plasma-mass spectroscopy (ICP-MS) 2. Synthesis of perfluorinated moiety-bearing peptide amphiphiles for 19F-MRI. The Gd(III) chelate gadoteridol was conjugated by copper-catalyzed "click" chemistry to a series of PAs known to form cylindrical nanostructures. By fitting nuclear magnetic resonance dispersion (NMRD) profiles to the Solomon-Bloembergen-Morgan (SBM) equations, it was observed that the water exchange parameter (tauM) depended on thermal annealing or calcium ion cross-linking. The sequence C16V 3A3E3G(Gd) exhibited an acceleration of nearly 100 ns after thermal annealing and calcium addition. These gadolinium-labeled PAs were used to track in vivo degradation of gels within the tibialis anterior muscle in a murine model. The half-life of biomaterial degradation was determined to be 13.5 days by inductively coupled plasma mass spectrometry (ICP-MS) of Gd(III). Gel implants could be monitored by MRI for eight days before the signal dispersed due to implant degradation and dilution. Additionally, nanostructures incorporating highly fluorinated domains were investigated for use as MRI contrast agents. Short, perfluoroalkyane tails of seven or eight carbon atoms in length were grafted to PA sequences containing a V2A2 beta-sheet forming sequence. The V2A2 sequence is known to drive 1D nanostructure assembly. It was found that the sequences C7F13V2A 2E2 and C7F13V2A 2K3 formed 1D assemblies in water which transition from ribbon-like to cylindrical shape as pH increases from 4.5 to 8.0. Ribbon-like nanostructures had reduced magnetic resonance signal by T 2 relaxation quenching, whereas their cylindrical counterparts

  18. Characterization via nuclear magnetic resonance of Portland cement and related materials

    NASA Astrophysics Data System (ADS)

    Edwards, Christopher Lane

    The physicochemical and engineering performance properties of several API class G and H ordinary Portland cements (OPCs) from various foreign and domestic sources have been investigated. The engineering performance properties are found to vary from sample to sample, and sources for this variation were sought out and identified. Magic angle spinning (MAS) 29Si nuclear magnetic resonance (NMR) experiments were marked by unusual relaxation behavior due to paramagnetism inherent in OPCs. A model system was created to mimic the paramagnetism of the cements and the system's relaxation behavior was analyzed. The iron in the calcium aluminoferrite (C4AF) provides the paramagnetism sufficient to substantially increase the relaxation rates of the 29Si in the tricalcium silicate (C3S) and dicalcium silicate (C2S) of cement. Several relaxation techniques were evaluated for analyzing cement relaxation, and saturation recovery was identified as the preferred technique. Correlations of data from the saturation recovery experiments with engineering performance properties, especially the strength development of cement pastes, were obtained facilely. An error analysis of the NMR and engineering performance testing techniques was conducted, which indicated that NMR measurements produced less error than the engineering performance tests. A best practice, modified from the saturation recovery experiment, is proposed for use in property correlations. Additionally, 13C MAS NMR was used to characterize various fluorinated single-walled carbon nanotubes (F-SWNTs), which proved surprisingly effective in attenuating 13C-19F dipolar interactions and quantifying the extent of functionalization present at high degrees of reaction. The mixed-metal nanocluster known as FeMoC was also characterized by MAS NMR. The impact of the paramagnetic Fe3+ in the Keplerate cage on the 31P nuclei in the caged Keggin ion of FeMoC was evident in the greatly reduced relaxation times measured.

  19. High Radiation Environment Nuclear Fragment Separator Magnet

    SciTech Connect

    Kahn, Stephen; Gupta, Ramesh

    2016-01-31

    Superconducting coils wound with HTS conductor can be used in magnets located in a high radiation environment. NbTi and Nb3Sn superconductors must operate at 4.5 K or below where removal of heat is less efficient. The HTS conductor can carry significant current at higher temperatures where the Carnot efficiency is significantly more favorable and where the coolant heat capacity is much larger. Using the HTS conductor the magnet can be operated at 40 K. This project examines the use of HTS conductor for the Michigan State University Facility For Rare Isotope Beams (FRIB) fragment separator dipole magnet which bends the beam by 30° and is located in a high radiation region that will not be easily accessible. Two of these magnets are needed to select the chosen isotope. There are a number of technical challenges to be addressed in the design of this magnet. The separator dipole is 2 m long and subtends a large angle. The magnet should keep a constant transverse field profile along its beam reference path. Winding coils with a curved inner segment is difficult as the conductor will tend to unwind during the process. In the Phase I project two approaches to winding the conductor were examined. The first was to wind the coils with curved sections on the inner and outer segments with the inner segment wound with negative curvature. The alternate approach was to use a straight segment on the inner segment to avoid negative curvature. In Phase I coils with a limited number of turns were successfully wound and tested at 77 K for both coil configurations. The Phase II program concentrated on the design, coil winding procedures, structural analysis, prototyping and testing of an HTS curved dipole coil at 40 K with a heat load representative of the radiation environment. One of the key criteria of the design of this magnet is to avoid the use of organic materials that would degrade rapidly in radiation. The Lorentz forces expected from the coils interacting with the

  20. DC SQUID Spectrometers for Nuclear Quadrupole and Low-Field Nuclear Magnetic Resonance Spectroscopy

    SciTech Connect

    TonThat, Dinh M.

    1998-04-01

    The dc Superconducting Quantum Interference Device (SQUJD) is a very sensitive detector of magnetic flux, with a typical flux noise of the order of 1 μΦ0Hz-1/2 at liquid helium temperature (Φ0=h/2e). This inherent flux sensitivity of the SQUID is used in a spectrometer for the detection of nuclear magnetic resonance (NMR.)and nuclear quadruple resonance (NQR). The processing magnetic field from the nuclear spins is coupled to the SQUID by mean of a flux transformer. The SQUID NMR spectrometer is used to measure the longitudinal relaxation time T1 of solid 129Xe at 4.2 K down to 0.1 mT.

  1. In vivo nuclear magnetic resonance imaging

    NASA Technical Reports Server (NTRS)

    Leblanc, A.

    1986-01-01

    During the past year the Woodlands Baylor Magnetic Resonance Imaging (MRI) facility became fully operational. A detailed description of this facility is given. One significant instrument addition this year was the 100 MHz, 40cm bore superconducting imaging spectrometer. This instrument gives researchers the capability to acquire high energy phosphate spectra. This will be used to investigate ATP, phosphocreatinine and inorganic phosphate changes in normal and atrophied muscle before, during and after exercise. An exercise device for use within the bore of the imaging magnet is under design/construction. The results of a study of T sub 1 and T sub 2 changes in atrophied muscle in animals and human subjects are given. The imaging and analysis of the lower leg of 15 research subjects before and after 5 weeks of complete bedrest was completed. A compilation of these results are attached.

  2. In vivo nuclear magnetic resonance imaging

    NASA Astrophysics Data System (ADS)

    Leblanc, A.

    1986-05-01

    During the past year the Woodlands Baylor Magnetic Resonance Imaging (MRI) facility became fully operational. A detailed description of this facility is given. One significant instrument addition this year was the 100 MHz, 40cm bore superconducting imaging spectrometer. This instrument gives researchers the capability to acquire high energy phosphate spectra. This will be used to investigate ATP, phosphocreatinine and inorganic phosphate changes in normal and atrophied muscle before, during and after exercise. An exercise device for use within the bore of the imaging magnet is under design/construction. The results of a study of T sub 1 and T sub 2 changes in atrophied muscle in animals and human subjects are given. The imaging and analysis of the lower leg of 15 research subjects before and after 5 weeks of complete bedrest was completed. A compilation of these results are attached.

  3. Using Nuclear Magnetic Resonance Spectroscopy for Measuring Ternary Phase Diagrams

    ERIC Educational Resources Information Center

    Woodworth, Jennifer K.; Terrance, Jacob C.; Hoffmann, Markus M.

    2006-01-01

    A laboratory experiment is presented for the upper-level undergraduate physical chemistry curriculum in which the ternary phase diagram of water, 1-propanol and n-heptane is measured using proton nuclear magnetic resonance (NMR) spectroscopy. The experiment builds upon basic concepts of NMR spectral analysis, typically taught in the undergraduate…

  4. Concepts in Biochemistry: Nuclear Magnetic Resonance Spectroscopy in Biochemistry.

    ERIC Educational Resources Information Center

    Cheatham, Steve

    1989-01-01

    Discusses the nature of a nuclear magnetic resonance (NMR) experiment, the techniques used, the types of structural and dynamic information obtained, and how one can view and refine structures using computer graphics techniques in combination with NMR data. Provides several spectra and a computer graphics image from B-form DNA. (MVL)

  5. C-13 nuclear magnetic resonance in organic geochemistry.

    NASA Technical Reports Server (NTRS)

    Balogh, B.; Wilson, D. M.; Burlingame, A. L.

    1972-01-01

    Study of C-13 nuclear magnetic resonance (NMR) spectra of polycyclic fused systems. The fingerprint qualities of the natural abundance in C-13 NMR spectra permitting unequivocal identification of these compounds is discussed. The principle of structural additivity of C-13 NMR information is exemplified on alpha and beta androstanes, alpha and beta cholestanes, ergostanes, sitostanes, and isodecanes.

  6. Using Nuclear Magnetic Resonance Spectroscopy for Measuring Ternary Phase Diagrams

    ERIC Educational Resources Information Center

    Woodworth, Jennifer K.; Terrance, Jacob C.; Hoffmann, Markus M.

    2006-01-01

    A laboratory experiment is presented for the upper-level undergraduate physical chemistry curriculum in which the ternary phase diagram of water, 1-propanol and n-heptane is measured using proton nuclear magnetic resonance (NMR) spectroscopy. The experiment builds upon basic concepts of NMR spectral analysis, typically taught in the undergraduate…

  7. Nuclear Magnetic Resonance Coupling Constants and Electronic Structure in Molecules.

    ERIC Educational Resources Information Center

    Venanzi, Thomas J.

    1982-01-01

    Theory of nuclear magnetic resonance spin-spin coupling constants and nature of the three types of coupling mechanisms contributing to the overall spin-spin coupling constant are reviewed, including carbon-carbon coupling (neither containing a lone pair of electrons) and carbon-nitrogen coupling (one containing a lone pair of electrons).…

  8. Nuclear Magnetic Resonance Coupling Constants and Electronic Structure in Molecules.

    ERIC Educational Resources Information Center

    Venanzi, Thomas J.

    1982-01-01

    Theory of nuclear magnetic resonance spin-spin coupling constants and nature of the three types of coupling mechanisms contributing to the overall spin-spin coupling constant are reviewed, including carbon-carbon coupling (neither containing a lone pair of electrons) and carbon-nitrogen coupling (one containing a lone pair of electrons).…

  9. Concepts in Biochemistry: Nuclear Magnetic Resonance Spectroscopy in Biochemistry.

    ERIC Educational Resources Information Center

    Cheatham, Steve

    1989-01-01

    Discusses the nature of a nuclear magnetic resonance (NMR) experiment, the techniques used, the types of structural and dynamic information obtained, and how one can view and refine structures using computer graphics techniques in combination with NMR data. Provides several spectra and a computer graphics image from B-form DNA. (MVL)

  10. Real or imaginary? Human metabolism through nuclear magnetism.

    PubMed

    Ross, B D

    2000-09-01

    This account of the beginnings and later applications of the use of nuclear magnetic resonance for noninvasive medical diagnosis was presented at a Symposium held in Oxford, UK, during September 13-15, 2000 to mark the centenary of the birth of Hans Krebs, on August 25, 1900.

  11. Contribution of 19F resonances on 18O( p, α)15N reaction rate

    NASA Astrophysics Data System (ADS)

    Benmeslem, Meriem; Chafa, Azzedine; Barhoumi, Slimane; Tribeche, Mouloud

    2014-08-01

    The 18O( p, α)15N reaction influences the isotopes production such as 19F, 18O, and 15N which can be used to test the models of stellar evolution. 19F is synthesized in both asymptotic giant branch (AGB) and metal-rich Wolf-Rayet (WR) stars. Using R-matrix theory we allow new values of resonances parameters in 19F. We show that the most important contribution to the differential and total cross section at low energies, comes from the levels in 19F situated at resonances energies E R =151, 680 and 840 keV with spin and parity 1/2+. The total width of the 680 keV resonance is badly known. So, we have focused on this broad resonance corresponding to the 8.65 MeV level in 19F. We delimit the temperature range in which each resonance contribution to the total reaction rate occurs by analyzing the ratio ( N A < σν> i / N A < σν>). This allowed us to show that the 680 and 840 keV broad resonances strongly dominate the reaction rate over the stellar temperature range T 9=0.02-0.06 and T 9=0.5-5. Finally, these results were compared to NACRE and Iliadis astrophysical compilations.

  12. Solid state 19F NMR parameters of fluorine-labeled amino acids. Part I: Aromatic substituents

    NASA Astrophysics Data System (ADS)

    Dürr, Ulrich H. N.; Grage, Stephan L.; Witter, Raiker; Ulrich, Anne S.

    2008-03-01

    Structural parameters of peptides and proteins in biomembranes can be directly measured by solid state NMR of selectively labeled amino acids. The 19F nucleus is a promising label to overcome the low sensitivity of 2H, 13C or 15N, and to serve as a background-free reporter group in biological compounds. To make the advantages of solid state 19F NMR fully available for structural studies of polypeptides, we have systematically measured the chemical shift anisotropies and relaxation properties of the most relevant aromatic and aliphatic 19F-labeled amino acids. In this first part of two consecutive contributions, six different 19F-substituents on representative aromatic side chains were characterized as polycrystalline powders by static and MAS experiments. The data are also compared with results on the same amino acids incorporated in synthetic peptides. The spectra show a wide variety of lineshapes, from which the principal values of the CSA tensors were extracted. In addition, temperature-dependent T1 and T2 relaxation times were determined by 19F NMR in the solid state, and isotropic chemical shifts and scalar couplings were obtained in solution.

  13. Solid-state 19F MAS NMR study on the conformation and molecular mobility of poly(chlorotrifluoroethylene).

    PubMed

    Tatsuno, Hiroto; Aimi, Keitaro; Ando, Shinji

    2007-05-01

    The temperature dependence of molecular mobility and conformational changes of poly(chlorotrifluoro- ethylene) (PCTFE) have been investigated by solid-state (19)F magic angle spinning (MAS) NMR spectroscopy. The pulse techniques of dipolar-filter and T(1rho)-filter allow selective observation of the amorphous and crystalline domains, respectively. The temperature dependence of T(1rho) (F) revealed that the segmental motion in the amorphous domain becomes vigorous above ca 80 degrees C, which is well above the glass transition (T(g)) temperature (52 degrees C) and more close to the beta-relaxation temperature (95 degrees C). On the other hand, vigorous molecular motions in the crystalline domain occur above 120 degrees C, which is much below the melting temperature (212 degrees C). This indicates that the polymer chains in the PCTFE crystallites are more mobile than those of typical semicrystalline fluoropolymers like poly(vinylidene fluoride) (PVDF), which can be associated with structural imperfections in the crystallites. In addition, the density functional theory (DFT) calculations of (19)F magnetic shielding suggest that the high-frequency shifts observed for the crystalline signals above 80 degrees C can be ascribed to the conformational change around meso diads toward more twisted and/or helical conformations in the main chain.

  14. Simultaneous dual frequency 1H and 19F open coil imaging of arthritic rabbit knee at 3T.

    PubMed

    Hockett, Franklin D; Wallace, Kirk D; Schmieder, Anne H; Caruthers, Shelton D; Pham, Christine T N; Wickline, Samuel A; Lanza, Gregory M

    2011-01-01

    The combination of sensitive magnetic resonance techniques with a selective site-targeted nanoparticle contrast agent has a demonstrated utility for molecular imaging studies. By detecting a unique signature of the contrast agent, this approach can be employed to identify specific bio-molecular markers and observe cellular-level processes within a large and complex organism (e.g., in vivo rabbit). The objective of the present investigation was to design, fabricate and characterize a radio-frequency (RF) coil for the dual frequency ((1)H and (19)F) simultaneous collection of both nuclei images in a 3T field, in order to facilitate studies of arthritic knee degradation in rabbits. The coil supports both transmit and receive modes. The supporting activities included: 1) establishing a technical database for calculating the required coil parameters, 2) selection of a favorable coil geometry, and 3) adaption of existing RF measurement techniques to the design, development and electrical evaluation of the coil. The coil is used in conjunction with a Philips Medical Systems clinical MRI scanner, requiring all RF simultaneous dual frequency ((1)H and (19)F) coils to operate in both transmit and receive modes. A commercial version of SPICE (simulation program with integrated circuit emphasis) was used to estimate significant operational parameters prior to fabricating the imaging coil. Excellent images were obtained with the fabricated coil and no operational problems were observed that would limit the use of other coil geometries and field strengths.

  15. Mobile high resolution xenon nuclear magnetic resonance spectroscopy in the earth's magnetic field.

    PubMed

    Appelt, Stephan; Häsing, F Wolfgang; Kühn, Holger; Perlo, Juan; Blümich, Bernhard

    2005-05-20

    Conventional high resolution nuclear magnetic resonance (NMR) spectra are usually measured in homogeneous, high magnetic fields (>1 T), which are produced by expensive and immobile superconducting magnets. We show that chemically resolved xenon (Xe) NMR spectroscopy of liquid samples can be measured in the Earth's magnetic field (5 x 10(-5) T) with a continuous flow of hyperpolarized Xe gas. It was found that the measured normalized Xe frequency shifts are significantly modified by the Xe polarization density, which causes different dipolar magnetic fields in the liquid and in the gas phases.

  16. Universal quantum control in zero-field nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Bian, Ji; Jiang, Min; Cui, Jiangyu; Liu, Xiaomei; Chen, Botao; Ji, Yunlan; Zhang, Bo; Blanchard, John; Peng, Xinhua; Du, Jiangfeng

    2017-05-01

    This paper describes a general method for the manipulation of nuclear spins in zero magnetic field. In the absence of magnetic fields, the spins lose the individual information on chemical shifts and inequivalent spins can only be distinguished by nuclear gyromagnetic ratios and spin-spin couplings. For spin-1/2 nuclei with different gyromagnetic ratios (i.e., different species) in zero magnetic field, we describe the scheme to realize a set of universal quantum logic gates, e.g., arbitrary single-qubit gates and a two-qubit controlled-not gate. This method allows for universal quantum control in systems which might provide promising applications in materials science, chemistry, biology, quantum information processing, and fundamental physics.

  17. Interactions of diastereomeric tripeptides of lysyl-5-fluorotryptophyllysine with DNA. 1. Optical and 19F NMR studies of native DNA complexes.

    PubMed

    Shine, N R; James, T L

    1985-07-30

    Lysyl-5-fluoro-L-tryptophyllysine and lysyl-5-fluoro-D-tryptophyllysine were synthesized, and their interactions with double-stranded DNA were investigated as a model for protein-nucleic acid interactions. The binding to DNA was studied by monitoring various 19F NMR parameters, the fluorescence, and the optical absorbance in thermal denaturation. The 19F resonance of the L-Trp peptide shifts upfield in the presence of DNA, and that of the D-Trp peptide shifts downfield with DNA present. The influence of ionic strength on the binding of each peptide to DNA and the fluorescence quenching titration of each with DNA indicate that electrostatic bonding (approximately 2 per peptide-DNA complex) dominates the binding in each case and accounts for the similar binding constants determined from the fluorescence quenching, i.e., 7.7 X 10(4) M-1 for the L-Trp complex and 6.2 X 10(-1) for the D-Trp complex. The 19F NMR chemical shift, line width, 19F[1H] nuclear Overhauser effect, and spin-lattice relaxation time (T1) changes all indicate that the aromatic moiety of the L-Trp complex, but not that of the D-Trp complex, is stacked between the bases of DNA. The relative increases in DNA melting temperature caused by binding of the tripeptide diastereomers are also consistent with stacking in the case of the L-Trp peptide. The magnitude of the changes and the susceptibility of the 19F NMR chemical shift to altering the solvent isotope (H2O vs. D2O) suggest that the L-Trp ring is not intercalated in the classical sense but is partially inserted between the bases of one strand of the double helix.

  18. A symmetrical fluorous dendron-cyanine dye conjugated bimodal nanoprobe for quantitative 19F MRI and NIR fluorescence bioimaging

    PubMed Central

    Wang, Zhe; Yue, Xuyi; Wang, Yu; Qian, Chunqi; Huang, Peng; Lizak, Marty; Niu, Gang; Wang, Fu; Rong, Pengfei; Kiesewetter, Dale O.; Ma, Ying; Chen, Xiaoyuan

    2014-01-01

    19F MRI and optical imaging are two powerful non-invasive molecular imaging modalities in biomedical applications. 19F MRI has great potential for high resolution in vivo imaging, while fluorescent probes enable ultracontrast cellular/tissue imaging with high accuracy and sensitivity. We, thus, developed a bimodal nanoprobe integrating the merits of 19F MRI and fluorescence imaging into a single synthetic molecule, which was further engineered into nanoprobe, by addressing shortcomings of conventional contrast agents to explore the quantitative 19F MRI and fluorescence imaging and cell tracking. Results showed that this bimodal imaging nanoprobe presented high correlation of 19F MR signal and NIR fluorescence intensity in vitro and in vivo. Additionally, this nanoprobe enabled quantitative 19F MR analysis, confirmed by complementary fluorescence analysis. This unique feature can hardly be obtained by traditional 19F MRI contrast agents. We envision that this nanoprobe would hold great potential for quantitative and sensitive multi-modal molecular imaging. PMID:24789108

  19. EFFECTS OF MAGNETIC FIELDS ON THE PROPAGATION OF NUCLEAR FLAMES IN MAGNETIC WHITE DWARFS

    SciTech Connect

    Kutsuna, Masamichi; Shigeyama, Toshikazu

    2012-04-10

    We investigate the effects of the magnetic field on the propagation of laminar flames of nuclear reactions taking place in white dwarfs with masses close to the Chandrasekhar limit. We calculate the velocities of laminar flames parallel and perpendicular to uniform magnetic fields as eigenvalues of steady solutions for magnetic hydrodynamical equations. As a result, we find that even when the magnetic pressure does not dominate the entire pressure it is possible for the magnetic field to suppress the flame propagation through the thermal conduction. Above the critical magnetic field, the flame velocity decreases with increasing magnetic field strength as v {approx} B{sup -1}. In media with densities of 10{sup 7}, 10{sup 8}, and 10{sup 9} g cm{sup -3}, the critical magnetic fields are orders of {approx}10{sup 10}, 10{sup 11}, and 10{sup 12} G, respectively.

  20. 73Ge-Nuclear Magnetic Resonance/Nuclear Quadrupole Resonance Investigation of Magnetic Properties of URhGe

    NASA Astrophysics Data System (ADS)

    Kotegawa, Hisashi; Fukumoto, Kenta; Toyama, Toshihiro; Tou, Hideki; Harima, Hisatomo; Harada, Atsushi; Kitaoka, Yoshio; Haga, Yoshinori; Yamamoto, Etsuji; Ōnuki, Yoshichika; Itoh, Kohei M.; Haller, Eugene E.

    2015-05-01

    We report on the 73Ge-nuclear magnetic resonance (NMR)/nuclear quadrupole resonance (NQR) results for the ferromagnetic (FM) superconductor URhGe. The magnitude and direction of the internal field, Hint, and the parameters of the electric field gradient at the Ge site were determined experimentally. By using powdered polycrystalline samples oriented by different methods, the field dependences of NMR shift and nuclear spin relaxation rates for H0 || c (easy axis) and H0 || b were obtained. From the NMR shifts for H0 || b, we confirmed a gradual suppression of the Curie temperature and observed a phase separation near the spin reorientation. The observation of the phase separation gives microscopic evidence that the spin reorientation under H0 || b is of first order at low temperatures. The nuclear spin-lattice relaxation rate 1/T1 indicates that the magnetic fluctuations are suppressed for H0 || c, whereas the fluctuations remain strongly for H0 || b. The enhancements of both 1/T1T and the nuclear spin-spin relaxation rate 1/T2 for H0 || b toward the spin reorientation field suggest that the field-induced superconductivity in URhGe emerges under the magnetic fluctuations along the b- and c-axes.

  1. Nuclear magnetic resonance and nuclear spin relaxation in AlAs quantum well probed by ESR

    NASA Astrophysics Data System (ADS)

    Shchepetilnikov, A. V.; Frolov, D. D.; Nefyodov, Yu. A.; Kukushkin, I. V.; Smirnov, D. S.; Tiemann, L.; Reichl, C.; Dietsche, W.; Wegscheider, W.

    2016-12-01

    The study of nuclear magnetic resonance and nuclear spin-lattice relaxation was conducted in an asymmetrically doped to n ˜1.8 ×1011cm-2 16 nm AlAs quantum well grown in the [001 ] direction. The dynamic polarization of nuclear spins due to a hyperfine interaction resulted in the so-called Overhauser shift of two-dimensional conduction electron spin resonance. The maximum shifts achieved in the experiments are several orders of magnitude smaller than in GaAs-based heterostructures, indicating that the hyperfine interaction is weak. The nuclear spin-lattice relaxation time extracted from the decay of the Overhauser shift over time turned out to depend on the filling factor of the two-dimensional electron system. This observation indicates that nuclear spin-lattice relaxation is mostly due to the interaction between electron and nuclear spins. The Overhauser shift diminishes resonantly when the rf radiation of certain frequencies was applied to the sample. This effect served as an indirect, yet powerful, method for nuclear magnetic resonance detection: NMR quadrupole splitting of 75As nuclei was clearly resolved. Theoretical calculations performed describe well these experimental findings.

  2. Calculation of vibrational branching ratios and hyperfine structure of 24Mg19F and its suitability for laser cooling and magneto-optical trapping

    NASA Astrophysics Data System (ADS)

    Xu, Liang; Yin, Yanning; Wei, Bin; Xia, Yong; Yin, Jianping

    2016-01-01

    More recently, laser cooling of the diatomic radical magnesium monofluoride (24Mg19F ) is being experimentally preformed [Appl. Phys. Express 8, 092701 (2015), 10.7567/APEX.8.092701 and Opt. Express 22, 28645 (2014), 10.1364/OE.22.028645] and was also studied theoretically [Phys. Rev. A 91, 042511 (2015), 10.1103/PhysRevA.91.042511]. However, some important problems still remain unsolved, so, in our paper, we perform further theoretical study for the feasibility of laser cooling and trapping the 24Mg19F molecule. At first, the highly diagonal Franck-Condon factors of the main transitions are verified by the closed-form approximation, Morse approximation, and Rydberg-Klein-Rees inversion methods, respectively. Afterwards, we investigate the lower X 2Σ1/2 + hyperfine manifolds using a quantum effective Hamiltonian approach and obtain the zero-field hyperfine spectrum with an accuracy of less than 30 kHz ˜5 μ K compared with the experimental results, and then find out that one cooling beam and one or two repumping beams with their first-order sidebands are enough to implement an efficient laser slowing and cooling of 24Mg19F . Meanwhile, we also calculate the accurate hyperfine structure magnetic g factors of the rotational state (X 2Σ1/2 +,N =1 ) and briefly discuss the influence of the external fields on the hyperfine structure of 24Mg19F as well as its possibility of preparing three-dimensional magneto-optical trapping. Finally we give an explanation for the difference between the Stark and Zeeman effects from the perspective of parity and time reversal symmetry. Our study shows that, besides appropriate excitation wavelengths, the short lifetime for the first excited state A 2Π1 /2 , and lighter mass, the 24Mg19F radical could be a good candidate molecule amenable to laser cooling and magneto-optical trapping.

  3. Nuclear magnetic resonance studies of biological systems

    SciTech Connect

    Antypas, W.G. Jr.

    1988-01-01

    The difference between intracellular and extracellular proton relaxation rates provides the basis for the determination of the mean hemoglobin concentration (MHC) in red blood cells. The observed water T{sub 1} relaxation data from red blood cell samples under various conditions were fit to the complete equation for the time-dependent decay of magnetization for a two-compartment system including chemical exchange. The MHC for each sample was calculated from the hematocrit and the intracellular water fraction as determined by NMR. The binding of the phosphorylcholine (PC) analogue, 2-(trimethylphosphonio)-ethylphosphate (phosphoryl-phosphocholine, PPC) to the PC binding myeloma proteins TEPC-15, McPC 603, and MOPC 167 was studied by {sup 31}P NMR.

  4. Nuclear magnetic resonance imaging at microscopic resolution

    NASA Astrophysics Data System (ADS)

    Johnson, G. Allan; Thompson, Morrow B.; Gewalt, Sally L.; Hayes, Cecil E.

    Resolution limits in NMR imaging are imposed by bandwidth considerations, available magnetic gradients for spatial encoding, and signal to noise. This work reports modification of a clinical NMR imaging device with picture elements of 500 × 500 × 5000 μm to yield picture elements of 50 × 50 × 1000 μm. Resolution has been increased by using smaller gradient coils permitting gradient fields >0.4 mT/cm. Significant improvements in signal to noise are achieved with smaller rf coils, close attention to choice of bandwidth, and signal averaging. These improvements permit visualization of anatomical structures in the rat brain with an effective diameter of 1 cm with the same definition as is seen in human imaging. The techniques and instrumentation should open a number of basic sciences such as embryology, plant sciences, and teratology to the potentials of NMR imaging.

  5. Investigation of the Possibility of Using Nuclear Magnetic Spin Alignment

    NASA Technical Reports Server (NTRS)

    Dent, William V., Jr.

    1998-01-01

    The goal of the program to investigate a "Gasdynamic fusion propulsion system for space exploration" is to develop a fusion propulsion system for a manned mission to the planet mars. A study using Deuterium and Tritium atoms are currently in progress. When these atoms under-go fusion, the resulting neutrons and alpha particles are emitted in random directions (isotropically). The probable direction of emission is equal for all directions, thus resulting in wasted energy, massive shielding and cooling requirements, and serious problems with the physics of achieving fusion. If the nuclear magnetic spin moments of the deuterium and tritium nuclei could be precisely aligned at the moment of fusion, the stream of emitted neutrons could be directed out the rear of the spacecraft for thrust and the alpha particles directed forward into an electromagnet ot produce electricity to continue operating the fusion engine. The following supporting topics are discussed: nuclear magnetic moments and spin precession in magnetic field, nuclear spin quantum mechanics, kinematics of nuclear reactions, and angular distribution of particles.

  6. High-resolution two-field nuclear magnetic resonance spectroscopy.

    PubMed

    Cousin, Samuel F; Charlier, Cyril; Kadeřávek, Pavel; Marquardsen, Thorsten; Tyburn, Jean-Max; Bovier, Pierre-Alain; Ulzega, Simone; Speck, Thomas; Wilhelm, Dirk; Engelke, Frank; Maas, Werner; Sakellariou, Dimitrios; Bodenhausen, Geoffrey; Pelupessy, Philippe; Ferrage, Fabien

    2016-12-07

    Nuclear magnetic resonance (NMR) is a ubiquitous branch of spectroscopy that can explore matter at the scale of an atom. Significant improvements in sensitivity and resolution have been driven by a steady increase of static magnetic field strengths. However, some properties of nuclei may be more favourable at low magnetic fields. For example, transverse relaxation due to chemical shift anisotropy increases sharply at higher magnetic fields leading to line-broadening and inefficient coherence transfers. Here, we present a two-field NMR spectrometer that permits the application of rf-pulses and acquisition of NMR signals in two magnetic centres. Our prototype operates at 14.1 T and 0.33 T. The main features of this system are demonstrated by novel NMR experiments, in particular a proof-of-concept correlation between zero-quantum coherences at low magnetic field and single quantum coherences at high magnetic field, so that high resolution can be achieved in both dimensions, despite a ca. 10 ppm inhomogeneity of the low-field centre. Two-field NMR spectroscopy offers the possibility to circumvent the limits of high magnetic fields, while benefiting from their exceptional sensitivity and resolution. This approach opens new avenues for NMR above 1 GHz.

  7. Unconventional nuclear magnetic resonance techniques using nanostructured diamond surfaces

    NASA Astrophysics Data System (ADS)

    Acosta, Victor; Jarmola, Andrey; Budker, Dmitry; Santori, Charles; Huang, Zhihong; Beausoleil, Raymond

    2014-03-01

    Nuclear magnetic resonance (NMR) technologies rely on obtaining high nuclear magnetization, motivating low operating temperatures and high magnetic fields. Dynamic nuclear polarization (DNP) techniques traditionally require another superconducting magnet and THz optics. We seek to use chip-scale devices to polarize nuclei in liquids at room temperature. The technique relies on optical pumping of nitrogen-vacancy (NV) centers and subsequent transfer of polarization to nuclei via hyperfine interaction, spin diffusion, and heteronuclear polarization transfer. We expect efficient polarization transfer will be realized by maximizing the diamond surface area. We have fabricated densely-packed (50 % packing fraction), high-aspect-ratio (10+) nanopillars over mm2 regions of the diamond surface. Pillars designed to have a few-hundred-nanometer diameter act as optical antennas, reducing saturation intensity. We also report progress in using nanopillar arrays as sensitive optical detectors of nano-scale NMR by measuring NV center Zeeman shifts produced by nearby external nuclei. The enhanced surface area increases the effective density of NV centers which couple to external nuclei. Combining these techniques may enable, e.g., identification of trace analytes and molecular imaging.

  8. Observation of force-detected nuclear magnetic resonance in a homogeneous field

    PubMed Central

    Madsen, L. A.; Leskowitz, G. M.; Weitekamp, D. P.

    2004-01-01

    We report the experimental realization of BOOMERANG (better observation of magnetization, enhanced resolution, and no gradient), a sensitive and general method of magnetic resonance. The prototype millimeter-scale NMR spectrometer shows signal and noise levels in agreement with the design principles. We present 1H and 19F NMR in both solid and liquid samples, including time-domain Fourier transform NMR spectroscopy, multiple-pulse echoes, and heteronuclear J spectroscopy. By measuring a 1H-19F J coupling, this last experiment accomplishes chemically specific spectroscopy with force-detected NMR. In BOOMERANG, an assembly of permanent magnets provides a homogeneous field throughout the sample, while a harmonically suspended part of the assembly, a detector, is mechanically driven by spin-dependent forces. By placing the sample in a homogeneous field, signal dephasing by diffusion in a field gradient is made negligible, enabling application to liquids, in contrast to other force-detection methods. The design appears readily scalable to μm-scale samples where it should have sensitivity advantages over inductive detection with microcoils and where it holds great promise for application of magnetic resonance in biology, chemistry, physics, and surface science. We briefly discuss extensions of the BOOMERANG method to the μm and nm scales. PMID:15326302

  9. Principles of nuclear magnetic resonance for medical application.

    PubMed

    Rosen, B R; Brady, T J

    1983-10-01

    Several important components must be combined to create an effective nuclear magnetic resonance (NMR) imaging system. The most imposing component is the magnet itself, which is most often either resistive or superconducting. In addition, the magnetic field gradient, radiofrequency (RF) coil, spectrometer, computer, and display system are critical factors that require special consideration before selecting an NMR system for a particular clinical usage. Although nuclear magnetic resonance and nuclear decay share a common object of interest (the nucleus), a number of differences between resonance and decay phenomena relating to information content and imaging techniques can be discussed. First, in NMR the frequency, and hence energy, of the detected electromagnetic radiation from a given nuclear type is dependent critically on the magnetic and molecular environment of the stimulated nuclei. This is contrasted to the situation in nuclear decay reactions, where the energy of gamma or positron emission is only weakly dependent on local factors. Thus in NMR, molecular information can be acquired without the use of external tracer molecules. In NMR energy exchange mechanisms (relaxation) take place on a microscopic scale, and hence local information is acquired by measuring relaxation times. Furthermore, the frequency output of an NMR experiment is transmitted to the detector with little change from its surroundings. This again differs from nuclear decay, where the observed spread of detected energies is a complex function of numerous interactions among the emitted radiation, the surrounding matter, and the detector, and energy exchange processes are spread in a random fashion over a large volume. However, this relative lack of interaction with matter in NMRs (RF) output comes at a price of sensitivity, since the energy level is orders of magnitude lower than that of gamma photons. In addition, the much longer wavelengths associated with such low energy radiation (on the

  10. Simple and Inexpensive Classroom Demonstrations of Nuclear Magnetic Resonance and Magnetic Resonance Imaging

    NASA Astrophysics Data System (ADS)

    Olson, Joel A.; Nordell, Karen J.; Chesnik, Marla A.; Landis, Clark R.; Ellis, Arthur B.; Rzchowski, M. S.; Condren, S. Michael; Lisensky, George C.

    2000-07-01

    Several demonstrations of resonance phenomena associated with nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) are described. The demonstrations comprise common orienteering compasses, whose needles represent magnetic dipoles, along with three collinear permanent magnets and a magnetic stir plate or pulseable electromagnets. The trio of permanent magnets provides a laterally uniform magnetic field, whose strength decreases with distance from the magnets. Resonance can be observed by adjusting the frequency of the magnetic stirrer to match the resonant frequency of the compass needle, which is shown to depend on magnetic field strength, that is, the needle's position relative to the permanent magnets. Another demonstration involves pulsing electromagnets that apply a perpendicular magnetic field that causes the compass needles to oscillate. The effects of shielding, spin-spin coupling, magnetogyric ratio, and free induction decay can also be demonstrated. By moving the trio of permanent magnets relative to the compasses, the MRI experiment can be mimicked. Complete instructions for the construction of the demonstrations, which can be used on an overhead projector, are included.

  11. Multinuclear solid state nuclear magnetic resonance investigation of water penetration in proton exchange membrane Nafion-117 by mechanical spinning.

    PubMed

    Sabarinathan, Venkatachalam; Wu, Zhen; Cheng, Ren-Hao; Ding, Shangwu

    2013-05-30

    (1)H, (17)O, and (19)F solid state NMR spectroscopies have been used to investigate water penetration in Nafion-117 under mechanical spinning. It is found that both (1)H and (17)O spectra depend on the orientation of the membrane with respect to the magnetic field. The intensities of the side chain (19)F spectra depend slightly on the orientation of membrane with respect to the magnetic field, but the backbone (19)F spectra do not exhibit orientation dependence. By analyzing the orientation dependent (1)H and (17)O spectra and time-resolved (1)H spectra, we show that the water loaded in Nafion-117, under high spinning speed, may penetrate into regions that are normally inaccessible by water. Water penetration is enhanced as the spinning speed is increased or the spinning time is increased. In the meantime, mechanical spinning accelerates water exchange. It is also found that water penetration by mechanical spinning is persistent; i.e., after spinning, water remains in those newly found regions. While water penetration changes the pores and channels in Nafion, (19)F spectra indicate that the chemical environments of the polymer backbone do not show change. These results provide new insights about the structure and dynamics of Nafion-117 and related materials. They are relevant to proton exchange membrane aging and offer enlightening points of view on antiaging and modification of this material for better proton conductivity. It is also interesting to view this phenomenon in the perspective of forced nanofiltration.

  12. New Versions of Terahertz Radiation Sources for Dynamic Nuclear Polarization in Nuclear Magnetic Resonance Spectroscopy

    NASA Astrophysics Data System (ADS)

    Bratman, V. L.; Kalynov, Yu. K.; Makhalov, P. B.; Fedotov, A. E.

    2014-01-01

    Dynamic nuclear polarization in strong-field nuclear magnetic resonance (NMR) spectroscopy requires terahertz radiation with moderate power levels. Nowadays, conventional gyrotrons are used almost exclusively to generate such radiation. In this review paper, we consider alternative variants of electronic microwave oscillators which require much weaker magnetic fields for their operation, namely, large-orbit gyrotrons operated at high cyclotron-frequency harmonics and Čerenkov-type devices, such as a backward-wave oscillator and a klystron frequency multiplier with tubular electron beams. Additionally, we consider the possibility to use the magnetic field created directly by the solenoid of an NMR spectrometer for operation of both the gyrotron and the backward-wave oscillator. Location of the oscillator in the spectrometer magnet makes it superfluous to use an additional superconducting magnet creating a strong field, significantly reduces the length of the radiation transmission line, and, in the case of Čerenkov-type devices, allows one to increase considerably the output-signal power. According to our calculations, all the electronic devices considered are capable of ensuring the power required for dynamic nuclear polarization (10 W or more) at a frequency of 260 GHz, whereas the gyrotrons, including their versions proposed in this paper, remain a single option at higher frequencies.

  13. Magnetic field simulation of magnetic phase detection sensor for steam generator tube in nuclear power plants

    NASA Astrophysics Data System (ADS)

    Ryu, Kwon-sang; Son, Derac; Park, Duck-gun; Kim, Yong-il

    2010-05-01

    Magnetic phases and defects are partly produced in steam generator tubes by stress and heat, because steam generator tubes in nuclear power plants are used under high temperature, high pressure, and radioactivity. The magnetic phases induce an error in the detection of the defects in steam generator tubes by the conventional eddy current method. So a new method is needed for detecting the magnetic phases in the steam generator tubes. We designed a new U-type yoke which has two kinds of coils and simulated the signal by the magnetic phases and defects in the Inconnel 600 tube.

  14. Stochastic Dipolar Recoupling in Nuclear Magnetic Resonance of Solids

    SciTech Connect

    Tycko, Robert

    2007-11-02

    I describe a nuclear magnetic resonance (NMR) technique, called stochastic dipolar recoupling (SDR), that permits continuous experimental control of the character of spin dynamics between coherent and incoherent limits in a system of magnetic dipole-coupled nuclei. In the fully incoherent limit of SDR, spin polarization transfers occur at distance-dependent rates without the quantum mechanical interferences among pairwise dipole-dipole couplings that often limit the feasibility or precision of structural studies of solids by NMR. In addition to facilitating structural studies, SDR represents a possible route to experimental studies of effects of decoherence on the dynamics of quantum many-body system000.

  15. Flat RF coils in static field gradient nuclear magnetic resonance.

    PubMed

    Stork, H; Gädke, A; Nestle, N; Fujara, F

    2009-10-01

    The use of flat RF coils allows considerable gains in the sensitivity of static field gradient (SFG) nuclear magnetic resonance (NMR) experiments. In this article, this effect is studied theoretically as well as experimentally. Additionally, the flat coil geometry has been studied theoretically depending on magnetic field gradient, pulse sequence and amplifier power. Moreover, detecting the signal directly from the free induction decay (FID) turned out to be quite attractive for STRAFI-like microimaging experiments, especially when using flat coils. In addition to wound rectangular flat coils also spiral flat coils have been developed which can be manufactured by photolithography from printed circuit boards.

  16. Stochastic dipolar recoupling in nuclear magnetic resonance of solids.

    PubMed

    Tycko, Robert

    2007-11-02

    I describe a nuclear magnetic resonance (NMR) technique, called stochastic dipolar recoupling (SDR), that permits continuous experimental control of the character of spin dynamics between coherent and incoherent limits in a system of magnetic dipole-coupled nuclei. In the fully incoherent limit of SDR, spin polarization transfers occur at distance-dependent rates without the quantum mechanical interferences among pairwise dipole-dipole couplings that often limit the feasibility or precision of structural studies of solids by NMR. In addition to facilitating structural studies, SDR represents a possible route to experimental studies of effects of decoherence on the dynamics of quantum many-body systems.

  17. Stochastic dipolar recoupling in nuclear magnetic resonance of solids

    PubMed Central

    Tycko, Robert

    2008-01-01

    I describe a nuclear magnetic resonance (NMR) technique, called stochastic dipolar recoupling (SDR), that permits continuous experimental control of the character of spin dynamics between coherent and incoherent limits in a system of magnetic dipole-coupled nuclei. In the fully incoherent limit of SDR, spin polarization transfers occur at distance-dependent rates without the quantum mechanical interferences among pairwise dipole-dipole couplings that often limit the feasibility or precision of structural studies of solids by NMR. In addition to facilitating structural studies, SDR represents a possible route to experimental studies of effects of decoherence on the dynamics of quantum many-body systems. PMID:17995438

  18. Algorithmic cooling in liquid-state nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Atia, Yosi; Elias, Yuval; Mor, Tal; Weinstein, Yossi

    2016-01-01

    Algorithmic cooling is a method that employs thermalization to increase qubit purification level; namely, it reduces the qubit system's entropy. We utilized gradient ascent pulse engineering, an optimal control algorithm, to implement algorithmic cooling in liquid-state nuclear magnetic resonance. Various cooling algorithms were applied onto the three qubits of C132-trichloroethylene, cooling the system beyond Shannon's entropy bound in several different ways. In particular, in one experiment a carbon qubit was cooled by a factor of 4.61. This work is a step towards potentially integrating tools of NMR quantum computing into in vivo magnetic-resonance spectroscopy.

  19. Discovery of a (19)F MRI sensitive salinomycin derivative with high cytotoxicity towards cancer cells.

    PubMed

    Shi, Qiuyan; Li, Yu; Bo, Shaowei; Li, Xiaofei; Zhao, Peng; Liu, Qi; Yang, Zhigang; Cong, Hengjiang; Deng, Hexiang; Chen, Mingnan; Chen, Shizhen; Zhou, Xin; Ding, Hong; Jiang, Zhong-Xing

    2016-04-14

    Salinomycin is a promising anti-cancer agent which selectively targets cancer stem cells. To improve its potency and selectivity, an analog library of salinomycin was generated by site-specific modification and CuAAc derivatization. Through a cytotoxicity analysis of the library, a fluorinated analog with high potency, selectivity, and (19)F MRI sensitivity was discovered as a novel theranostic agent.

  20. 19F MRI Detection of Acute Allograft Rejection with In Vivo Perfluorocarbon Labeling of Immune Cells

    PubMed Central

    Hitchens, T. Kevin; Ye, Qing; Eytan, Danielle F.; Janjic, Jelena M.; Ahrens, Eric T.; Ho, Chien

    2010-01-01

    Current diagnosis of organ rejection following transplantation relies on tissue biopsy, which is not ideal due to sampling limitations and risks associated with the invasive procedure. We have previously shown that cellular MRI of iron-oxide labeled immune-cell infiltration can provide a non-invasive measure of rejection status by detecting areas of hypointensity on T2*-weighted images. In the current study, we tested the feasibility of using a fluorine-based cellular tracer agent to detect macrophage accumulation in rodent models of acute allograft rejection by fluorine-19 (19F) MRI and MRS. This study used two rat models of acute rejection, including abdominal heterotopic cardiac transplant and orthotopic kidney transplant models. Following in vivo labeling of monocytes and macrophages with a commercially available agent containing perfluoro-15-crown-5-ether, we observed 19F-signal intensity in the organs experiencing rejection by 19F MRI, and conventional 1H MRI was used for anatomical context. Immunofluorescense and histology confirmed macrophage labeling. These results are consistent with our previous studies and show the complementary nature of the two cellular imaging techniques. With no background signal, 19F MRI/MRS can provide unambiguous detection of fluorine labeled cells, and may be a useful technique for detecting and quantifying rejection grade in patients. PMID:21305593

  1. AGB nucleosynthesis: The 19F(α, p)22Ne reaction at astrophysical energies

    NASA Astrophysics Data System (ADS)

    D'Agata, G.; Pizzone, R. G.; Spitaleri, C.; Blagus, S.; Figuera, P.; Grassi, L.; Guardo, G. L.; Gulino, M.; Hayakawa, S.; Indelicato, I.; Kshetri, R.; La Cognata, M.; Lamia, L.; Lattuada, M.; Mijatović, T.; Milin, M.; Miljanic, D.; Prepolec, L.; Sergi, M. L.; Skukan, N.; Soic, N.; Tokic, V.; Tumino, A.; Uroic, M.

    2017-06-01

    Learning how 19F is produced and destructed in AGB-stars is crucial. Fluorine abundance is in fact important, given that it is strongly tied to standard and extra-mixing processes taking place in AGB-stars. This kind of objects are considered to be the main sources of fluorine in galactic environment, in which experimental abundances are far overestimated. For this reason the reaction 19F(α, p)22Ne, that represents the main destruction channel in He-rich environment, was studied at energies corresponding to T˜2.108 K. Such reaction has been studied with direct method at Ebeam = 1100 keV for alpha particles impinging on a fluorine target, corresponding to EC.M. ˜ 900 keV, still far from the Gamow window, placed at 390÷800 keV, below the Coulomb barrier (3.81 MeV). An experiment was performed at Rujer Boskovic Institut (Zagreb), applying the Trojan Horse Method. With this experimental procedure we were able to select the quasi-free contribution coming from 6Li(19F,p 22Ne)2H at Ebeam = 6 MeV at kinematically useful angles. We measured the 19F(α, p)22Ne at 0 MeV ≤ EC.M ≤ 0.9 MeV, extracting the two body cross-section in absolute units at energies of astrophysical interest.

  2. Storage of nuclear magnetization as long-lived singlet order in low magnetic field.

    PubMed

    Pileio, Giuseppe; Carravetta, Marina; Levitt, Malcolm H

    2010-10-05

    Hyperpolarized nuclear states provide NMR signals enhanced by many orders of magnitude, with numerous potential applications to analytical NMR, in vivo NMR, and NMR imaging. However, the lifetime of hyperpolarized magnetization is normally limited by the relaxation time constant T(1), which lies in the range of milliseconds to minutes, apart from in exceptional cases. In many cases, the lifetime of the hyperpolarized state may be enhanced by converting the magnetization into nuclear singlet order, where it is protected against many common relaxation mechanisms. However, all current methods for converting magnetization into singlet order require the use of a high-field, high-homogeneity NMR magnet, which is incompatible with most hyperpolarization procedures. We demonstrate a new method for converting magnetization into singlet order and back again. The new technique is suitable for magnetically inequivalent spin-pair systems in weak and inhomogeneous magnetic fields, and is compatible with known hyperpolarization technology. The method involves audio-frequency pulsed irradiation at the low-field nuclear Larmor frequency, employing coupling-synchronized trains of 180° pulses to induce singlet-triplet transitions. The echo trains are used as building blocks for a pulse sequence called M2S that transforms longitudinal magnetization into long-lived singlet order. The time-reverse of the pulse sequence, called S2M, converts singlet order back into longitudinal magnetization. The method is demonstrated on a solution of (15)N-labeled nitrous oxide. The magnetization is stored in low magnetic field for over 30 min, even though the T(1) is less than 3 min under the same conditions.

  3. Storage of nuclear magnetization as long-lived singlet order in low magnetic field

    PubMed Central

    Pileio, Giuseppe; Carravetta, Marina; Levitt, Malcolm H.

    2010-01-01

    Hyperpolarized nuclear states provide NMR signals enhanced by many orders of magnitude, with numerous potential applications to analytical NMR, in vivo NMR, and NMR imaging. However, the lifetime of hyperpolarized magnetization is normally limited by the relaxation time constant T1, which lies in the range of milliseconds to minutes, apart from in exceptional cases. In many cases, the lifetime of the hyperpolarized state may be enhanced by converting the magnetization into nuclear singlet order, where it is protected against many common relaxation mechanisms. However, all current methods for converting magnetization into singlet order require the use of a high-field, high-homogeneity NMR magnet, which is incompatible with most hyperpolarization procedures. We demonstrate a new method for converting magnetization into singlet order and back again. The new technique is suitable for magnetically inequivalent spin-pair systems in weak and inhomogeneous magnetic fields, and is compatible with known hyperpolarization technology. The method involves audio-frequency pulsed irradiation at the low-field nuclear Larmor frequency, employing coupling-synchronized trains of 180° pulses to induce singlet–triplet transitions. The echo trains are used as building blocks for a pulse sequence called M2S that transforms longitudinal magnetization into long-lived singlet order. The time-reverse of the pulse sequence, called S2M, converts singlet order back into longitudinal magnetization. The method is demonstrated on a solution of 15N-labeled nitrous oxide. The magnetization is stored in low magnetic field for over 30 min, even though the T1 is less than 3 min under the same conditions. PMID:20855584

  4. The origins and future of nuclear magnetic resonance imaging

    SciTech Connect

    Wehrli, F.W. )

    1992-06-01

    What began as a curiosity of physics has become the preeminent method of diagnostic medical imaging and may displace x-ray-based techniques in the 21st century. During the past two decades nuclear magnetic resonance has revolutionized chemistry, biochemistry, biology and, more recently, diagnostic medicine. Nuclear magnetic resonance imaging, (MRI) as it is commonly called, is fundamentally different from x-ray-based techniques in terms of the principles of spatial encoding and mechanisms of signal and contrast generation involved. MRI has a far richer ultimate potential than any other imaging technique known today, and its technology and applications are still far from maturation, which may not occur until early in the 21st century. 23 refs., 6 figs.

  5. Nuclear chiral and magnetic rotation in covariant density functional theory

    NASA Astrophysics Data System (ADS)

    Meng, Jie; Zhao, Pengwei

    2016-05-01

    Excitations of chiral rotation observed in triaxial nuclei and magnetic and/or antimagnetic rotations (AMR) seen in near-spherical nuclei have attracted a lot of attention. Unlike conventional rotation in well-deformed or superdeformed nuclei, here the rotational axis is not necessary coinciding with any principal axis of the nuclear density distribution. Thus, tilted axis cranking (TAC) is mandatory to describe these excitations self-consistently in the framework of covariant density functional theory (CDFT). We will briefly introduce the formalism of TAC-CDFT and its application for magnetic and AMR phenomena. Configuration-fixed CDFT and its predictions for nuclear chiral configurations and for favorable triaxial deformation parameters are also presented, and the discoveries of the multiple chiral doublets in 133Ce and 103Rh are discussed.

  6. Chemometric Analysis of Nuclear Magnetic Resonance Spectroscopy Data

    SciTech Connect

    ALAM,TODD M.; ALAM,M. KATHLEEN

    2000-07-20

    Chemometric analysis of nuclear magnetic resonance (NMR) spectroscopy has increased dramatically in recent years. A variety of different chemometric techniques have been applied to a wide range of problems in food, agricultural, medical, process and industrial systems. This article gives a brief review of chemometric analysis of NMR spectral data, including a summary of the types of mixtures and experiments analyzed with chemometric techniques. Common experimental problems encountered during the chemometric analysis of NMR data are also discussed.

  7. The metabolism of 2-trifluormethylaniline and its acetanilide in the rat by 19F NMR monitored enzyme hydrolysis and 1H/19F HPLC-NMR spectroscopy.

    PubMed

    Tugnait, M; Lenz, E M; Hofmann, M; Spraul, M; Wilson, I D; Lindon, J C; Nicholson, J K

    2003-01-01

    The urinary excretion profile and identity of the metabolites of 2-trifluoromethyl aniline (2-TFMA) and 2-trifluoromethyl acetanilide (2-TFMAc), following i.p. administration to the rat at 50 mg kg(-1), were determined using a combination of 19F NMR monitored enzyme hydrolysis, SPEC-MS and 19F/1H HPLC-NMR. A total recovery of approximately 96.4% of the dose was excreted into the urine as seven metabolites. The major routes of metabolism were N-conjugation (glucuronidation), and ring-hydroxylation followed by sulphation (and to a lesser extent glucuronidation). The major metabolites excreted into the urine for both compounds were a labile N-conjugated metabolite (a postulated N-glucuronide) and a sulphated ring-hydroxylated metabolite (a postulated 4-amino-5-trifluoromethylphenyl sulphate) following dosing of 2-TFMA. These accounted for approximately 53.0 and 31.5% of the dose, respectively. This study identifies problems on sample component instability in the preparation and analysis procedures.

  8. Analysis of the transient response of nuclear spins in GaAs with/without nuclear magnetic resonance

    SciTech Connect

    Rasly, Mahmoud; Lin, Zhichao; Yamamoto, Masafumi; Uemura, Tetsuya

    2016-05-15

    As an alternative to studying the steady-state responses of nuclear spins in solid state systems, working within a transient-state framework can reveal interesting phenomena. The response of nuclear spins in GaAs to a changing magnetic field was analyzed based on the time evolution of nuclear spin temperature. Simulation results well reproduced our experimental results for the transient oblique Hanle signals observed in an all-electrical spin injection device. The analysis showed that the so called dynamic nuclear polarization can be treated as a cooling tool for the nuclear spins: It works as a provider to exchange spin angular momentum between polarized electron spins and nuclear spins through the hyperfine interaction, leading to an increase in the nuclear polarization. In addition, a time-delay of the nuclear spin temperature with a fast sweep of the external magnetic field produces a possible transient state for the nuclear spin polarization. On the other hand, the nuclear magnetic resonance acts as a heating tool for a nuclear spin system. This causes the nuclear spin temperature to jump to infinity: i.e., the average nuclear spins along with the nuclear field vanish at resonant fields of {sup 75}As, {sup 69}Ga and {sup 71}Ga, showing an interesting step-dip structure in the oblique Hanle signals. These analyses provide a quantitative understanding of nuclear spin dynamics in semiconductors for application in future computation processing.

  9. Accelerated nanoscale magnetic resonance imaging through phase multiplexing

    SciTech Connect

    Moores, B. A.; Eichler, A. Takahashi, H.; Navaretti, P.; Degen, C. L.; Tao, Y.

    2015-05-25

    We report a method for accelerated nanoscale nuclear magnetic resonance imaging by detecting several signals in parallel. Our technique relies on phase multiplexing, where the signals from different nuclear spin ensembles are encoded in the phase of an ultrasensitive magnetic detector. We demonstrate this technique by simultaneously acquiring statistically polarized spin signals from two different nuclear species ({sup 1}H, {sup 19}F) and from up to six spatial locations in a nanowire test sample using a magnetic resonance force microscope. We obtain one-dimensional imaging resolution better than 5 nm, and subnanometer positional accuracy.

  10. Magnetic Flux Compression Concept for Nuclear Pulse Propulsion and Power

    NASA Technical Reports Server (NTRS)

    Litchford, Ronald J.

    2000-01-01

    The desire for fast, efficient interplanetary transport requires propulsion systems having short acceleration times and very high specific impulse attributes. Unfortunately, most highly efficient propulsion systems which are within the capabilities of present day technologies are either very heavy or yield very low impulse such that the acceleration time to final velocity is too long to be of lasting interest, One exception, the nuclear thermal thruster, could achieve the desired acceleration but it would require inordinately large mass ratios to reach the range of desired final velocities. An alternative approach, among several competing concepts that are beyond our modern technical capabilities, is a pulsed thermonuclear device utilizing microfusion detonations. In this paper, we examine the feasibility of an innovative magnetic flux compression concept for utilizing microfusion detonations, assuming that such low yield nuclear bursts can be realized in practice. In this concept, a magnetic field is compressed between an expanding detonation driven diamagnetic plasma and a stationary structure formed from a high temperature superconductor (HTSC). In general, we are interested in accomplishing two important functions: (1) collimation of a hot diamagnetic plasma for direct thrust production; and (2) pulse power generation for dense plasma ignition. For the purposes of this research, it is assumed that rnicrofusion detonation technology may become available within a few decades, and that this approach could capitalize on recent advances in inertial confinement fusion ICF) technologies including magnetized target concepts and antimatter initiated nuclear detonations. The charged particle expansion velocity in these detonations can be on the order of 10 (exp 6)- 10 (exp 7) meters per second, and, if effectively collimated by a magnetic nozzle, can yield the Isp and the acceleration levels needed for practical interplanetary spaceflight. The ability to ignite pure

  11. Magnetic Flux Compression Concept for Nuclear Pulse Propulsion and Power

    NASA Technical Reports Server (NTRS)

    Litchford, Ronald J.

    2000-01-01

    The desire for fast, efficient interplanetary transport requires propulsion systems having short acceleration times and very high specific impulse attributes. Unfortunately, most highly efficient propulsion systems which are within the capabilities of present day technologies are either very heavy or yield very low impulse such that the acceleration time to final velocity is too long to be of lasting interest, One exception, the nuclear thermal thruster, could achieve the desired acceleration but it would require inordinately large mass ratios to reach the range of desired final velocities. An alternative approach, among several competing concepts that are beyond our modern technical capabilities, is a pulsed thermonuclear device utilizing microfusion detonations. In this paper, we examine the feasibility of an innovative magnetic flux compression concept for utilizing microfusion detonations, assuming that such low yield nuclear bursts can be realized in practice. In this concept, a magnetic field is compressed between an expanding detonation driven diamagnetic plasma and a stationary structure formed from a high temperature superconductor (HTSC). In general, we are interested in accomplishing two important functions: (1) collimation of a hot diamagnetic plasma for direct thrust production; and (2) pulse power generation for dense plasma ignition. For the purposes of this research, it is assumed that rnicrofusion detonation technology may become available within a few decades, and that this approach could capitalize on recent advances in inertial confinement fusion ICF) technologies including magnetized target concepts and antimatter initiated nuclear detonations. The charged particle expansion velocity in these detonations can be on the order of 10 (exp 6)- 10 (exp 7) meters per second, and, if effectively collimated by a magnetic nozzle, can yield the Isp and the acceleration levels needed for practical interplanetary spaceflight. The ability to ignite pure

  12. Quantitative velocity distributions via nuclear magnetic resonance flow metering

    NASA Astrophysics Data System (ADS)

    O'Neill, Keelan T.; Fridjonsson, Einar O.; Stanwix, Paul L.; Johns, Michael L.

    2016-08-01

    We demonstrate the use of Tikhonov regularisation as a data inversion technique to determine the velocity distributions of flowing liquid streams. Regularisation is applied to the signal produced by a nuclear magnetic resonance (NMR) flow measurement system consisting of a pre-polarising permanent magnet located upstream of an Earth's magnetic field NMR detection coil. A simple free induction decay (FID) NMR signal is measured for the flowing stream in what is effectively a 'time-of-flight' measurement. The FID signal is then modelled as a function of fluid velocity and acquisition time, enabling determination of the velocity probability distributions via regularisation. The mean values of these velocity distributions were successfully validated against in-line rotameters. The ability to quantify multi-modal velocity distributions was also demonstrated using a two-pipe system.

  13. DC superconducting quantum interference device usable in nuclear quadrupole resonance and zero field nuclear magnetic spectrometers

    DOEpatents

    Fan, Non Q.; Clarke, John

    1993-01-01

    A spectrometer for measuring the nuclear quadrupole resonance spectra or the zero-field nuclear magnetic resonance spectra generated by a sample is disclosed. The spectrometer uses an amplifier having a dc SQUID operating in a flux-locked loop for generating an amplified output as a function of the intensity of the signal generated by the sample. The flux-locked loop circuit includes an integrator. The amplifier also includes means for preventing the integrator from being driven into saturation. As a result, the time for the flux-locked loop to recover from the excitation pulses generated by the spectrometer is reduced.

  14. DC superconducting quantum interference device usable in nuclear quadrupole resonance and zero field nuclear magnetic spectrometers

    DOEpatents

    Fan, N.Q.; Clarke, J.

    1993-10-19

    A spectrometer for measuring the nuclear quadrupole resonance spectra or the zero-field nuclear magnetic resonance spectra generated by a sample is disclosed. The spectrometer uses an amplifier having a dc SQUID operating in a flux-locked loop for generating an amplified output as a function of the intensity of the signal generated by the sample. The flux-locked loop circuit includes an integrator. The amplifier also includes means for preventing the integrator from being driven into saturation. As a result, the time for the flux-locked loop to recover from the excitation pulses generated by the spectrometer is reduced. 7 figures.

  15. Measurement of 1323 and 1487 keV resonances in 15N(α ,γ )19F with the recoil separator ERNA

    NASA Astrophysics Data System (ADS)

    Di Leva, A.; Imbriani, G.; Buompane, R.; Gialanella, L.; Best, A.; Cristallo, S.; De Cesare, M.; D'Onofrio, A.; Duarte, J. G.; Gasques, L. R.; Morales-Gallegos, L.; Pezzella, A.; Porzio, G.; Rapagnani, D.; Roca, V.; Romoli, M.; Schürmann, D.; Straniero, O.; Terrasi, F.; ERNA Collaboration

    2017-04-01

    Background: The origin of fluorine is a widely debated issue. Nevertheless, the 15N(α ,γ )19F reaction is a common feature among the various production channels so far proposed. Its reaction rate at relevant temperatures is determined by a number of narrow resonances together with the direct capture and the tails of the two broad resonances at Ec .m .=1323 and 1487 keV. Purpose: The broad resonances widths, Γγ and Γα, have to be measured with adequate precision in order to better determine their contribution to the 15N(α ,γ )19F stellar reaction rate. Methods: Measurement through the direct detection of the 19F recoil ions with the European Recoil separator for Nuclear Astrophysics (ERNA) were performed. The reaction was initiated by a 15N beam impinging onto a 4He windowless gas target. The observed yield of the resonances at Ec .m .=1323 and 1487 keV is used to determine their widths in the α and γ channels. Results: We show that a direct measurement of the cross section of the 15N(α ,γ )19F reaction can be successfully obtained with the recoil separator ERNA, and the widths Γγ and Γα of the two broad resonances have been determined. While a fair agreement is found with earlier determination of the widths of the 1487 keV resonance, a significant difference is found for the 1323 keV resonance Γα. Conclusions: The revision of the widths of the two more relevant broad resonances in the 15N(α ,γ )19F reaction presented in this work is the first step toward a more firm determination of the reaction rate. At present, the residual uncertainty at the temperatures of the 19F stellar nucleosynthesis is dominated by the uncertainties affecting the direct capture component and the 364 keV narrow resonance, both so far investigated only through indirect experiments.

  16. Decoherence and fluctuation dynamics of the quantum dot nuclear spin bath probed by nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Chekhovich, Evgeny A.

    2017-06-01

    Dynamics of nuclear spin decoherence and nuclear spin flip-flops in self-assembled InGaAs/GaAs quantum dots are studied experimentally using optically detected nuclear magnetic resonance (NMR). Nuclear spin-echo decay times are found to be in the range 1-4 ms. This is a factor of ~3 longer than in strain-free GaAs/AlGaAs structures and is shown to result from strain-induced quadrupolar effects that suppress nuclear spin flip-flops. The correlation times of the flip-flops are examined using a novel frequency-comb NMR technique and are found to exceed 1 s, a factor of ~1000 longer than in strain-free structures. These findings complement recent studies of electron spin coherence and reveal the paradoxical dual role of the quadrupolar effects in self-assembled quantum dots: large increase of the nuclear spin bath coherence and at the same time significant reduction of the electron spin-qubit coherence. Approaches to increasing electron spin coherence are discussed. In particular the nanohole filled GaAs/AlGaAs quantum dots are an attractive option: while their optical quality matches the self-assembled dots the quadrupolar effects measured in NMR spectra are a factor of 1000 smaller.

  17. High-resolution (19)F MAS NMR spectroscopy: structural disorder and unusual J couplings in a fluorinated hydroxy-silicate.

    PubMed

    Griffin, John M; Yates, Jonathan R; Berry, Andrew J; Wimperis, Stephen; Ashbrook, Sharon E

    2010-11-10

    High-resolution (19)F magic angle spinning (MAS) NMR spectroscopy is used to study disorder and bonding in a crystalline solid. (19)F MAS NMR reveals four distinct F sites in a 50% fluorine-substituted deuterated hydrous magnesium silicate (clinohumite, 4Mg(2)SiO(4)·Mg(OD(1-x)F(x))(2) with x = 0.5), indicating extensive structural disorder. The four (19)F peaks can be assigned using density functional theory (DFT) calculations of NMR parameters for a number of structural models with a range of possible local F environments generated by F(-)/OH(-) substitution. These assignments are supported by two-dimensional (19)F double-quantum MAS NMR experiments that correlate F sites based on either spatial proximity (via dipolar couplings) or through-bond connectivity (via scalar, or J, couplings). The observation of (19)F-(19)F J couplings is unexpected as the fluorines coordinate Mg atoms and the Mg-F interaction is normally considered to be ionic in character (i.e., there is no formal F-Mg-F covalent bonding arrangement). However, DFT calculations predict significant (19)F-(19)F J couplings, and these are in good agreement with the splittings observed in a (19)F J-resolved MAS NMR experiment. The existence of these J couplings is discussed in relation to both the nature of bonding in the solid state and the occurrence of so-called "through-space" (19)F-(19)F J couplings in solution. Finally, we note that we have found similar structural disorder and spin-spin interactions in both synthetic and naturally occurring clinohumite samples.

  18. Line broadening interference for high-resolution nuclear magnetic resonance spectra under inhomogeneous magnetic fields

    SciTech Connect

    Wei, Zhiliang; Yang, Jian; Lin, Yanqin E-mail: chenz@xmu.edu.cn; Chen, Zhong E-mail: chenz@xmu.edu.cn; Chen, Youhe

    2015-04-07

    Nuclear magnetic resonance spectroscopy serves as an important tool for analyzing chemicals and biological metabolites. However, its performance is subject to the magnetic-field homogeneity. Under inhomogeneous fields, peaks are broadened to overlap each other, introducing difficulties for assignments. Here, we propose a method termed as line broadening interference (LBI) to provide high-resolution information under inhomogeneous magnetic fields by employing certain gradients in the indirect dimension to interfere the magnetic-field inhomogeneity. The conventional spectral-line broadening is thus interfered to be non-diagonal, avoiding the overlapping among adjacent resonances. Furthermore, an inhomogeneity correction algorithm is developed based on pattern recognition to recover the high-resolution information from LBI spectra. Theoretical deductions are performed to offer systematic and detailed analyses on the proposed method. Moreover, experiments are conducted to prove the feasibility of the proposed method for yielding high-resolution spectra in inhomogeneous magnetic fields.

  19. Line broadening interference for high-resolution nuclear magnetic resonance spectra under inhomogeneous magnetic fields.

    PubMed

    Wei, Zhiliang; Yang, Jian; Chen, Youhe; Lin, Yanqin; Chen, Zhong

    2015-04-07

    Nuclear magnetic resonance spectroscopy serves as an important tool for analyzing chemicals and biological metabolites. However, its performance is subject to the magnetic-field homogeneity. Under inhomogeneous fields, peaks are broadened to overlap each other, introducing difficulties for assignments. Here, we propose a method termed as line broadening interference (LBI) to provide high-resolution information under inhomogeneous magnetic fields by employing certain gradients in the indirect dimension to interfere the magnetic-field inhomogeneity. The conventional spectral-line broadening is thus interfered to be non-diagonal, avoiding the overlapping among adjacent resonances. Furthermore, an inhomogeneity correction algorithm is developed based on pattern recognition to recover the high-resolution information from LBI spectra. Theoretical deductions are performed to offer systematic and detailed analyses on the proposed method. Moreover, experiments are conducted to prove the feasibility of the proposed method for yielding high-resolution spectra in inhomogeneous magnetic fields.

  20. Detection and estimation of magnetization induced resonances in unilateral nuclear magnetic resonance (NMR) sensors

    NASA Astrophysics Data System (ADS)

    Prabhu Gaunkar, N.; Bulu, I.; Song, Y. Q.; Mina, M.; Jiles, D. C.

    2017-05-01

    In this work a systematic identification of factors contributing to signal ringing in unilateral nuclear magnetic resonance (NMR) sensors is conducted. Resonant peaks that originate due to multiple factors such as NMR, electrical, magneto-acoustic, core material response, eddy currents and other factors were observed. The peaks caused by the measurement system or electrical resonances and induced magnet vibrations are further analyzed. They appear in every measurement and are considered as interference to signals received from the magnetic core. Forming a distinction between different peaks is essential in identifying the primary contribution to the captured resonant signal. The measurements for the magnetic core indicate that the magnetization induced resonant peaks of the core have relatively higher amplitudes and shorter decay times at low frequencies.

  1. Nuclear-Targeted Multifunctional Magnetic Nanoparticles for Photothermal Therapy.

    PubMed

    Peng, Haibao; Tang, Jing; Zheng, Rui; Guo, Guannan; Dong, Angang; Wang, Yajun; Yang, Wuli

    2017-01-27

    The pursuit of multifunctional, innovative, more efficient, and safer cancer treatment has gained increasing interest in the research of preclinical nanoparticle-mediated photothermal therapy (PTT). Cell nucleus is recognized as the ideal target for cancer treatment because it plays a central role in genetic information and the transcription machinery reside. In this work, an efficient nuclear-targeted PTT strategy is proposed using transferrin and TAT peptide (TAT: YGRKKRRQRRR) conjugated monodisperse magnetic nanoparticles, which can be readily functionalized and stabilized for potential diagnostic and therapeutic applications. The monodisperse magnetic nanoparticles exhibit high photothermal conversion efficiency (≈37%) and considerable photothermal stability. They also show a high magnetization value and transverse relaxivity (207.1 mm(-1) s(-1) ), which could be applied for magnetic resonance imaging. The monodisperse magnetic nanoparticles conjugated with TAT peptides can efficiently target the nucleus and achieve the imaging-guided function, efficient cancer cells killing ability. Therefore, this work may present a practicable strategy to develop subcellular organelle targeted PTT agents for simultaneous cancer targeting, imaging, and therapy.

  2. [Qualitative and quantitative analysis of fluoxetine hydrochloride by 19F NMR].

    PubMed

    Yang, Bai-Qin; Kong, Er-Li; Xue, Xiao-Di; Zhao, Shou-Qian; Lin, Shrong-Shi

    2012-05-01

    The chemical shift of fluoxetine hydrochloride appears at delta 14.15 in 19F NMR analysis. The delta moved upfield slightly from 14.158 to 14.145 when the concentration of solution became diluted from 2.00 to 0.05 mmol x L(-1). Spiking test was suggested to confirm the existence of the compound for qualitative analysis. 19F NMR detection sensitivity test illustrated that a concentration of 17 mg in 1 L water could be detected while the sample was scanned 500 times with optimum parameters. In quantitative analysis, standard curve of concentration versus fluorine signal intensity was proposed to determine the amount of fluoxetine. Long capillary tube containing trifluoroacetic acid was used as internal standard for the integration measurements and straight line was obtained with good fitting. Direct additions of trifluoroethanol to fluoxetine solutions gave a poorer standard curve.

  3. Structure Determination Using 19-F NMR: A Simple Fluorination Experiment of Cinnamyl Alcohol

    NASA Astrophysics Data System (ADS)

    Demendonca, Daniel J.; Digits, Cheryl A.; Navin, Erin W.; Sander, Tanya C.; Hammond, Gerald B.

    1995-08-01

    Described here is the nucleophilic substitution of a hydroxyl group, in cinnamyl alcohol, by fluorine, and analysis of the product using 19-F NMR spectroscopy. This experiment brings important innovations to the teaching of experimental organic chemistry at the undergraduate level. The fluorination of cinnamyl alcohol requires only a mild fluorinating agent and so it provides the student with a direct contact with organofluorine, chemistry. The allylic nucleophilic substitution typified by our experiment will enhance the instruction of nucleophilic substitution in the laboratory, traditionally limited to SN1 or SN2 substitutions. Because the ratio of SN2 to SN2' derived products cannot be determined directly using 1-H NMR spectroscopy but it can be measured easily using 19-F NMR spectroscopy. The experiment gives the student a firsthand experience of the usefulness of NMR spectra of different nuclei.

  4. Using O2 to probe membrane immersion depth by 19F NMR

    PubMed Central

    Prosser, R. Scott; Luchette, Paul A.; Westerman, Philip W.

    2000-01-01

    A fluorinated detergent, CF3(CF2)5C2H4-O-maltose, was reconstituted into a lipid bilayer model membrane system to demonstrate the feasibility of determining solvent accessibility and membrane immersion depth of each fluorinated group by 19F NMR. Apolar oxygen, which is known to partition with an increasing concentration gradient toward the hydrophobic membrane interior, exhibits a range of paramagnetic relaxation effects on 19F nuclei, depending on its depth in the membrane. This effect, which is predominately associated with spin-lattice relaxation rates (R1) and chemical shifts, can be amplified greatly with minimal line broadening by increasing the partial pressure of O2 at least 100-fold (i.e., PO2 greater than 20 bar). The differences of longitudinal relaxation rates at 20 bar of oxygen pressure to those under ambient pressure (R120bar − R10) are largest for those fluorine groups expected to be most deeply buried in the membrane bilayer. This result contrasts with the reverse trend, which is observed on addition of a membrane surface-associated paramagnetic species, 4-(N,N-dimethyl-N-hexadecyl) ammonium-2,2,6,6-tetramethylpiperidine-1-oxyl iodide (CAT-16) at ambient pressures. Thus, differential relaxation rates may be observed in 19F-labeled membrane-associated molecules resulting from the addition of apolar oxygen under high pressure. The results demonstrate that the degree of solvent accessibility and membrane immersion depth of specific fluorinated species in membrane-associated macromolecules can be probed by 19F NMR. PMID:10954744

  5. Highly sensitive detection of protein biomarkers via nuclear magnetic resonance biosensor with magnetically engineered nanoferrite particles.

    PubMed

    Jeun, Minhong; Park, Sungwook; Lee, Hakho; Lee, Kwan Hyi

    Magnetic-based biosensors are attractive for on-site detection of biomarkers due to the low magnetic susceptibility of biological samples. Here, we report a highly sensitive magnetic-based biosensing system that is composed of a miniaturized nuclear magnetic resonance (NMR) device and magnetically engineered nanoferrite particles (NFPs). The sensing performance, also identified as the transverse relaxation (R2) rate, of the NMR device is directly related to the magnetic properties of the NFPs. Therefore, we developed magnetically engineered NFPs (MnMg-NFP) and used them as NMR agents to exhibit a significantly improved R2 rate. The magnetization of the MnMg-NFPs was increased by controlling the Mn and Mg cation concentration and distribution during the synthesis process. This modification of the Mn and Mg cation directly contributed to improving the R2 rate. The miniaturized NMR system, combined with the magnetically engineered MnMg-NFPs, successfully detected a small amount of infectious influenza A H1N1 nucleoprotein with high sensitivity and stability.

  6. Magnetism and nuclear magnetic resonance of hectorite and montmorillonite layered silicates

    NASA Astrophysics Data System (ADS)

    Levin, E. M.; Hou, S.-S.; Bud'ko, S. L.; Schmidt-Rohr, K.

    2004-11-01

    The temperature and magnetic-field (H) dependencies of the bulk dc magnetization (M) and the M /H ratio of montmorillonite (MMT), hectorite (HCT), and synthetic mica-montmorillonite (SMMT) clays have been measured and compared with the signal intensity of H1 and Si29 nuclear magnetic resonance (NMR) spectra. MMT exhibits Langevin paramagnetism with an effective magnetic moment of 5.5±0.1μB per Fe ion whereas SMMT has diamagnetic properties. At 300K, M /H of HCT measured in a magnetic field of H ⩽1kOe is larger than that of MMT, whereas in a field of 50kOe, the inverse situation is observed. The difference arises because the magnetization of HCT is dominated by a contribution from ferromagneticlike impurities. The H1 and Si29 NMR signals of MMT are broadened beyond detectability due to the paramagnetic effect. Although HCT contains ferromagneticlike components that result in a large M /H in low field, it yields H1 and Si29 NMR spectra with signal intensities similar to those of diamagnetic SMMT. Our data highlight that the quality of the NMR spectra is not related to the low-field magnetic susceptibility but to the bulk magnetization in the high magnetic field used for NMR.

  7. Highly sensitive detection of protein biomarkers via nuclear magnetic resonance biosensor with magnetically engineered nanoferrite particles

    PubMed Central

    Jeun, Minhong; Park, Sungwook; Lee, Hakho; Lee, Kwan Hyi

    2016-01-01

    Magnetic-based biosensors are attractive for on-site detection of biomarkers due to the low magnetic susceptibility of biological samples. Here, we report a highly sensitive magnetic-based biosensing system that is composed of a miniaturized nuclear magnetic resonance (NMR) device and magnetically engineered nanoferrite particles (NFPs). The sensing performance, also identified as the transverse relaxation (R2) rate, of the NMR device is directly related to the magnetic properties of the NFPs. Therefore, we developed magnetically engineered NFPs (MnMg-NFP) and used them as NMR agents to exhibit a significantly improved R2 rate. The magnetization of the MnMg-NFPs was increased by controlling the Mn and Mg cation concentration and distribution during the synthesis process. This modification of the Mn and Mg cation directly contributed to improving the R2 rate. The miniaturized NMR system, combined with the magnetically engineered MnMg-NFPs, successfully detected a small amount of infectious influenza A H1N1 nucleoprotein with high sensitivity and stability. PMID:27799772

  8. First evidences for 19F(α, p)22Ne at astrophysical energies

    NASA Astrophysics Data System (ADS)

    D'Agata, G.; Spitaleri, C.; Pizzone, R. G.; Blagus, S.; Figuera, P.; Grassi, L.; Guardo, G. L.; Gulino, M.; Hayakawa, S.; Indelicato, I.; Kshetri, R.; La Cognata, M.; Lamia, L.; Lattuada, M.; Mijatović, T.; Milin, M.; Miljanic, D.; Prepolec, L.; Sergi, M. L.; Skukan, N.; Soic, N.; Tokic, V.; Tumino, A.; Uroic, M.

    2016-04-01

    19F experimental abundances is overestimated in respect to the theoretical one: it is therefore clear that further investigations are needed. We focused on the 19F(α, p) 22 Ne reaction, representing the main destruction channel in He-rich environments. The lowest energy at which this reaction has been studied with direct methods is E C.M. ≈ 0.91 MeV, while the Gamow region is between 0.39 ÷ 0.8 MeV, far below the Coulomb barrier (3.8 MeV). For this reason, an experiment at Rudjer Boskovic Institute (Zagreb) was performed, applying the Trojan Horse Method. Following this method we selected the quasi-free contribution coming from 6Li(19 F,p22 Ne)2 H at Ebeam=6 MeV at kinematically favourable angles, and the cross section at energies 0 < EC.M. < 1.4 MeV was extracted in arbitrary units, covering the astrophysical region of interest.

  9. Mechanism of dynamic nuclear polarization in high magnetic fields

    NASA Astrophysics Data System (ADS)

    Farrar, C. T.; Hall, D. A.; Gerfen, G. J.; Inati, S. J.; Griffin, R. G.

    2001-03-01

    Solid-state NMR signal enhancements of about two orders of magnitude (100-400) have been observed in dynamic nuclear polarization (DNP) experiments performed at high magnetic field (5 T) and low temperature (10 K) using the nitroxide radical 4-amino TEMPO as the source of electron polarization. Since the breadth of the 4-amino TEMPO EPR spectrum is large compared to the nuclear Larmor frequency, it has been assumed that thermal mixing (TM) is the dominate mechanism by which polarization is transferred from electron to nuclear spins. However, theoretical explanations of TM generally assume a homogeneously broadened EPR line and, since the 4-amino TEMPO line at 5 T is inhomogeneously broadened, they do not explain the observed DNP enhancements. Accordingly, we have developed a treatment of DNP that explicitly uses electron-electron cross-relaxation to mediate electron-nuclear polarization transfer. The process proceeds via spin flip-flops between pairs of electronic spin packets whose Zeeman temperatures differ from one another. To confirm the essential features of the model we have studied the field dependence of electron-electron double resonance (ELDOR) data and DNP enhancement data. Both are well simulated using a simple model of electron cross-relaxation in the inhomogeneously broadened 4-amino TEMPO EPR line.

  10. Nuclear-magnetic-resonance quantum calculations of the Jones polynomial

    PubMed Central

    Marx, Raimund; Fahmy, Amr; Kauffman, Louis; Lomonaco, Samuel; Spörl, Andreas; Pomplun, Nikolas; Schulte-Herbrüggen, Thomas; Myers, John M.; Glaser, Steffen J.

    2011-01-01

    The repertoire of problems theoretically solvable by a quantum computer recently expanded to include the approximate evaluation of knot invariants, specifically the Jones polynomial. The experimental implementation of this evaluation, however, involves many known experimental challenges. Here we present experimental results for small-scale approximate evaluation of the Jones polynomial by nuclear magnetic resonance (NMR); in addition, we show how to escape from the limitations of NMR approaches that employ pseudopure states. Specifically, we use two spin-1/2 nuclei of natural abundance chloroform and apply a sequence of unitary transforms representing the trefoil knot, the figure-eight knot, and the Borromean rings. After measuring the nuclear spin state of the molecule in each case, we are able to estimate the value of the Jones polynomial for each of the knots. PMID:21461143

  11. Magnetic Imaging: a New Tool for UK National Nuclear Security

    PubMed Central

    Darrer, Brendan J.; Watson, Joe C.; Bartlett, Paul; Renzoni, Ferruccio

    2015-01-01

    Combating illicit trafficking of Special Nuclear Material may require the ability to image through electromagnetic shields. This is the case when the trafficking involves cargo containers. Thus, suitable detection techniques are required to penetrate a ferromagnetic enclosure. The present study considers techniques that employ an electromagnetic based principle of detection. It is generally assumed that a ferromagnetic metallic enclosure will effectively act as a Faraday cage to electromagnetic radiation and therefore screen any form of interrogating electromagnetic radiation from penetrating, thus denying the detection of any eventual hidden material. In contrast, we demonstrate that it is actually possible to capture magnetic images of a conductive object through a set of metallic ferromagnetic enclosures. This validates electromagnetic interrogation techniques as a potential detection tool for National Nuclear Security applications. PMID:25608957

  12. A highly integrated FPGA-based nuclear magnetic resonance spectrometer

    NASA Astrophysics Data System (ADS)

    Takeda, Kazuyuki

    2007-03-01

    The digital circuits required for a nuclear magnetic resonance (NMR) spectrometer, including a pulse programmer, a direct digital synthesizer, a digital receiver, and a PC interface, have been built inside a single chip of the field-programmable gate-array (FPGA). By combining the FPGA chip with peripheral analog components, a compact, laptop-sized homebuilt spectrometer has been developed, which is capable of a rf output of up to 400 MHz with amplitude-, phase-, frequency-, and pulse-modulation. The number of rf channels is extendable up to three without further increase in size.

  13. A highly integrated FPGA-based nuclear magnetic resonance spectrometer.

    PubMed

    Takeda, Kazuyuki

    2007-03-01

    The digital circuits required for a nuclear magnetic resonance (NMR) spectrometer, including a pulse programmer, a direct digital synthesizer, a digital receiver, and a PC interface, have been built inside a single chip of the field-programmable gate-array (FPGA). By combining the FPGA chip with peripheral analog components, a compact, laptop-sized homebuilt spectrometer has been developed, which is capable of a rf output of up to 400 MHz with amplitude-, phase-, frequency-, and pulse-modulation. The number of rf channels is extendable up to three without further increase in size.

  14. Applications of nuclear magnetic resonance sensors to cultural heritage.

    PubMed

    Proietti, Noemi; Capitani, Donatella; Di Tullio, Valeria

    2014-04-21

    In recent years nuclear magnetic resonance (NMR) sensors have been increasingly applied to investigate, characterize and monitor objects of cultural heritage interest. NMR is not confined to a few specific applications, but rather its use can be successfully extended to a wide number of different cultural heritage issues. A breakthrough has surely been the recent development of portable NMR sensors which can be applied in situ for non-destructive and non-invasive investigations. In this paper three studies illustrating the potential of NMR sensors in this field of research are reported.

  15. Resonantly Detecting Axion-Mediated Forces with Nuclear Magnetic Resonance

    NASA Astrophysics Data System (ADS)

    Arvanitaki, Asimina; Geraci, Andrew A.

    2014-10-01

    We describe a method based on precision magnetometry that can extend the search for axion-mediated spin-dependent forces by several orders of magnitude. By combining techniques used in nuclear magnetic resonance and short-distance tests of gravity, our approach can substantially improve upon current experimental limits set by astrophysics, and probe deep into the theoretically interesting regime for the Peccei-Quinn (PQ) axion. Our method is sensitive to PQ axion decay constants between 109 and 1012 GeV or axion masses between 10-6 and 10-3 eV, independent of the cosmic axion abundance.

  16. Applications of Nuclear Magnetic Resonance Sensors to Cultural Heritage

    PubMed Central

    Proietti, Noemi; Capitani, Donatella; Di Tullio, Valeria

    2014-01-01

    In recent years nuclear magnetic resonance (NMR) sensors have been increasingly applied to investigate, characterize and monitor objects of cultural heritage interest. NMR is not confined to a few specific applications, but rather its use can be successfully extended to a wide number of different cultural heritage issues. A breakthrough has surely been the recent development of portable NMR sensors which can be applied in situ for non-destructive and non-invasive investigations. In this paper three studies illustrating the potential of NMR sensors in this field of research are reported. PMID:24755519

  17. A versatile pulse programmer for pulsed nuclear magnetic resonance spectroscopy.

    NASA Technical Reports Server (NTRS)

    Tarr, C. E.; Nickerson, M. A.

    1972-01-01

    A digital pulse programmer producing the standard pulse sequences required for pulsed nuclear magnetic resonance spectroscopy is described. In addition, a 'saturation burst' sequence, useful in the measurement of long relaxation times in solids, is provided. Both positive and negative 4 V trigger pulses are produced that are fully synchronous with a crystal-controlled time base, and the pulse programmer may be phase-locked with a maximum pulse jitter of 3 ns to the oscillator of a coherent pulse spectrometer. Medium speed TTL integrated circuits are used throughout.

  18. Nuclear Magnetic Resonance Applications to Unconventional Fossil Fuel Resources

    NASA Astrophysics Data System (ADS)

    Kleinberg, R. L.; Leu, G.

    2008-12-01

    Technical and economic projections strongly suggest that fossil fuels will continue to play a dominant role in the global energy market through at least the mid twenty-first century. However, low-cost conventional oil and gas will be depleted in that time frame. Therefore new sources of energy will be needed. We discuss two relatively untapped unconventional fossil fuels: heavy oil and gas hydrate. In both cases, nuclear magnetic resonance plays a key role in appraising the resource and providing information needed for designing production processes.

  19. Nuclear magnetic resonance: principles of blood flow imaging

    SciTech Connect

    Mills, C.M.; Brant-Zawadzki, M.; Crooks, L.E.; Kaufman, L.; Sheldon, P.; Norman, D.; Bank, W.; Newton, T.H.

    1984-01-01

    Nuclear magnetic resonance (NMR) imaging with spin-echo techniques defines vascular structures with superb anatomic detail. Contrast agents are not necessary as there is intrinsic contrast between flowing blood and the vascular wall. The signal intensity from blood within the vessel lumen varies with the sequence of gradient and radiofrequency pulses used to generate the image as well as with the velocity of blood flow. Appropriate imaging techniques can optimize anatomic detail, distinguish slow from rapidly flowing blood, and serve to identify marked impairment or complete obstruction of flow in an artery or vein. Some examples of these principles in the intracranial circulation are illustrated.

  20. Random matrix theory in biological nuclear magnetic resonance spectroscopy.

    PubMed Central

    Lacelle, S

    1984-01-01

    The statistical theory of energy levels or random matrix theory is presented in the context of the analysis of chemical shifts of nuclear magnetic resonance (NMR) spectra of large biological systems. Distribution functions for the spacing between nearest-neighbor energy levels are discussed for uncorrelated, correlated, and random superposition of correlated energy levels. Application of this approach to the NMR spectra of a vitamin, an antibiotic, and a protein demonstrates the state of correlation of an ensemble of energy levels that characterizes each system. The detection of coherent and dissipative structures in proteins becomes feasible with this statistical spectroscopic technique. PMID:6478032

  1. Nuclear magnetic resonance-based quantification of organic diphosphates.

    PubMed

    Lenevich, Stepan; Distefano, Mark D

    2011-01-15

    Phosphorylated compounds are ubiquitous in life. Given their central role, many such substrates and analogs have been prepared for subsequent evaluation. Prior to biological experiments, it is typically necessary to determine the concentration of the target molecule in solution. Here we describe a method where concentrations of stock solutions of organic diphosphates and bisphosphonates are quantified using (31)P nuclear magnetic resonance (NMR) spectroscopy with standard instrumentation using a capillary tube with a secondary standard. The method is specific and is applicable down to a concentration of 200 μM. The capillary tube provides the reference peak for quantification and deuterated solvent for locking.

  2. Development of Metallic Magnetic Calorimeters for Nuclear Safeguards Applications

    SciTech Connect

    Bates, Cameron Russell

    2015-03-11

    Many nuclear safeguards applications could benefit from high-resolution gamma-ray spectroscopy achievable with metallic magnetic calorimeters. This dissertation covers the development of a system for these applications based on gamma-ray detectors developed at the University of Heidelberg. It demonstrates new calorimeters of this type, which achieved an energy resolution of 45.5 eV full-width at half-maximum at 59.54 keV, roughly ten times better than current state of the art high purity germanium detectors. This is the best energy resolution achieved with a gamma-ray metallic magnetic calorimeter at this energy to date. In addition to demonstrating a new benchmark in energy resolution, an experimental system for measuring samples with metallic magnetic calorimeters was constructed at Lawrence Livermore National Laboratory. This system achieved an energy resolution of 91.3 eV full-width at half-maximum at 59.54 keV under optimal conditions. Using this system it was possible to characterize the linearity of the response, the count-rate limitations, and the energy resolution as a function of temperature of the new calorimeter. With this characterization it was determined that it would be feasible to measure 242Pu in a mixed isotope plutonium sample. A measurement of a mixed isotope plutonium sample was performed over the course of 12 days with a single two-pixel metallic magnetic calorimeter. The relative concentration of 242Pu in comparison to other plutonium isotopes was determined by direct measurement to less than half a percent accuracy. This is comparable with the accuracy of the best-case scenario using traditional indirect methods. The ability to directly measure the relative concentration of 242Pu in a sample could enable more accurate accounting and detection of indications of undeclared activities in nuclear safeguards, a better constraint on source material in forensic samples containing plutonium, and improvements in verification in a future plutonium

  3. A personal computer-based nuclear magnetic resonance spectrometer

    NASA Astrophysics Data System (ADS)

    Job, Constantin; Pearson, Robert M.; Brown, Michael F.

    1994-11-01

    Nuclear magnetic resonance (NMR) spectroscopy using personal computer-based hardware has the potential of enabling the application of NMR methods to fields where conventional state of the art equipment is either impractical or too costly. With such a strategy for data acquisition and processing, disciplines including civil engineering, agriculture, geology, archaeology, and others have the possibility of utilizing magnetic resonance techniques within the laboratory or conducting applications directly in the field. Another aspect is the possibility of utilizing existing NMR magnets which may be in good condition but unused because of outdated or nonrepairable electronics. Moreover, NMR applications based on personal computer technology may open up teaching possibilities at the college or even secondary school level. The goal of developing such a personal computer (PC)-based NMR standard is facilitated by existing technologies including logic cell arrays, direct digital frequency synthesis, use of PC-based electrical engineering software tools to fabricate electronic circuits, and the use of permanent magnets based on neodymium-iron-boron alloy. Utilizing such an approach, we have been able to place essentially an entire NMR spectrometer console on two printed circuit boards, with the exception of the receiver and radio frequency power amplifier. Future upgrades to include the deuterium lock and the decoupler unit are readily envisioned. The continued development of such PC-based NMR spectrometers is expected to benefit from the fast growing, practical, and low cost personal computer market.

  4. Nuclear conversion theory: molecular hydrogen in non-magnetic insulators

    NASA Astrophysics Data System (ADS)

    Ilisca, Ernest; Ghiglieno, Filippo

    2016-09-01

    The hydrogen conversion patterns on non-magnetic solids sensitively depend upon the degree of singlet/triplet mixing in the intermediates of the catalytic reaction. Three main `symmetry-breaking' interactions are brought together. In a typical channel, the electron spin-orbit (SO) couplings introduce some magnetic excitations in the non-magnetic solid ground state. The electron spin is exchanged with a molecular one by the electric molecule-solid electron repulsion, mixing the bonding and antibonding states and affecting the molecule rotation. Finally, the magnetic hyperfine contact transfers the electron spin angular momentum to the nuclei. Two families of channels are considered and a simple criterion based on the SO coupling strength is proposed to select the most efficient one. The denoted `electronic' conversion path involves an emission of excitons that propagate and disintegrate in the bulk. In the other denoted `nuclear', the excited electron states are transients of a loop, and the electron system returns to its fundamental ground state. The described model enlarges previous studies by extending the electron basis to charge-transfer states and `continui' of band states, and focuses on the broadening of the antibonding molecular excited state by the solid conduction band that provides efficient tunnelling paths for the hydrogen conversion. After working out the general conversion algebra, the conversion rates of hydrogen on insulating and semiconductor solids are related to a few molecule-solid parameters (gap width, ionization and affinity potentials) and compared with experimental measures.

  5. Nuclear conversion theory: molecular hydrogen in non-magnetic insulators.

    PubMed

    Ilisca, Ernest; Ghiglieno, Filippo

    2016-09-01

    The hydrogen conversion patterns on non-magnetic solids sensitively depend upon the degree of singlet/triplet mixing in the intermediates of the catalytic reaction. Three main 'symmetry-breaking' interactions are brought together. In a typical channel, the electron spin-orbit (SO) couplings introduce some magnetic excitations in the non-magnetic solid ground state. The electron spin is exchanged with a molecular one by the electric molecule-solid electron repulsion, mixing the bonding and antibonding states and affecting the molecule rotation. Finally, the magnetic hyperfine contact transfers the electron spin angular momentum to the nuclei. Two families of channels are considered and a simple criterion based on the SO coupling strength is proposed to select the most efficient one. The denoted 'electronic' conversion path involves an emission of excitons that propagate and disintegrate in the bulk. In the other denoted 'nuclear', the excited electron states are transients of a loop, and the electron system returns to its fundamental ground state. The described model enlarges previous studies by extending the electron basis to charge-transfer states and 'continui' of band states, and focuses on the broadening of the antibonding molecular excited state by the solid conduction band that provides efficient tunnelling paths for the hydrogen conversion. After working out the general conversion algebra, the conversion rates of hydrogen on insulating and semiconductor solids are related to a few molecule-solid parameters (gap width, ionization and affinity potentials) and compared with experimental measures.

  6. Nuclear conversion theory: molecular hydrogen in non-magnetic insulators

    NASA Astrophysics Data System (ADS)

    Ilisca, Ernest; Ghiglieno, Filippo

    2016-09-01

    The hydrogen conversion patterns on non-magnetic solids sensitively depend upon the degree of singlet/triplet mixing in the intermediates of the catalytic reaction. Three main `symmetry-breaking' interactions are brought together. In a typical channel, the electron spin-orbit (SO) couplings introduce some magnetic excitations in the non-magnetic solid ground state. The electron spin is exchanged with a molecular one by the electric molecule-solid electron repulsion, mixing the bonding and antibonding states and affecting the molecule rotation. Finally, the magnetic hyperfine contact transfers the electron spin angular momentum to the nuclei. Two families of channels are considered and a simple criterion based on the SO coupling strength is proposed to select the most efficient one. The denoted `electronic' conversion path involves an emission of excitons that propagate and disintegrate in the bulk. In the other denoted `nuclear', the excited electron states are transients of a loop, and the electron system returns to its fundamental ground state. The described model enlarges previous studies by extending the electron basis to charge-transfer states and `continui' of band states, and focuses on the broadening of the antibonding molecular excited state by the solid conduction band that provides efficient tunnelling paths for the hydrogen conversion. After working out the general conversion algebra, the conversion rates of hydrogen on insulating and semiconductor solids are related to a few molecule-solid parameters (gap width, ionization and affinity potentials) and compared with experimental measures.

  7. Verification of threshold activation detection (TAD) technique in prompt fission neutron detection using scintillators containing 19F

    NASA Astrophysics Data System (ADS)

    Sibczynski, P.; Kownacki, J.; Moszyński, M.; Iwanowska-Hanke, J.; Syntfeld-Każuch, A.; Gójska, A.; Gierlik, M.; Kaźmierczak, Ł.; Jakubowska, E.; Kędzierski, G.; Kujawiński, Ł.; Wojnarowicz, J.; Carrel, F.; Ledieu, M.; Lainé, F.

    2015-09-01

    In the present study ⌀ 5''× 3'' and ⌀ 2''× 2'' EJ-313 liquid fluorocarbon as well as ⌀ 2'' × 3'' BaF2 scintillators were exposed to neutrons from a 252Cf neutron source and a Sodern Genie 16GT deuterium-tritium (D+T) neutron generator. The scintillators responses to β- particles with maximum endpoint energy of 10.4 MeV from the n+19F reactions were studied. Response of a ⌀ 5'' × 3'' BC-408 plastic scintillator was also studied as a reference. The β- particles are the products of interaction of fast neutrons with 19F which is a component of the EJ-313 and BaF2 scintillators. The method of fast neutron detection via fluorine activation is already known as Threshold Activation Detection (TAD) and was proposed for photofission prompt neutron detection from fissionable and Special Nuclear Materials (SNM) in the field of Homeland Security and Border Monitoring. Measurements of the number of counts between 6.0 and 10.5 MeV with a 252Cf source showed that the relative neutron detection efficiency ratio, defined as epsilonBaF2 / epsilonEJ-313-5'', is 32.0% ± 2.3% and 44.6% ± 3.4% for front-on and side-on orientation of the BaF2, respectively. Moreover, the ⌀ 5'' EJ-313 and side-on oriented BaF2 were also exposed to neutrons from the D+T neutron generator, and the relative efficiency epsilonBaF2 / epsilonEJ-313-5'' was estimated to be 39.3%. Measurements of prompt photofission neutrons with the BaF2 detector by means of data acquisition after irradiation (out-of-beam) of nuclear material and between the beam pulses (beam-off) techniques were also conducted on the 9 MeV LINAC of the SAPHIR facility.

  8. Probing atomic scale transformation of fossil dental enamel using Fourier transform infrared and nuclear magnetic resonance spectroscopy: a case study from the Tugen Hills (Rift Gregory, Kenya).

    PubMed

    Yi, Haohao; Balan, Etienne; Gervais, Christel; Ségalen, Loïc; Roche, Damien; Person, Alain; Fayon, Franck; Morin, Guillaume; Babonneau, Florence

    2014-09-01

    A series of fossil tooth enamel samples was investigated by Fourier transform infrared (FTIR) spectroscopy, (13)C and (19)F magic-angle spinning nuclear magnetic resonance (MAS NMR) and scanning electron microscopy (SEM). Tooth remains were collected in Mio-Pliocene deposits of the Tugen Hills in Kenya. Significant transformations were observed in fossil enamel as a function of increasing fluorine content (up to 2.8wt.%). FTIR spectroscopy revealed a shift of the ν1 PO4 stretching band to higher frequency. The ν2 CO3 vibrational band showed a decrease in the intensity of the primary B-type carbonate signal, which was replaced by a specific band at 864cm(-1). This last band was ascribed to a specific carbonate environment in which the carbonate group is closely associated to a fluoride ion. The occurrence of this carbonate defect was consistently attested by the observation of two different fluoride signals in the (19)F NMR spectra. One main signal, at ∼-100ppm, is related to structural F ions in the apatite channel and the other, at -88ppm, corresponds to the composite defect. These spectroscopic observations can be understood as resulting from the mixture of two phases: biogenic hydroxylapatite (bioapatite) and secondary fluorapatite. SEM observations of the most altered sample confirmed the extensive replacement of the bioapatite by fluorapatite, resulting from the dissolution of the primary bioapatite followed by the precipitation of carbonate-fluorapatite. The ν2 CO3 IR bands can be efficiently used to monitor the extent of this type of bioapatite transformation during fossilization.

  9. Rotating-frame gradient fields for magnetic resonance imaging and nuclear magnetic resonance in low fields

    SciTech Connect

    Bouchard, Louis-Serge; Pines, Alexander; Demas, Vasiliki

    2014-01-21

    A system and method for Fourier encoding a nuclear magnetic resonance (NMR) signal is disclosed. A static magnetic field B.sub.0 is provided along a first direction. An NMR signal from the sample is Fourier encoded by applying a rotating-frame gradient field B.sub.G superimposed on the B.sub.0, where the B.sub.G comprises a vector component rotating in a plane perpendicular to the first direction at an angular frequency .omega.in a laboratory frame. The Fourier-encoded NMR signal is detected.

  10. Pre-equilibrium emission and clustering in medium-mass nuclei: 46Ti from 16O + 30Si, 18O + 28Si, 19F + 27Al

    NASA Astrophysics Data System (ADS)

    Cicerchia, M.; Marchi, T.; Gramegna, F.; Cinausero, M.; Mabiala, J.; Fabris, D.; Caciolli, A.; Collazzuol, G.; Mengoni, D.; Degerlier, M.; Morelli, L.; Bruno, M.; D'Agostino, M.; Barlini, S.; Bini, M.; Pasquali, G.; Piantelli, S.; Casini, G.; Pastore, G.; Gruyer, D.; Ottanelli, P.; Valdrè, S.; Gelli, N.; Olmi, A.; Poggi, G.; Vardaci, E.; Lombardo, I.; Dell'Aquila, D.; Leoni, S.; Cieplicka, N.; Fornal, B.

    2017-06-01

    The study of nuclear cluster states bound by valence neutrons is a field of recent large interest. In particular, it is interesting to study the pre-formation of α-clusters in α-conjugate nuclei and the dynamical condensation of clusters during nuclear reactions. The NUCL-EX collaboration (INFN, Italy) is carrying out a research campaign studying pre-equilibrium emission of light charged particles and cluster properties of light and medium-mass nuclei. For this purpose, a comparative study of the three nuclear reactions: 16O + 30Si, 18O + 28Si and 19F + 27Al, has been recently carried out using the GARFIELD+RCo 4π setup. After a general introduction on the experimental campaign, the preliminary results for the three systems are presented.

  11. Magnetism and nuclear magnetic resonance of smectite clays and their polymer nanocomposites

    NASA Astrophysics Data System (ADS)

    Levin, E. M.; Rawal, A.; Hou, S. S.; Budko, S. L.; Schmidt-Rohr, K.

    2004-03-01

    In an effort to understand the magnetic properties of polymer-clay nanocomposites and improve their nuclear magnetic resonance (NMR) spectroscopy, we have measured the "bulk" magnetization and magnetic susceptibility of three smectite clays (2:1 layered silicates), namely natural montmorillonite (MMT), synthetic mica-montmorillonite (SMMT), and natural hectorite (HCT), and correlated these data with the ^1H and ^29Si NMR signal intensities. As observed before, HCT provides much better NMR spectra than does MMT, even though its low-field magnetic susceptibility is larger than that of MMT. The reason is that the magnetization of HCT at ambient temperature is dominated by a contribution from ferromagnetic-like impurities, while MMT exhibits Langevin paramagnetism. Based on this insight, we have improved the HCT purification procedure, introducing magnetic separation and also avoiding centrifugation which enriches the sample with carbonates. This has increased the NMR signal intensity of HCT 4-fold. The resulting improvement in the quality of ^1H-^29Si NMR spectra of HCT dispersed in a polymer matrix is demonstrated.

  12. The Design and Testing of Magnets for Nuclear Magnetic Resonance Imaging

    NASA Astrophysics Data System (ADS)

    Evans, P. R.

    Available from UMI in association with The British Library. Recently, images of the inside of the human body have been produced non-invasively using nuclear magnetic resonance (nmr). The technique involves placing the patient in a strong, homogeneous magnetic field. The heart of any nmr imaging system is the magnet that produces this field and this thesis is concerned with the design and testing of such magnets. Various computer programs have been written that allow the designer to model a magnet either in terms of axisymmetric coils, or in terms of the discrete conductors that simulate the actual form of the winding. The axisymmetric program automatically optimises the design so as to produce a uniform field, and the data from this program may be used directly to generate an appropriate helical or spiral winding. These programs not only allow the designer to produce a suitable design, but also to put tolerances on the dimensions of the conductors and formers that support the winding. The problem of removing imhomogeneities produced by dimensional inaccuracies and surrounding ferromagnetic materials is also considered. A nmr probe system has been developed that allows the homogeneity of a magnet to be assessed independently of the stability of its power supply. The probe has been used for field measurements in a magnet designed using the above techniques, and the results are presented.

  13. Detection of molecules and cells using nuclear magnetic resonance with magnetic nanoparticles

    NASA Astrophysics Data System (ADS)

    Rümenapp, Christine; Gleich, Bernhard; Mannherz, Hans Georg; Haase, Axel

    2015-04-01

    For the detection of small molecules, proteins or even cells in vitro, functionalised magnetic nanoparticles and nuclear magnetic resonance measurements can be applied. In this work, magnetic nanoparticles with the size of 5-7 nm were functionalised with antibodies to detect two model systems of different sizes, the protein avidin and Saccharomyces cerevisiae as the model organism. The synthesised magnetic nanoparticles showed a narrow size distribution, which was determined using transmission electron microscopy and dynamic light scattering. The magnetic nanoparticles were functionalised with the according antibodies via EDC/NHS chemistry. The binding of the antigen to magnetic nanoparticles was detected through the change in the NMR T2 relaxation time at 0.5 T (≈21.7 MHz). In case of a specific binding the particles cluster and the T2 relaxation time of the sample changes. The detection limit in buffer for FITC-avidin was determined to be 1.35 nM and 107 cells/ml for S. cerevisiae. For fluorescent microscopy the avidin molecules were labelled with FITC and for the detection of S. cerevisiae the magnetic nanoparticles were additionally functionalised with rhodamine. The binding of the particles to S. cerevisiae and the resulting clustering was also seen by transmission electron microscopy.

  14. Defect-induced magnetism in SiC probed by nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Zhang, Z. T.; Dmytriieva, D.; Molatta, S.; Wosnitza, J.; Wang, Yutian; Helm, M.; Zhou, Shengqiang; Kühne, H.

    2017-02-01

    We give evidence for intrinsic defect-induced bulk paramagnetism in SiC by means of 13C and 29Si nuclear magnetic resonance (NMR) spectroscopy. The temperature dependence of the internal dipole-field distribution, probed by the spin part of the NMR Knight shift and the spectral linewidth, follows the Curie law and scales very well with the macroscopic dc susceptibility. In order to quantitatively analyze the NMR spectra, a microscopic model based on dipole-dipole interactions was developed. The very good agreement between these simulations and the NMR data establishes a direct relation between the frequency distribution of the spectral intensity and the corresponding real-space volumes of nuclear spins. The presented approach by NMR can be applied to a variety of similar materials and, thus, opens a new avenue for the microscopic exploration and exploitation of diluted bulk magnetism in semiconductors.

  15. TANKS 18 AND 19-F EQUIPMENT GROUT FILL MATERIAL EVALUATION AND RECOMMENDATIONS

    SciTech Connect

    Stefanko, D.; Langton, C.

    2011-12-15

    The United States Department of Energy (US DOE) intends to remove Tanks 18-F and 19-F at the Savannah River Site (SRS) from service. The high-level waste (HLW) tanks have been isolated from the F-area Tank Farm (FTF) facilities and will be filled with cementitious grout for the purpose of: (1) physically stabilizing the empty volumes in the tanks, (2) limiting/eliminating vertical pathways from the surface to residual waste on the bottom of the tanks, (3) providing an intruder barrier, and (4) providing an alkaline, chemical reducing environment within the closure boundary to limit solubility of residual radionuclides. Bulk waste and heel waste removal equipment will remain in Tanks 18-F and 19-F when the tanks are closed. This equipment includes: mixer pumps, transfer pumps, transfer jets, equipment support masts, sampling masts and dip tube assemblies. The current Tank 18-F and 19-F closure strategy is to grout the internal void spaces in this equipment to eliminate fast vertical pathways and slow water infiltration to the residual material on the tank floor. This report documents the results of laboratory testing performed to identify a grout formulation for filling the abandoned equipment in Tanks 18-F and 19-F. The objective of this work was to formulate a flowable grout for filling internal voids of equipment that will remain in Tanks 18-F and 19-F during the final closures. This work was requested by V. A. Chander, Tank Farm Closure Engineering, in HLW-TTR-2011-008. The scope for this task is provided in the Task Technical and Quality Assurance Plan (TTQAP), SRNL-RP-2011-00587. The specific objectives of this task were to: (1) Prepare and evaluate the SRR cooling coil grout identified in WSRC-STI-2008-00298 per the TTR for this work. The cooling coil grout is a mixture of BASF MasterFlow{reg_sign} 816 cable grout (67.67 wt. %), Grade 100 ground granulated blast furnace slag (7.52 wt. %) and water (24.81 wt. %); (2) Identify equipment grout placement and

  16. Updated THM Astrophysical Factor of the 19F(p, α)16O Reaction and Influence of New Direct Data at Astrophysical Energies

    NASA Astrophysics Data System (ADS)

    La Cognata, M.; Palmerini, S.; Spitaleri, C.; Indelicato, I.; Mukhamedzhanov, A. M.; Lombardo, I.; Trippella, O.

    2015-06-01

    Fluorine nucleosynthesis represents one of the most intriguing open questions in nuclear astrophysics. It has triggered new measurements which may modify the presently accepted paradigm of fluorine production and establish fluorine as an accurate probe of the inner layers of asymptotic giant branch (AGB) stars. Both direct and indirect measurements have attempted to improve the recommended extrapolation to astrophysical energies, showing no resonances. In this work, we will demonstrate that the interplay between direct and indirect techniques represents the most suitable approach to attain the required accuracy for the astrophysical factor at low energies, {{E}c.m.}≲ 300 keV, which is of interest for fluorine nucleosynthesis in AGB stars. We will use the recently measured direct 19F{{(p,α )}16}O astrophysical factor in the 600 keV≲ {{E}c.m.}≲ 800 keV energy interval to renormalize the existing Trojan Horse Method (THM) data spanning the astrophysical energies, accounting for all identified sources of uncertainty. This has a twofold impact on nuclear astrophysics. It shows the robustness of the THM approach even in the case of direct data of questionable quality, as normalization is extended over a broad range, minimizing systematic effects. Moreover, it allows us to obtain more accurate resonance data at astrophysical energies, thanks to the improved 19F{{(p,α )}16}O direct data. Finally, the present work strongly calls for more accurate direct data at low energies, so that we can obtain a better fitting of the direct reaction mechanism contributing to the 19F{{(p,α )}16}O astrophysical factor. Indeed, this work points out that the major source of uncertainty affecting the low-energy S(E) factor is the estimate of the non-resonant contribution, as the dominant role of the 113 keV resonance is now well established.

  17. A symmetrical fluorous dendron-cyanine dye-conjugated bimodal nanoprobe for quantitative 19F MRI and NIR fluorescence bioimaging.

    PubMed

    Wang, Zhe; Yue, Xuyi; Wang, Yu; Qian, Chunqi; Huang, Peng; Lizak, Marty; Niu, Gang; Wang, Fu; Rong, Pengfei; Kiesewetter, Dale O; Ma, Ying; Chen, Xiaoyuan

    2014-08-01

    (19)F MRI and optical imaging are two powerful noninvasive molecular imaging modalities in biomedical applications. (19)F MRI has great potential for high resolution in vivo imaging, while fluorescent probes enable ultracontrast cellular/tissue imaging with high accuracy and sensitivity. A bimodal nanoprobe is developed, integrating the merits of (19)F MRI and fluorescence imaging into a single synthetic molecule, which is further engineered into nanoprobe, by addressing shortcomings of conventional contrast agents to explore the quantitative (19)F MRI and fluorescence imaging and cell tracking. Results show that this bimodal imaging nanoprobe presents high correlation of (19)F MR signal and NIR fluorescence intensity in vitro and in vivo. Additionally, this nanoprobe enables quantitative (19)F MR analysis, confirmed by a complementary fluorescence analysis. This unique feature can hardly be obtained by traditional (19)F MRI contrast agents. It is envisioned that this nanoprobe can hold great potential for quantitative and sensitive multi-modal molecular imaging. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Solid-state (19)F-NMR of peptides in native membranes.

    PubMed

    Koch, Katja; Afonin, Sergii; Ieronimo, Marco; Berditsch, Marina; Ulrich, Anne S

    2012-01-01

    To understand how membrane-active peptides (MAPs) function in vivo, it is essential to obtain structural information about them in their membrane-bound state. Most biophysical approaches rely on the use of bilayers prepared from synthetic phospholipids, i.e. artificial model membranes. A particularly successful structural method is solid-state NMR, which makes use of macroscopically oriented lipid bilayers to study selectively isotope-labelled peptides. Native biomembranes, however, have a far more complex lipid composition and a significant non-lipidic content (protein and carbohydrate). Model membranes, therefore, are not really adequate to address questions concerning for example the selectivity of these membranolytic peptides against prokaryotic vs eukaryotic cells, their varying activities against different bacterial strains, or other related biological issues.Here, we discuss a solid-state (19)F-NMR approach that has been developed for structural studies of MAPs in lipid bilayers, and how this can be translated to measurements in native biomembranes. We review the essentials of the methodology and discuss key objectives in the practice of (19)F-labelling of peptides. Furthermore, the preparation of macroscopically oriented biomembranes on solid supports is discussed in the context of other membrane models. Two native biomembrane systems are presented as examples: human erythrocyte ghosts as representatives of eukaryotic cell membranes, and protoplasts from Micrococcus luteus as membranes from Gram-positive bacteria. Based on our latest experimental experience with the antimicrobial peptide gramicidin S, the benefits and some implicit drawbacks of using such supported native membranes in solid-state (19)F-NMR analysis are discussed.

  19. Nuclear Magnetic Moment of the {sup 57}Cu Ground State

    SciTech Connect

    Minamisono, K.; Mertzimekis, T.J.; Pereira, J.; Mantica, P.F.; Pinter, J.S.; Stoker, J.B.; Tomlin, B.E.; Weerasiri, R.R.; Davies, A.D.; Hass, M.; Rogers, W.F.

    2006-03-17

    The nuclear magnetic moment of the ground state of {sup 57}Cu(I{sup {pi}}=3/2{sup -},T{sub 1/2}=196.3 ms) has been measured to be vertical bar {mu}({sup 57}Cu) vertical bar =(2.00{+-}0.05){mu}{sub N} using the {beta}-NMR technique. Together with the known magnetic moment of the mirror partner {sup 57}Ni, the spin expectation value was extracted as <{sigma}{sigma}{sub z}>=-0.78{+-}0.13. This is the heaviest isospin T=1/2 mirror pair above the {sup 40}Ca region for which both ground state magnetic moments have been determined. The discrepancy between the present results and shell-model calculations in the full fp shell giving {mu}({sup 57}Cu){approx}2.4{mu}{sub N} and <{sigma}{sigma}{sub z}>{approx}0.5 implies significant shell breaking at {sup 56}Ni with the neutron number N=28.

  20. TOPICAL REVIEW: Spatial localization in nuclear magnetic resonance spectroscopy

    NASA Astrophysics Data System (ADS)

    Keevil, Stephen F.

    2006-08-01

    The ability to select a discrete region within the body for signal acquisition is a fundamental requirement of in vivo NMR spectroscopy. Ideally, it should be possible to tailor the selected volume to coincide exactly with the lesion or tissue of interest, without loss of signal from within this volume or contamination with extraneous signals. Many techniques have been developed over the past 25 years employing a combination of RF coil properties, static magnetic field gradients and pulse sequence design in an attempt to meet these goals. This review presents a comprehensive survey of these techniques, their various advantages and disadvantages, and implications for clinical applications. Particular emphasis is placed on the reliability of the techniques in terms of signal loss, contamination and the effect of nuclear relaxation and J-coupling. The survey includes techniques based on RF coil and pulse design alone, those using static magnetic field gradients, and magnetic resonance spectroscopic imaging. Although there is an emphasis on techniques currently in widespread use (PRESS, STEAM, ISIS and MRSI), the review also includes earlier techniques, in order to provide historical context, and techniques that are promising for future use in clinical and biomedical applications.

  1. 6-Trifluoromethyl Pyridoxine: Novel 19F-NMR pH Indicator for In Vivo Detection

    PubMed Central

    Yu, Jian-Xin; Cui, Weina; Bourke, Vincent A.; Mason, Ralph P.

    2012-01-01

    pH plays an important role in tumor proliferation, angiogenesis, metabolic control and the efficacy of cytotoxic therapy, and accurate non-invasive assessment of tumor pH promises to provide insight into developmental processes and prognostic information. In this paper, we report the design, synthesis and characterization of two novel pH indicators 6-trifluoromethyl pyridoxine 8 and α4, α5-di-O-[3’-O-(β-D-glucopyranosyl)-propyl]-6-trifluoromethyl pyridoxine 17, and demonstrate 8 as an extracellular 19F-NMR pH probe to assess pHe of various tumors in vivo. PMID:22775397

  2. Pre-fission neutron emission in {sup 19}F+{sup 209}Bi reaction

    SciTech Connect

    Singh, Hardev; Sugathan, P.; Shidling, P. D.; Behera, B. R.; Singh, Gulzar; Govil, I. M.; Golda, K. S.; Jhingan, Akhil; Singh, R. P.; Chatterjee, M. B.; Datta, S. K.; Pal, Santanu; Viesti, G.

    2009-03-04

    The pre- and post-scission neutron multiplicities are measured for {sup 19}F+{sup 209}Bi reaction at E{sub lab} = 100, 104, 108, 112 and 116 MeV. The measured value of pre-scission neutron multiplicity was found to be increasing with the excitation energy. The comparison of experimental values with the statistical model calculations shows that the measured values are much larger than the model predictions. This difference in excess yield over the model predictions amounts to the survival time of 80{+-}5x10{sup -21} s for the {sup 228}U compound nucleus before it undergoes fission.

  3. 6-Trifluoromethylpyridoxine: novel (19)F NMR pH indicator for in vivo detection.

    PubMed

    Yu, Jian-Xin; Cui, Weina; Bourke, Vincent A; Mason, Ralph P

    2012-08-09

    pH plays an important role in tumor proliferation, angiogenesis, metabolic control, and the efficacy of cytotoxic therapy, and accurate noninvasive assessment of tumor pH promises to provide insight into developmental processes and prognostic information. In this paper, we report the design, synthesis, and characterization of two novel pH indicators 6-trifluoromethylpyridoxine 8 and α(4),α(5)-di-O-[3'-O-(β-d-glucopyranosyl)propyl]-6-trifluoromethylpyridoxine 17 and demonstrate 8 as an extracellular (19)F NMR pH probe to assess pH(e) of various tumors in vivo.

  4. Nuclear Magnetic Resonance Studies in Heavy Fermion Materials

    NASA Astrophysics Data System (ADS)

    Shirer, Kent Robert

    29Si, 31P, and 115In nuclear magnetic resonance studies of heavy fermion materials URu2Si 2, CeRhIn5, and URu2Si2- xPx were conducted as a function of temperature, pressure, and, in the case of URu2Si2- xPx, doping. Knight shift measurements in these systems probe the hybridization between conduction and local f-electrons which is described by the heavy fermion coherence temperature, T*, and can be captured by a two fluid model. This model takes the dual nature of the local moments and the heavy electron fluid into account. In URu2Si2 in a pressure range from 0-9.1 kbar, spin-lattice-relaxation data were taken and suggest a partial suppression of the density of states below 30 K. The data are analyzed in terms of a two component spin-fermion model. The spin-lattice-relaxation behavior is then compared to other materials that demonstrate precursor fluctuations in a pseudogap regime above a ground state with long-range order. Nuclear magnetic resonance data in CeRhIn5 for both the In(1) and In(2) sites are also taken under hydrostatic pressure. The Knight shift data reveal a suppression of the hyperfine coupling to the In(1) site as a function of pressure, and the electric field gradient at the In(2) site exhibits a change of slope. These changes to these coupling constants reflect alterations to the electronic structure at the quantum critical point. Finally, we report 31P nuclear magnetic resonance measurements in single crystals of URu2Si2-xP x with x = 0.09, 0.33. In the case of the x = 0.09 doping, we find no evidence for a phase transition, though the material still exhibits heavy fermion coherence. In the x = 0.33 doping, we find that it undergoes an antiferromagnetic (AFM) phase transition. When we include the pure compound in our analysis, we find that the hyperfine couplings and coherence temperatures evolve with doping. We compare this evolution with the trends seen in other compounds.

  5. Multinucleon transfer in O,1816,19F+208Pb reactions at energies near the fusion barrier

    NASA Astrophysics Data System (ADS)

    Rafferty, D. C.; Dasgupta, M.; Hinde, D. J.; Simenel, C.; Simpson, E. C.; Williams, E.; Carter, I. P.; Cook, K. J.; Luong, D. H.; McNeil, S. D.; Ramachandran, K.; Vo-Phuoc, K.; Wakhle, A.

    2016-08-01

    Background: Nuclear reactions are complex, involving collisions between composite systems where many-body dynamics determines outcomes. Successful models have been developed to explain particular reaction outcomes in distinct energy and mass regimes, but a unifying picture remains elusive. The irreversible transfer of kinetic energy from the relative motion of the collision partners to their internal states, as is known to occur in deep inelastic collisions, has yet to be successfully incorporated explicitly into fully quantal reaction models. The influence of these processes on fusion is not yet quantitatively understood. Purpose: To investigate the population of high excitation energies in transfer reactions at sub-barrier energies, which are precursors to deep inelastic processes, and their dependence on the internuclear separation. Methods: Transfer probabilities and excitation energy spectra have been measured in collisions of O,1816,19F+208Pb , at various energies below and around the fusion barrier, by detecting the backscattered projectile-like fragments in a Δ E -E telescope. Results: The relative yields of different transfer outcomes are strongly driven by Q values, but change with the internuclear separation. In 16O+208Pb , single nucleon transfer dominates, with a strong contribution from -2 p transfer close to the Coulomb barrier, though this channel becomes less significant in relation to the -2 p 2 n transfer channel at larger separations. For 18O+208Pb , the -2 p 2 n channel is the dominant charge transfer mode at all separations. In the reactions with 19F,-3 p 2 n transfer is significant close to the barrier, but falls off rapidly with energy. Multinucleon transfer processes are shown to lead to high excitation energies (up to ˜15 MeV), which is distinct from single nucleon transfer modes which predominantly populate states at low excitation energy. Conclusions: Kinetic energy is transferred into internal excitations following transfer, with this

  6. Analysis of ringing effects due to magnetic core materials in pulsed nuclear magnetic resonance circuits

    SciTech Connect

    Prabhu Gaunkar, N. Bouda, N. R. Y.; Nlebedim, I. C.; Hadimani, R. L.; Mina, M.; Jiles, D. C.; Bulu, I.; Ganesan, K.; Song, Y. Q.

    2015-05-07

    This work presents investigations and detailed analysis of ringing in a non-resonant pulsed nuclear magnetic resonance (NMR) circuit. Ringing is a commonly observed phenomenon in high power switching circuits. The oscillations described as ringing impede measurements in pulsed NMR systems. It is therefore desirable that those oscillations decay fast. It is often assumed that one of the causes behind ringing is the role of the magnetic core used in the antenna (acting as an inductive load). We will demonstrate that an LRC subcircuit is also set-up due to the inductive load and needs to be considered due to its parasitic effects. It is observed that the parasitics associated with the inductive load become important at certain frequencies. The output response can be related to the response of an under-damped circuit and to the magnetic core material. This research work demonstrates and discusses ways of controlling ringing by considering interrelationships between different contributing factors.

  7. A novel power amplification scheme for nuclear magnetic resonance/nuclear quadrupole resonance systems.

    PubMed

    Zhang, Xinwang; Schemm, Nathan; Balkır, Sina

    2011-03-01

    Nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR)-based chemical analysis systems have been widely utilized in various areas such as medicine, security, and academic research. In these applications, the power amplifier stage plays a key role in generating the required oscillating magnetic fields within a radio frequency coil that serves as the probe. However, the bulky size and relatively low efficiency of the traditional power amplification schemes employed present a bottleneck for the realization of compact sized and portable NMR and NQR systems. To address this problem, this work presents a class D voltage-switching power amplification scheme with novel fast-start and fast-stop functions that are suitable for generating ideal NMR and NQR excitation signals. Compared to the traditional analog power amplifiers (PAs), the proposed switched-mode PA can achieve significant improvement on the power efficiency as well as the physical volume. A PA circuit for portable NQR-based explosive detection systems has been designed and built using the proposed scheme with 1 kW possible maximum output power and 10 MHz maximum operating frequency. Test results show that the presented PA achieves more than 60% measured efficiency within a highly compact volume while sustaining fast start and stop of excitation signals in the order of microseconds.

  8. Development of a micro nuclear magnetic resonance system

    NASA Astrophysics Data System (ADS)

    Goloshevsky, Artem

    Application of Nuclear Magnetic Resonance (NMR) to on-line/in-line control of industrial processes is currently limited by equipment costs and requirements for installation. A superconducting magnet generating strong fields is the most expensive part of a typical NMR instrument. In industrial environments, fringe magnetic fields make accommodation of NMR instruments difficult. However, a portable, low-cost and low-field magnetic resonance system can be used in virtually any environment. Development of a number of hardware components for a portable, low-cost NMR instrument is reported in this dissertation. Chapter one provides a discussion on a miniaturized Helmholtz spiral radio-frequency (RF) coil (average diameter equal to 3.5 mm) and an NMR probe built around a capillary (outer diameter = 1.59 mm and inner diameter = 1.02 mm) for flow imaging. Experiments of NMR spectroscopy, static and dynamic (flow) imaging, conducted with the use of the miniaturized coil, are described. Chapter two presents a microfabricated package of two biaxial gradient coils and a Helmholtz RF coil. Planar configuration of discrete wires was used to create magnetic field gradients. Performance of the microfabricated gradient coils while imaging water flow compared well with a commercial gradient set of much larger size. Chapter three reports on flow imaging experiments with power law fluids (aqueous solutions of sodium salt of carboxymethyl cellulose (CMC)) of different viscosities, carried out in the NMR probe with the miniaturized RF coil and capillary. Viscosities of the CMC solutions were determined based on the curve fits of the velocity profiles and simultaneous measurements of the flow rates. The curve fits were carried out according to the power law model equations. The NMR viscosity measurements compared well with measurements of the same CMC samples, performed on a conventional rotational rheometer. A portable, home-built transceiver, designed for NMR applications utilizing a

  9. {sup 19}F NMR measurements of NO production in hypertensive ISIAH and OXYS rats

    SciTech Connect

    Bobko, Andrey A. . E-mail: bobko@kinetics.nsc.ru; Sergeeva, Svetlana V.; Bagryanskaya, Elena G.; Markel, Arkadii L.; Khramtsov, Valery V.; Reznikov, Vladimir A.; Kolosova, Nataljya G.

    2005-05-06

    Recently we demonstrated the principal possibility of application of {sup 19}F NMR spin-trapping technique for in vivo {sup {center_dot}}NO detection [Free Radic. Biol. Med. 36 (2004) 248]. In the present study, we employed this method to elucidate the significance of {sup {center_dot}}NO availability in animal models of hypertension. In vivo {sup {center_dot}}NO-induced conversion of the hydroxylamine of the fluorinated nitronyl nitroxide (HNN) to the hydroxylamine of the iminonitroxide (HIN) in hypertensive ISIAH and OXYS rat strains and normotensive Wistar rat strain was measured. Significantly lower HIN/HNN ratios were measured in the blood of the hypertensive rats. The NMR data were found to positively correlate with the levels of nitrite/nitrate evaluated by Griess method and negatively correlate with the blood pressure. In comparison with other traditionally used methods {sup 19}F NMR spectroscopy allows in vivo evaluation of {sup {center_dot}}NO production and provides the basis for in vivo {sup {center_dot}}NO imaging.

  10. TANK 18-F AND 19-F TANK FILL GROUT SCALE UP TEST SUMMARY

    SciTech Connect

    Stefanko, D.; Langton, C.

    2012-01-03

    High-level waste (HLW) tanks 18-F and 19-F have been isolated from FTF facilities. To complete operational closure the tanks will be filled with grout for the purpose of: (1) physically stabilizing the tanks, (2) limiting/eliminating vertical pathways to residual waste, (3) entombing waste removal equipment, (4) discouraging future intrusion, and (5) providing an alkaline, chemical reducing environment within the closure boundary to control speciation and solubility of select radionuclides. This report documents the results of a four cubic yard bulk fill scale up test on the grout formulation recommended for filling Tanks 18-F and 19-F. Details of the scale up test are provided in a Test Plan. The work was authorized under a Technical Task Request (TTR), HLE-TTR-2011-008, and was performed according to Task Technical and Quality Assurance Plan (TTQAP), SRNL-RP-2011-00587. The bulk fill scale up test described in this report was intended to demonstrate proportioning, mixing, and transportation, of material produced in a full scale ready mix concrete batch plant. In addition, the material produced for the scale up test was characterized with respect to fresh properties, thermal properties, and compressive strength as a function of curing time.

  11. Dissection of the ion-induced folding of the hammerhead ribozyme using 19F NMR

    PubMed Central

    Hammann, Christian; Norman, David G.; Lilley, David M. J.

    2001-01-01

    We have used 19F NMR to analyze the metal ion-induced folding of the hammerhead ribozyme by selective incorporation of 5fluorouridine. We have studied the chemical shift and linewidths of 19F resonances of 5-fluorouridine at the 4 and 7 positions in the ribozyme core as a function of added Mg2+. The data fit well to a simple two-state model whereby the formation of domain 1 is induced by the noncooperative binding of Mg2+ with an association constant in the range of 100 to 500 M−1, depending on the concentration of monovalent ions present. The results are in excellent agreement with data reporting on changes in the global shape of the ribozyme. However, the NMR experiments exploit reporters located in the center of the RNA sections undergoing the folding transitions, thereby allowing the assignment of specific nucleotides to the separate stages. The results define the folding pathway at high resolution and provide a time scale for the first transition in the millisecond range. PMID:11331743

  12. Phosphorus-31 nuclear magnetic resonance spectroscopy of toad retina.

    PubMed Central

    Apte, D V; Koutalos, Y; McFarlane, D K; Dawson, M J; Ebrey, T G

    1989-01-01

    Phosphorus-31 nuclear magnetic resonance (31P-NMR) spectra were obtained from living toad retinae and toad retinal extracts at 4 degrees C. Several phosphorus metabolites--nucleoside di- and triphosphates (NTP), phosphocreatine, phosphodiesters, inorganic phosphate, and phosphomonoesters--were identified from the spectra of whole retinae. The intracellular pH was determined to be 7.27 +/- 0.06 at 4 degrees C and the intracellular MgNTP/NTP ratio was at least 0.77. These results are consistent with those reported by other techniques, and they show that 31P-NMR spectroscopy can be used for noninvasively and quantitatively studying the metabolism of living toad retinae, and for monitoring its changes over time. PMID:2506940

  13. Blood species discrimination using proton nuclear magnetic resonance spectroscopy.

    PubMed

    Zailer, Elina; Diehl, Bernd W K; Monakhova, Yulia B

    2017-05-01

    Blood species identification is an important challenge in forensic science. Conventional methods used for blood species analysis are destructive and associated with time-consuming sample preparation steps. Nuclear magnetic resonance (NMR) spectroscopy is known for its nondestructive properties and fast results. This research study presents a proton ((1)H) NMR method to discriminate blood species including human, cat, dog, elephant, and bison. Characteristic signals acting as markers are observed for each species. Moreover, the data are evaluated by principle component analysis (PCA) and support vector machines (SVM). A 100% correct species recognition between human and nonhuman species is achieved using radial basis kernel function (RBF) and standardized data. The research study shows that (1)H NMR spectroscopy is a powerful tool for differentiating human and nonhuman blood showing a great significance to forensic science.

  14. First principles nuclear magnetic resonance signatures of graphene oxide.

    PubMed

    Lu, Ning; Huang, Ying; Li, Hai-bei; Li, Zhenyu; Yang, Jinlong

    2010-07-21

    Nuclear magnetic resonance (NMR) has been widely used in graphene oxide (GO) structure studies. However, the detailed relationship between its spectroscopic features and the GO structural configuration remains elusive. Based on first principles (13)C chemical shift calculations using the gauge including projector augmented waves method, we provide a reliable spectrum-structure connection. The (13)C chemical shift in GO is found to be very sensitive to the atomic environment, even for the same type of oxidation groups. Factors determining the chemical shifts of epoxy and hydroxy groups have been discussed. GO structures previously reported in the literature have been checked from the NMR point of view. The energetically favorable hydroxy chain structure is not expected to be widely existed in real GO samples according to our NMR simulations. The epoxy pair species we proposed previously is also supported by chemical shift calculations.

  15. First principles nuclear magnetic resonance signatures of graphene oxide

    NASA Astrophysics Data System (ADS)

    Lu, Ning; Huang, Ying; Li, Hai-bei; Li, Zhenyu; Yang, Jinlong

    2010-07-01

    Nuclear magnetic resonance (NMR) has been widely used in graphene oxide (GO) structure studies. However, the detailed relationship between its spectroscopic features and the GO structural configuration remains elusive. Based on first principles C13 chemical shift calculations using the gauge including projector augmented waves method, we provide a reliable spectrum-structure connection. The C13 chemical shift in GO is found to be very sensitive to the atomic environment, even for the same type of oxidation groups. Factors determining the chemical shifts of epoxy and hydroxy groups have been discussed. GO structures previously reported in the literature have been checked from the NMR point of view. The energetically favorable hydroxy chain structure is not expected to be widely existed in real GO samples according to our NMR simulations. The epoxy pair species we proposed previously is also supported by chemical shift calculations.

  16. Applications of nuclear magnetic resonance imaging in process engineering

    NASA Astrophysics Data System (ADS)

    Gladden, Lynn F.; Alexander, Paul

    1996-03-01

    During the past decade, the application of nuclear magnetic resonance (NMR) imaging techniques to problems of relevance to the process industries has been identified. The particular strengths of NMR techniques are their ability to distinguish between different chemical species and to yield information simultaneously on the structure, concentration distribution and flow processes occurring within a given process unit. In this paper, examples of specific applications in the areas of materials and food processing, transport in reactors and two-phase flow are discussed. One specific study, that of the internal structure of a packed column, is considered in detail. This example is reported to illustrate the extent of new, quantitative information of generic importance to many processing operations that can be obtained using NMR imaging in combination with image analysis.

  17. Nuclear magnetic resonance of iron and copper disease states

    SciTech Connect

    Runge, V.M.; Clanton, J.A.; Smith, F.W.; Hutchison, J.; Mallard, J.; Partain, C.L.; James, A.E. Jr.

    1983-11-01

    The tissue levels of paramagnetic ions are an important factor in the determination of T/sub 1/ values as observed by nuclear magnetic resonance (NMR) imaging. The increased levels of iron present in human disease states such as hemochromatosis lead to decreased T/sub 1/ values. The mean liver T/sub 1/ of three patients with iron storage disease was determined to be 130 msec, significantly different from the value of 154 msec, the mean for 14 normal controls. Whether NMR will be able to detect the increased copper levels in liver and brain in Wilson disease remains for further clinical trials to evaluate. NMR imaging, however, does serve as a noninvasive method for the diagnosis of states of iron overload and as a technique to follow progression of disease or response to medical therapy.

  18. Microwave-free nuclear magnetic resonance at molecular scales

    NASA Astrophysics Data System (ADS)

    Wood, James D. A.; Tetienne, Jean-Philippe; Broadway, David A.; Hall, Liam T.; Simpson, David A.; Stacey, Alastair; Hollenberg, Lloyd C. L.

    2017-07-01

    The implementation of nuclear magnetic resonance (NMR) at the nanoscale is a major challenge, as the resolution of conventional methods is limited to mesoscopic scales. Approaches based on quantum spin probes, such as the nitrogen-vacancy (NV) centre in diamond, have achieved nano-NMR under ambient conditions. However, the measurement protocols require application of complex microwave pulse sequences of high precision and relatively high power, placing limitations on the design and scalability of these techniques. Here we demonstrate NMR on a nanoscale organic environment of proton spins using the NV centre while eliminating the need for microwave manipulation of either the NV or the environmental spin states. We also show that the sensitivity of our significantly simplified approach matches that of existing techniques using the NV centre. Removing the requirement for coherent manipulation while maintaining measurement sensitivity represents a significant step towards the development of robust, non-invasive nanoscale NMR probes.

  19. Serum metabonomics of acute leukemia using nuclear magnetic resonance spectroscopy

    PubMed Central

    Musharraf, Syed Ghulam; Siddiqui, Amna Jabbar; Shamsi, Tahir; Choudhary, M. Iqbal; Rahman, Atta-ur

    2016-01-01

    Acute leukemia is a critical neoplasm of white blood cells. In order to differentiate between the metabolic alterations associated with two subtypes of acute leukemia, acute lymphoblastic leukemia (ALL) and acute myeloid leukemia (AML), we investigated the serum of ALL and AML patients and compared with two controls (healthy and aplastic anemia) using 1H NMR (nuclear magnetic resonance) spectroscopy. Thirty-seven putative metabolites were identified using Carr-Purcell-Meiboom-Gill (CPMG) sequence. The use of PLS-DA and OPLS-DA models gave results with 84.38% and 90.63% classification rate, respectively. The metabolites responsible for classification are mainly lipids, lactate and glucose. Compared with controls, ALL and AML patients showed serum metabonomic differences involving aberrant metabolism pathways including glycolysis, TCA cycle, lipoprotein changes, choline and fatty acid metabolisms. PMID:27480133

  20. Microwave-free nuclear magnetic resonance at molecular scales.

    PubMed

    Wood, James D A; Tetienne, Jean-Philippe; Broadway, David A; Hall, Liam T; Simpson, David A; Stacey, Alastair; Hollenberg, Lloyd C L

    2017-07-03

    The implementation of nuclear magnetic resonance (NMR) at the nanoscale is a major challenge, as the resolution of conventional methods is limited to mesoscopic scales. Approaches based on quantum spin probes, such as the nitrogen-vacancy (NV) centre in diamond, have achieved nano-NMR under ambient conditions. However, the measurement protocols require application of complex microwave pulse sequences of high precision and relatively high power, placing limitations on the design and scalability of these techniques. Here we demonstrate NMR on a nanoscale organic environment of proton spins using the NV centre while eliminating the need for microwave manipulation of either the NV or the environmental spin states. We also show that the sensitivity of our significantly simplified approach matches that of existing techniques using the NV centre. Removing the requirement for coherent manipulation while maintaining measurement sensitivity represents a significant step towards the development of robust, non-invasive nanoscale NMR probes.

  1. Microwave-free nuclear magnetic resonance at molecular scales

    PubMed Central

    Wood, James D. A.; Tetienne, Jean-Philippe; Broadway, David A.; Hall, Liam T.; Simpson, David A.; Stacey, Alastair

    2017-01-01

    The implementation of nuclear magnetic resonance (NMR) at the nanoscale is a major challenge, as the resolution of conventional methods is limited to mesoscopic scales. Approaches based on quantum spin probes, such as the nitrogen-vacancy (NV) centre in diamond, have achieved nano-NMR under ambient conditions. However, the measurement protocols require application of complex microwave pulse sequences of high precision and relatively high power, placing limitations on the design and scalability of these techniques. Here we demonstrate NMR on a nanoscale organic environment of proton spins using the NV centre while eliminating the need for microwave manipulation of either the NV or the environmental spin states. We also show that the sensitivity of our significantly simplified approach matches that of existing techniques using the NV centre. Removing the requirement for coherent manipulation while maintaining measurement sensitivity represents a significant step towards the development of robust, non-invasive nanoscale NMR probes. PMID:28671183

  2. Nuclear magnetic resonance spectral analysis and molecular properties of berberine

    NASA Astrophysics Data System (ADS)

    Huang, Ming-Ju; Lee, Ken S.; Hurley, Sharon J.

    An extensive theoretical study of berberine has been performed at the ab initio HF/6-31G**, HF/6-311G**, and B3LYP/6-311G** levels with and without solvent effects. The optimized structures are compared with X-ray data. We found that the optimized structures with solvent effects are in slightly better agreement with X-ray data than those without solvent effects. The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of berberine were calculated by using the gauge-independent atomic orbital (GIAO) (with and without solvent effects), CSGT, and IGAIM methods. The calculated chemical shifts were compared with the two-dimensional NMR experimental data. Overall, the calculated chemical shifts show very good agreement with the experimental results. The harmonic vibrational frequencies for berberine were calculated at the B3LYP/6-311G** level.

  3. State interrogation in nuclear magnetic resonance quantum-information processing

    SciTech Connect

    Leskowitz, Garett M.; Mueller, Leonard J.

    2004-05-01

    Reconstruction of a reduced density operator for weakly coupled systems of spins (1/2) from fits to nuclear magnetic resonance spectra is described in detail. Particular emphasis is placed on data treatment procedures that specify fewer than the 3{sup n} complete spectra that are implicitly prescribed in published references to state tomography on n-spin systems. It is shown that if the density operator is expanded in the so-called product-operator basis, it is always possible to estimate a desired coefficient in the expansion by measuring a single spectral multiplet. This simple observation can substantially reduce the experimental effort required for either complete density-matrix reconstruction or estimation of subsets of the coefficients in the product-operator expansion. A simple iterative algorithm can be used to produce reduced measurement procedures for experiments involving small numbers of qubits.

  4. Nuclear magnetic resonance imaging of induced renal lesions

    SciTech Connect

    London, D.A.; Davis, P.L.; Williams, R.D.; Crooks, L.E.; Sheldon, P.E.; Gooding, C.A.

    1983-07-01

    Nuclear magnetic resonance (NMR) images obtained after unilateral ligation of the ureter, renal artery, or renal vein in the rat were analyzed and compared with NMR images of the normal rat kidney. Anatomic and functional correlation of the induced renal lesions was made by concurrent CT and by gross examination of the excised kidneys. Many normal anatomic structures at the level of the renal hilum can be identified by high resolution NMR imaging. Differentiation of urine from renal parenchyma permits detection of gross changes both in renal function and in the mass of the renal parenchyma. NMR imaging is capable of diagnosing hydronephrosis, acute renal ischemia, and acute venous congestion in this rat model. In addition, a trend toward prolongation of the relaxation times T1 and T2 for abnormal renal parenchyma is demonstrated.

  5. Effect of a strong magnetic field on the energy yield of nuclear reactions in dense nuclear matter

    SciTech Connect

    Sekerzhitskii, V.S.

    1995-01-01

    According to modern concepts, the electron-neutron-nuclear (Aen) phase of dense highly degenerate matter can be realized in the shells of neutron stars. This phase has relatively stable and absolutely stable states of thermodynamic equilibrium. Strong magnetic fields can exist in neutron stars. For this reason, analysis of their effect on the characteristics of the Aen phase is of great interest. It is specially important to study the influence of strong magnetic fields on the energy yield of nuclear reactions in dense nuclear matter because the transition to the absolute equilibrium state proceeds through these reactions.

  6. TANK 18 AND 19-F TIER 1A EQUIPMENT FILL MOCK UP TEST SUMMARY

    SciTech Connect

    Stefanko, D.; Langton, C.

    2011-11-04

    The United States Department of Energy (US DOE) has determined that Tanks 18-F and 19-F have met the F-Tank Farm (FTF) General Closure Plan Requirements and are ready to be permanently closed. The high-level waste (HLW) tanks have been isolated from FTF facilities. To complete operational closure they will be filled with grout for the purpose of: (1) physically stabilizing the tanks, (2) limiting/eliminating vertical pathways to residual waste, (3) discouraging future intrusion, and (4) providing an alkaline, chemical reducing environment within the closure boundary to control speciation and solubility of select radionuclides. Bulk waste removal and heel removal equipment remain in Tanks 18-F and 19-F. This equipment includes the Advance Design Mixer Pump (ADMP), transfer pumps, transfer jets, standard slurry mixer pumps, equipment-support masts, sampling masts, dip tube assemblies and robotic crawlers. The present Tank 18 and 19-F closure strategy is to grout the equipment in place and eliminate vertical pathways by filling voids in the equipment to vertical fast pathways and water infiltration. The mock-up tests described in this report were intended to address placement issues identified for grouting the equipment that will be left in Tank 18-F and Tank 19-F. The Tank 18-F and 19-F closure strategy document states that one of the Performance Assessment (PA) requirements for a closed tank is that equipment remaining in the tank be filled to the extent practical and that vertical flow paths 1 inch and larger be grouted. The specific objectives of the Tier 1A equipment grout mock-up testing include: (1) Identifying the most limiting equipment configurations with respect to internal void space filling; (2) Specifying and constructing initial test geometries and forms that represent scaled boundary conditions; (3) Identifying a target grout rheology for evaluation in the scaled mock-up configurations; (4) Scaling-up production of a grout mix with the target rheology

  7. Nuclear magnetic resonance probes of membrane biophysics: Structure and dynamics

    NASA Astrophysics Data System (ADS)

    Leftin, Avigdor

    The phospholipid membrane is a self-assembled, dynamic molecular system that may exist alone in association with only water, or in complex systems comprised of multiple lipid types and proteins. In this dissertation the intra- and inter-molecular forces responsible for the atomistic, molecular and collective equilibrium structure and dynamics are studied by nuclear magnetic resonance spectroscopy (NMR). The multinuclear NMR measurements and various experimental techniques are able to provide data that enable the characterization of the hierarchical spatio-temporal organization of the phospholipid membrane. The experimental and theoretical studies conducted target membrane interactions ranging from model systems composed of only water and lipids, to multiple component domain forming membranes that are in association with peripheral and trans-membrane proteins. These measurements consisit of frequency spectrum lineshapes and nuclear-spin relaxation rates obtained using 2H NMR, 13C NMR, 31P NMR and 1H NMR. The changes of these experimental observables are interpreted within a statistical thermodynamic framework that allows the membrane structure, activation energies, and correlation times of motion to be determined. The cases presented demonstrate how fundamental principles of NMR spectroscopy may be applied to a host of membranes, leading to the biophysical characterization of membrane structure and dynamics.

  8. Single crystal nuclear magnetic resonance in spinning powders.

    PubMed

    Pell, Andrew J; Pintacuda, Guido; Emsley, Lyndon

    2011-10-14

    We present a method for selectively exciting nuclear magnetic resonances (NMRs) from well-defined subsets of crystallites from a powdered sample under magic angle spinning. Magic angle spinning induces a time dependence in the anisotropic interactions, which results in a time variation of the resonance frequencies which is different for different crystallite orientations. The proposed method exploits this by applying selective pulses, which we refer to as XS (for crystallite-selective) pulses, that follow the resonance frequencies of nuclear species within particular crystallites, resulting in the induced flip angle being orientation dependent. By selecting the radiofrequency field to deliver a 180° pulse for the target orientation and employing a train of such pulses combined with cogwheel phase cycling, we obtain a high degree of orientational selectivity with the resulting spectrum containing only contributions from orientations close to the target. Typically, this leads to the selection of between 0.1% and 10% of the crystallites, and in extreme cases to the excitation of a single orientation resulting in single crystal spectra of spinning powders. Two formulations of this method are described and demonstrated with experimental examples on [1-(13)C]-alanine and the paramagnetic compound Sm(2)Sn(2)O(7).

  9. Single crystal nuclear magnetic resonance in spinning powders

    NASA Astrophysics Data System (ADS)

    Pell, Andrew J.; Pintacuda, Guido; Emsley, Lyndon

    2011-10-01

    We present a method for selectively exciting nuclear magnetic resonances (NMRs) from well-defined subsets of crystallites from a powdered sample under magic angle spinning. Magic angle spinning induces a time dependence in the anisotropic interactions, which results in a time variation of the resonance frequencies which is different for different crystallite orientations. The proposed method exploits this by applying selective pulses, which we refer to as XS (for crystallite-selective) pulses, that follow the resonance frequencies of nuclear species within particular crystallites, resulting in the induced flip angle being orientation dependent. By selecting the radiofrequency field to deliver a 180 ○ pulse for the target orientation and employing a train of such pulses combined with cogwheel phase cycling, we obtain a high degree of orientational selectivity with the resulting spectrum containing only contributions from orientations close to the target. Typically, this leads to the selection of between 0.1% and 10% of the crystallites, and in extreme cases to the excitation of a single orientation resulting in single crystal spectra of spinning powders. Two formulations of this method are described and demonstrated with experimental examples on [1 - 13C]-alanine and the paramagnetic compound Sm2Sn2O7.

  10. Low-frequency nuclear magnetic resonance and nuclear quadrupole resonance spectrometer based on a dc superconducting quantum interference device

    SciTech Connect

    Fan, N.Q.; Clarke, J. )

    1991-06-01

    A sensitive spectrometer, based on a dc superconducting quantum interference device, for the direct detection of low-frequency pulsed nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR), is described. The frequency response extends from about 10 to 200 kHz, and the recovery time after the magnetic pulse is removed is typically 50 {mu}s. As examples, NMR spectra are shown from Pt and Cu metal powders in a magnetic field of 6 mT, and NQR spectra are shown from {sup 2}D in a tunneling methyl group and {sup 14}N in NH{sub 4}ClO{sub 4}.

  11. Optically Pumped Nuclear Magnetic Resonance in the Quantum Hall Regimes

    NASA Astrophysics Data System (ADS)

    Barrett, S. E.; Khandelwal, P.; Kuzma, N. N.; Pfeiffer, L. N.; West, K. W.

    1997-03-01

    Optical pumping enables the direct detection of the nuclear magnetic resonance signal of ^71Ga nuclei located in an electron doped GaAs quantum well.footnote S. E. Barrett et al., Phys. Rev. Lett. 72, 1368 (1994) Using this technique, measurements of the Knight shift (K_S)footnote S. E. Barrett et al., Phys. Rev. Lett. 74, 5112 (1995) and spin-lattice relaxation time (T_1)footnote R. Tycko et al., Science 268, 1460 (1995) have been carried out in the Quantum Hall regimes. This talk will focus on our latest measurements of KS and T1 near Landau level filling ν=1, which extend our earlier results to higher magnetic fields (B=12 Tesla) and lower temperatures (T < 1 Kelvin). We will compare these results to the theoretical predictionsfootnote S. L. Sondhi et al., Phys. Rev. B 47, 16419 (1993); H. A. Fertig et al., Phys. Rev. B 50, 11018 (1994) that the charged excitations of the ν = 1 ground state are novel spin textures called skyrmions. The current status of this picture will be discussed.

  12. Observation of the Nuclear Magnetic Octupole Moment of 137Ba+

    NASA Astrophysics Data System (ADS)

    Hoffman, Matthew

    Single trapped ions are ideal systems in which to test atomic physics at high precision, which can in turn be used for searches for violations of fundamental symmetries and physics beyond the standard model, in addition to quantum computation and a number of other applications. The ion is confined in ultra-high vacuum, is laser cooled to mK temperatures, and kept well isolated from the environment which allows these experimental efforts. In this thesis, a few diagnostic techniques will be discussed, covering a method to measure the linewidth of a narrowband laser in the presence of magnetic field noise, as well as a procedure to measure the ion's temperature using such a narrowband laser. This work has led to two precision experiments to measure atomic structure in 138Ba+, and 137Ba+ discussed here. First, employing laser and radio frequency spectroscopy techniques in 138Ba+, we measured the Lande- gJ factor of the 5D5/2 level at the part-per-million level, the highest precision to date. Later, the development of apparatus to efficiently trap and laser cool 137Ba+ has enabled a measurement of the hyperfine splittings of the 5D3/2 manifold, culminating in the observation of the nuclear magnetic octupole moment of 137Ba+.

  13. Nuclear Magnetic Shieldings of Stacked Aromatic and Antiaromatic Molecules.

    PubMed

    Sundholm, Dage; Rauhalahti, Markus; Özcan, Nergiz; Mera-Adasme, Raúl; Kussmann, Jörg; Luenser, Arne; Ochsenfeld, Christian

    2017-04-04

    Nuclear magnetic shieldings have been calculated at the density functional theory (DFT) level for stacks of benzene, hexadehydro[12]annulene, dodecadehydro[18]annulene, and hexabenzocoronene. The magnetic shieldings due to the ring currents in the adjacent molecules have been estimated by calculating nucleus independent molecular shieldings for the monomer in the atomic positions of neighbor molecules. The calculations show that the independent shielding model works reasonably well for the (1)H NMR shieldings of benzene and hexadehydro[12]annulene, whereas for the larger molecules and for the (13)C NMR shieldings the interaction between the molecules leads to shielding effects that are at least of the same size as the ring current contributions from the adjacent molecules. A better agreement is obtained when the nearest neighbors are also considered at full quantum mechanical (QM) level. The calculations suggest that the nearest solvent molecules must be included in the quantum mechanical system, at least when estimating solvent shifts at the molecular mechanics (MM) level. Current density calculations show that the stacking does not significantly affect the ring current strengths of the individual molecules, whereas the shape of the ring current for a single molecule differs from that of the stacked molecules.

  14. Phosphorus nuclear magnetic resonance in isolated perfused rat pancreas

    SciTech Connect

    Matsumoto, Takehisa; Kanno, Tomio; Seo, Yoshiteru; Murakami, Masataka; Watari, Hiroshi National Institute for Physiological Sciences, Okazaki )

    1988-04-01

    Phosphorus nuclear magnetic resonance spectroscopy was applied to measure phosphorus energy metabolites in isolated perfused rat pancreas. The gland was perfused with a modified Krebs-Henseleit solution at room temperature (25{degree}C). {sup 31}P resonances of creatine phosphate (PCr), ATP, ADP, inorganic phosphate (P{sub i}) and phosphomonoesters (PMEs) were observed in all the preparations of pancreas. In different individual preparations, the resonance of PCr varied, but those of ATP were almost the same. The initial levels of PCr and ATP in individual preparations, however, remained almost unchanged during perfusion with the standard solution for 2 h. When the perfusion was stopped, the levels of ATP and PCr decreased, while the levels of PME and P{sub i} increased. At that time, the P{sub i} resonance shfted to a higher magnetic field, indicating that the tissue pH decreased. On reperfusion, the tissue levels of phosphorus compounds and the tissue pH were restored to their initial resting levels. Continuous infusion of 0.1 {mu}M acetylcholine caused marked and sustained increases in the flow of pancreatic juice and protein output. During the stimulation the tissue levels of phosphorus compounds remained unchanged, while the tissue pH was decreased slightly.

  15. Nuclear magnetic resonance study of the crystallization kinetics in soft magnetic nanocrystalline materials

    NASA Astrophysics Data System (ADS)

    Barbatti, C. F.; Sinnecker, E. H. C. P.; Sarthour, R. S.; Guimarães, A. P.

    2002-05-01

    We used the nuclear magnetic resonance technique to study the evolution of the structural and magnetic properties of Fe-based melt-spun ribbons of Fe73.5Cu1Nb3Si13.5B9, Fe73.5Cu1Nb3Si18.5B4, and Fe86Zr7Cu1B6, as-cast and annealed at 500, 540, and 430 °C, respectively. Experiments were carried out at 4.2 K and zero-applied magnetic field, and in a controlled radio-frequency (rf) field. This type of measurement allows us to observe B and Nb sites, and makes it possible to distinguish signals associated with regions of different magnetic hardnesses. The results exhibit a high dependence of the spectra on rf power. For Fe-Si-based alloys, we observe well-defined 93Nb resonance signals from three distinct sites according to the concentration of Fe atoms in their neighborhood. In the Fe73.5Cu1Nb3Si18.5B4 spectra we also observe a peak around 34 MHz, connected to the 11B resonance in different Fe-B compounds, which remains as the rf power decreases, suggesting that the signals come from atoms inside a soft magnetic region. As for the Fe-Zr alloy, we also observe a peak around 36 MHz, identified as the 11B resonance, and a broad line around 62 MHz.

  16. Nuclear Magnetic Resonance Study of High Temperature Superconductivity

    NASA Astrophysics Data System (ADS)

    Mounce, Andrew M.

    The high temperature superconductors HgBa2CuO 4+delta (Hg1201) and Bi2SrCa2Cu2O 8+delta (Bi2212) have been treated with 17O for both nuclear magnetic resonance (NMR) sensitivity and various electronic properties. Subsequently, NMR experiments were performed on Hg1201 and Bi2212 to reveal the nature of the pseudogap, in the normal state, and vortex phases, in the superconducting state. NMR has been performed on 17O in an underdoped Hg1201 crystal with a superconducting transition transition temperature of 74 K to look for circulating orbital currents proposed theoretically and inferred from neutron scattering. The measurements reveal narrow spectra which preclude static local fields in the pseudogap phase at the apical site, suggesting that the moments observed with neutrons are fluctuating or the orbital current ordering is not the correct model for the neutron scattering observation. The fine detail of the NMR frequency shifts at the apical oxygen site are consistent with a dipolar field from the Cu+2 site and diamagnetism below the superconducting transition. It has been predicted that superconducting vortices should be electrically charged and that this effect is particularly enhanced for high temperature superconductors. Here it is shown that the Abrikosov vortex lattice, characteristic of the mixed state of superconductors, will become unstable at sufficiently high magnetic field if there is charge trapped on the vortex core for highly anisotropic superconductors. NMR measurements of the magnetic fields generated by vortices in Bi2212 single crystals provide evidence for an electro-statically driven vortex lattice reconstruction with the magnitude of charge on each vortex pancake of 2x10-3e, depending on doping, in line with theoretical estimates. Competition with magnetism is at the heart of high temperature superconductivity, most intensely felt near a vortex core. To investigate vortex magnetism spatially resolved NMR has been used, finding a strongly non

  17. High temperature spin dynamics in linear magnetic chains, molecular rings, and segments by nuclear magnetic resonance

    SciTech Connect

    Adelnia, Fatemeh; Lascialfari, Alessandro; Mariani, Manuel; Ammannato, Luca; Caneschi, Andrea; Rovai, Donella; Winpenny, Richard; Timco, Grigore; Corti, Maurizio Borsa, Ferdinando

    2015-05-07

    We present the room temperature proton nuclear magnetic resonance (NMR) nuclear spin-lattice relaxation rate (NSLR) results in two 1D spin chains: the Heisenberg antiferromagnetic (AFM) Eu(hfac){sub 3}NITEt and the magnetically frustrated Gd(hfac){sub 3}NITEt. The NSLR as a function of external magnetic field can be interpreted very well in terms of high temperature spin dynamics dominated by a long time persistence of the decay of the two-spin correlation function due to the conservation of the total spin value for isotropic Heisenberg chains. The high temperature spin dynamics are also investigated in Heisenberg AFM molecular rings. In both Cr{sub 8} closed ring and in Cr{sub 7}Cd and Cr{sub 8}Zn open rings, i.e., model systems for a finite spin segment, an enhancement of the low frequency spectral density is found consistent with spin diffusion but the high cut-off frequency due to intermolecular anisotropic interactions prevents a detailed analysis of the spin diffusion regime.

  18. Rotatable Small Permanent Magnet Array for Ultra-Low Field Nuclear Magnetic Resonance Instrumentation: A Concept Study

    PubMed Central

    Vegh, Viktor; Reutens, David C.

    2016-01-01

    Object We studied the feasibility of generating the variable magnetic fields required for ultra-low field nuclear magnetic resonance relaxometry with dynamically adjustable permanent magnets. Our motivation was to substitute traditional electromagnets by distributed permanent magnets, increasing system portability. Materials and Methods The finite element method (COMSOL®) was employed for the numerical study of a small permanent magnet array to calculate achievable magnetic field strength, homogeneity, switching time and magnetic forces. A manually operated prototype was simulated and constructed to validate the numerical approach and to verify the generated magnetic field. Results A concentric small permanent magnet array can be used to generate strong sample pre-polarisation and variable measurement fields for ultra-low field relaxometry via simple prescribed magnet rotations. Using the array, it is possible to achieve a pre-polarisation field strength above 100 mT and variable measurement fields ranging from 20–50 μT with 200 ppm absolute field homogeneity within a field-of-view of 5 x 5 x 5 cubic centimetres. Conclusions A dynamic small permanent magnet array can generate multiple highly homogeneous magnetic fields required in ultra-low field nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) instruments. This design can significantly reduce the volume and energy requirements of traditional systems based on electromagnets, improving portability considerably. PMID:27271886

  19. Rotatable Small Permanent Magnet Array for Ultra-Low Field Nuclear Magnetic Resonance Instrumentation: A Concept Study.

    PubMed

    Vogel, Michael W; Giorni, Andrea; Vegh, Viktor; Pellicer-Guridi, Ruben; Reutens, David C

    2016-01-01

    We studied the feasibility of generating the variable magnetic fields required for ultra-low field nuclear magnetic resonance relaxometry with dynamically adjustable permanent magnets. Our motivation was to substitute traditional electromagnets by distributed permanent magnets, increasing system portability. The finite element method (COMSOL®) was employed for the numerical study of a small permanent magnet array to calculate achievable magnetic field strength, homogeneity, switching time and magnetic forces. A manually operated prototype was simulated and constructed to validate the numerical approach and to verify the generated magnetic field. A concentric small permanent magnet array can be used to generate strong sample pre-polarisation and variable measurement fields for ultra-low field relaxometry via simple prescribed magnet rotations. Using the array, it is possible to achieve a pre-polarisation field strength above 100 mT and variable measurement fields ranging from 20-50 μT with 200 ppm absolute field homogeneity within a field-of-view of 5 x 5 x 5 cubic centimetres. A dynamic small permanent magnet array can generate multiple highly homogeneous magnetic fields required in ultra-low field nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) instruments. This design can significantly reduce the volume and energy requirements of traditional systems based on electromagnets, improving portability considerably.

  20. Superconductivity and magnetic fluctuations in Cd(2))Re(2)O(7) via Cd nuclear magnetic resonance and re nuclear quadrupole resonance.

    PubMed

    Vyaselev, O; Arai, K; Kobayashi, K; Yamazaki, J; Kodama, K; Takigawa, M; Hanawa, M; Hiroi, Z

    2002-07-01

    We report Cd nuclear magnetic resonance (NMR) and Re nuclear quadrupole resonance (NQR) studies on Cd(2)Re(2)O(7), the first superconductor among pyrochlore oxides (T(c) approximately 1 K). The Re NQR spectrum at zero magnetic field below 100 K rules out any magnetic or charge order. The spin-lattice relaxation rate below T(c) exhibits a pronounced coherence peak and follows the weak-coupling BCS theory with nearly isotropic energy gap. The results of Cd NMR point to a moderate ferromagnetic enhancement at high temperatures followed by a rapid decrease of the density of states below the structural transition temperature of 200 K.

  1. Nuclear magnetic resonance dephasing effects in a spherical pore with a magnetic dipolar field

    NASA Astrophysics Data System (ADS)

    Valckenborg, R. M. E.; Huinink, H. P.; Kopinga, K.

    2003-02-01

    The NMR dephasing behavior of the nuclear spins of a fluid confined in a porous material can be investigated by Hahn spin echoes. Previous experimental results on water in a magnetically doped clay have shown a nonmonoexponentially decaying magnetization, which can be understood neither by the known dephasing rate of freely diffusing spins in a uniform gradient nor by spins diffusing in a restricted geometry. For a better understanding of NMR measurements on these systems, a systematic survey was performed of the various length scales that are involved. The standard length scales for the situation of a uniform gradient are diffusing length, structure length, and dephasing length. We show that for a nonuniform gradient, a new length scale has to be introduced: the magnetic-field curvature length. When a particle diffuses less than this length scale, it experiences a local uniform gradient. In that case the spin-echo decay can be described by the so-called local gradient approximation (LGA). When a particle diffuses over a longer distance than the structure length, the spin-echo decay can be described by the motional averaging regime. For both regimes, scaling laws are derived. In this paper, a random-walk model is used to simulate the dephasing effect of diffusing spins in a spherical pore in the presence of a magnetic dipole field. By varying the dipole magnitude, situations can be created in which the dephasing behavior scales according to the motional averaging regime or according to the LGA regime, for certain ranges of echo times. Two model systems are investigated: a spherical pore in the vicinity of a magnetic point dipole and a spherical pore adjacent to a magnetic dipolar grain of the same size as the pore. The simulated magnetization decay curves of both model systems confirm the scaling laws. The LGA, characterized by a nonmonoexponential magnetization decay, is also investigated by calculating the spatially resolved magnetization in the pore. For this

  2. 19F MAS-NMR studies of strontium oxyfluoride aluminosilicate glass

    NASA Astrophysics Data System (ADS)

    Środa, M.; Olejniczak, Z.

    2011-08-01

    Local environment of fluorine atoms in the lanthanum oxyfluoride aluminosilicate glasses and glass-ceramics modified by SrO was studied by solid state 19F MAS-NMR spectroscopy and X-ray diffraction. The effect of strontium concentration on the formation of crystalline LaF 3 phase was determined, as a function of heat treatment conditions. In all glasses studied, the F-Me( n) (where Me = Sr, La), but no Na-F species were observed. The presence of F-La,Sr( n) units, in which fluorine is coordinated by both lanthanum and strontium, was detected in the glass with higher content of SrO. Supplementary XRD analysis of this series confirmed that an increase of strontium contents leads to the formation of Sr 0.69La 0.31F 2.31 and LaSr 2F 7, instead of the pure LaF 3 only.

  3. 19F NMR measurements of the rotational mobility of proteins in vivo.

    PubMed Central

    Williams, S P; Haggie, P M; Brindle, K M

    1997-01-01

    Three glycolytic enzymes, hexokinase, phosphoglycerate kinase, and pyruvate kinase, were fluorine labeled in the yeast Saccharomyces cerevisiae by biosynthetic incorporation of 5-fluorotryptophan. 19F NMR longitudinal relaxation time measurements on the labeled enzymes were used to assess their rotational mobility in the intact cell. Comparison with the results obtained from relaxation time measurements of the purified enzymes in vitro and from theoretical calculations showed that two of the labeled enzymes, phosphoglycerate kinase and hexokinase, were tumbling in a cytoplasm that had a viscosity approximately twice that of water. There were no detectable signals from pyruvate kinase in vivo, although it could be detected in diluted cell extracts, indicating that there was some degree of motional restriction of the enzyme in the intact cell. PMID:8994636

  4. Tanks 18 And 19-F Structural Flowable Grout Fill Material Evaluation And Recommendations

    SciTech Connect

    Langton, C. A.; Stefanko, D. B.

    2013-04-23

    Cementitious grout will be used to close Tanks 18-F and 19-F. The functions of the grout are to: 1) physically stabilize the final landfill by filling the empty volume in the tanks with a non-compressible material; 2) provide a barrier for inadvertent intrusion into the tank; 3) reduce contaminant mobility by a) limiting the hydraulic conductivity of the closed tank and b) reducing contact between the residual waste and infiltrating water; and 4) providing an alkaline, chemically reducing environment in the closed tank to control speciation and solubility of selected radionuclides. The objective of this work was to identify a single (all-in-one) grout to stabilize and isolate the residual radionuclides in the tank, provide structural stability of the closed tank and serve as an inadvertent intruder barrier. This work was requested by V. A. Chander, High Level Waste (HLW) Tank Engineering, in HLW-TTR-2011-008. The complete task scope is provided in the Task Technical and QA Plan, SRNL-RP-2011-00587 Revision 0. The specific objectives of this task were to: 1) Identify new admixtures and dosages for formulating a zero bleed flowable tank fill material selected by HLW Tank Closure Project personnel based on earlier tank fill studies performed in 2007. The chemical admixtures used for adjusting the flow properties needed to be updated because the original admixture products are no longer available. Also, the sources of cement and fly ash have changed, and Portland cements currently available contain up to 5 wt. % limestone (calcium carbonate). 2) Prepare and evaluate the placement, compressive strength, and thermal properties of the selected formulation with new admixture dosages. 3) Identify opportunities for improving the mix selected by HLW Closure Project personnel and prepare and evaluate two potentially improved zero bleed flowable fill design concepts; one based on the reactor fill grout and the other based on a shrinkage compensating flowable fill mix design. 4

  5. Nuclear forward scattering of synchrotron radiation in pulsed high magnetic fields.

    PubMed

    Strohm, C; Van der Linden, P; Rüffer, R

    2010-02-26

    We report the demonstration of nuclear forward scattering of synchrotron radiation from 57Fe in ferromagnetic alpha iron in pulsed high magnetic fields up to 30 T. The observed magnetic hyperfine field follows the calculated high field bulk magnetization within 1%, establishing the technique as a precise tool for the study of magnetic solids in very high magnetic fields. To perform these experiments in pulsed fields, we have developed a detection scheme for fully time resolved nuclear forward scattering applicable to other pump probe experiments.

  6. Intracellular free calcium concentration measured with /sup 19/F NMR spectroscopy in intact ferret hearts

    SciTech Connect

    Marban, E.; Kitakaze, M.; Kusuoka, H.; Porterfield, J.K.; Yue, D.T.; Chacko, V.P.

    1987-08-01

    Changes in the intracellular free Ca/sup 2 +/ concentration, (Ca/sup 2 +/)/sub i/, mediate excitation-contraction coupling in the heart and contribute to cellular injury during ischemia and reperfusion. To study these processes directly, the authors measured (Ca/sup 2 +/)/sub i/ in perfused ferret (Mustela putorius furo) hearts using /sup 19/F NMR spectroscopy to detect the 5,5'-difluoro derivative of the Ca/sup 2 +/ chelator, 1,2-bis(o-aminophenoxy)ethane-N,N,N',N'-tetraacetic acid (BAPTA). To load cells, hearts were perfused with the acetoxymethyl ester derivative of 5,5'-F/sub 2/-BAPTA. They measured /sup 19/F NMR spectra and left ventricular pressure simultaneously,at rest and during pacing at various external Ca concentrations ((Ca)/sub 0/). Although contractile force was attenuated by the Ca/sup 2 +/ buffering properties of 5,5'-F/sup 2/-BAPTA, the decrease in pressure could be overcome by raising (Ca)/sub 0/. The mean value of 104 nM for (Ca/sup 2 +/)/sub i/ at rest in the perfused heart agrees well with previous measurements in isolated ventricular muscle. During pacing at 0.6-4 Hz, time-averaged (Ca/sup 2 +/)/sub i/ increased; the effect of pacing was augmented by increasing (Ca)/sub 0/. (Ca/sup 2 +/)/sub i/ more than tripled during 10-20 min of global ischemia, and returned toward control levels upon reperfusion. This approach promises to be particularly useful in investigating the physiology of intact hearts and the pathophysiology of alterations in the coronary circulation

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

    SciTech Connect

    Keating, Kristina; Slater, Lee; Ntarlagiannis, Dimitris; Williams, Kenneth H.

    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

  8. Partial homogeneity based high-resolution nuclear magnetic resonance spectra under inhomogeneous magnetic fields

    SciTech Connect

    Wei, Zhiliang; Lin, Liangjie; Lin, Yanqin E-mail: chenz@xmu.edu.cn; Chen, Zhong E-mail: chenz@xmu.edu.cn; Chen, Youhe

    2014-09-29

    In nuclear magnetic resonance (NMR) technique, it is of great necessity and importance to obtain high-resolution spectra, especially under inhomogeneous magnetic fields. In this study, a method based on partial homogeneity is proposed for retrieving high-resolution one-dimensional NMR spectra under inhomogeneous fields. Signals from series of small voxels, which characterize high resolution due to small sizes, are recorded simultaneously. Then, an inhomogeneity correction algorithm is developed based on pattern recognition to correct the influence brought by field inhomogeneity automatically, thus yielding high-resolution information. Experiments on chemical solutions and fish spawn were carried out to demonstrate the performance of the proposed method. The proposed method serves as a single radiofrequency pulse high-resolution NMR spectroscopy under inhomogeneous fields and may provide an alternative of obtaining high-resolution spectra of in vivo living systems or chemical-reaction systems, where performances of conventional techniques are usually degenerated by field inhomogeneity.

  9. Nuclear spin conversion of water inside fullerene cages detected by low-temperature nuclear magnetic resonance

    SciTech Connect

    Mamone, Salvatore Concistrè, Maria; Carignani, Elisa; Meier, Benno; Krachmalnicoff, Andrea; Johannessen, Ole G.; Denning, Mark; Carravetta, Marina; Whitby, Richard J.; Levitt, Malcolm H.; Lei, Xuegong; Li, Yongjun; Goh, Kelvin; Horsewill, Anthony J.

    2014-05-21

    The water-endofullerene H{sub 2}O@C{sub 60} provides a unique chemical system in which freely rotating water molecules are confined inside homogeneous and symmetrical carbon cages. The spin conversion between the ortho and para species of the endohedral H{sub 2}O was studied in the solid phase by low-temperature nuclear magnetic resonance. The experimental data are consistent with a second-order kinetics, indicating a bimolecular spin conversion process. Numerical simulations suggest the simultaneous presence of a spin diffusion process allowing neighbouring ortho and para molecules to exchange their angular momenta. Cross-polarization experiments found no evidence that the spin conversion of the endohedral H{sub 2}O molecules is catalysed by {sup 13}C nuclei present in the cages.

  10. Nuclear spin conversion of water inside fullerene cages detected by low-temperature nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Mamone, Salvatore; Concistrè, Maria; Carignani, Elisa; Meier, Benno; Krachmalnicoff, Andrea; Johannessen, Ole G.; Lei, Xuegong; Li, Yongjun; Denning, Mark; Carravetta, Marina; Goh, Kelvin; Horsewill, Anthony J.; Whitby, Richard J.; Levitt, Malcolm H.

    2014-05-01

    The water-endofullerene H2O@C60 provides a unique chemical system in which freely rotating water molecules are confined inside homogeneous and symmetrical carbon cages. The spin conversion between the ortho and para species of the endohedral H2O was studied in the solid phase by low-temperature nuclear magnetic resonance. The experimental data are consistent with a second-order kinetics, indicating a bimolecular spin conversion process. Numerical simulations suggest the simultaneous presence of a spin diffusion process allowing neighbouring ortho and para molecules to exchange their angular momenta. Cross-polarization experiments found no evidence that the spin conversion of the endohedral H2O molecules is catalysed by 13C nuclei present in the cages.

  11. Towards a beyond 1 GHz solid-state nuclear magnetic resonance: External lock operation in an external current mode for a 500 MHz nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Takahashi, Masato; Ebisawa, Yusuke; Tennmei, Konosuke; Yanagisawa, Yoshinori; Hosono, Masami; Takasugi, Kenji; Hase, Takashi; Miyazaki, Takayoshi; Fujito, Teruaki; Nakagome, Hideki; Kiyoshi, Tsukasa; Yamazaki, Toshio; Maeda, Hideaki

    2012-10-01

    Achieving a higher magnetic field is important for solid-state nuclear magnetic resonance (NMR). But a conventional low temperature superconducting (LTS) magnet cannot exceed 1 GHz (23.5 T) due to the critical magnetic field. Thus, we started a project to replace the Nb3Sn innermost coil of an existing 920 MHz NMR (21.6 T) with a Bi-2223 high temperature superconducting (HTS) innermost coil. Unfortunately, the HTS magnet cannot be operated in persistent current mode; an external dc power supply is required to operate the NMR magnet, causing magnetic field fluctuations. These fluctuations can be stabilized by a field-frequency lock system based on an external NMR detection coil. We demonstrate here such a field-frequency lock system in a 500 MHz LTS NMR magnet operated in an external current mode. The system uses a 7Li sample in a microcoil as external NMR detection system. The required field compensation is calculated from the frequency of the FID as measured with a frequency counter. The system detects the FID signal, determining the FID frequency, and calculates the required compensation coil current to stabilize the sample magnetic field. The magnetic field was stabilized at 0.05 ppm/3 h for magnetic field fluctuations of around 10 ppm. This method is especially effective for a magnet with large magnetic field fluctuations. The magnetic field of the compensation coil is relatively inhomogeneous in these cases and the inhomogeneity of the compensation coil can be taken into account.

  12. Study of natural diamonds by dynamic nuclear polarization-enhanced 13C nuclear magnetic resonance spectroscopy.

    PubMed

    Zhou, J; Li, L; Hu, H; Yang, B; Dan, Z; Qiu, J; Guo, J; Chen, F; Ye, C

    1994-11-01

    The results of a study of two types of natural-diamond crystals by dynamic nuclear polarization (DNP)-enhanced high-resolution solid-state 13C nuclear magnetic resonance (NMR) are reported. The home-built DNP magic-angle spinning (MAS) 13C NMR spectrometer operates at 54 GHz for electrons and 20.2 MHz for carbons. The power of the microwave source was about 30 W and the highest DNP enhancement factor came near to 10(3). It was shown that in the MAS spectra the 13C NMR linewidths of the Ib-type diamond were broader than those of IaB3-type diamond. From the hyperfine structure of the DNP enhancement as a function of frequency, four kinds of nitrogen-centred and one kind of carbon-centred free radicals could be identified in the Ib-type diamond. The hyperfine structures of the DNP enhancement curve that originated from the anisotropic hyperfine interaction between electron and nuclei could be partially averaged out by MAS. The 13C polarization time of DNP was rather long, i.e. 1500 s, and the spin-lattice relaxation time (without microwave irradiation) was about 300 s, which was somewhat shorter than anticipated. Discussions on these experimental results have been made in this report.

  13. Nuclear magnetic resonance experiments with dc SQUID amplifiers

    SciTech Connect

    Heaney, M.B. . Dept. of Physics Lawrence Berkeley Lab., CA )

    1990-11-01

    The development and fabrication of dc SQUIDs (Superconducting QUantum Interference Devices) with Nb/Al{sub 2}O{sub 3}/Nb Josephson junctions is described. A theory of the dc SQUID as a radio-frequency amplifier is presented, with an optimization strategy that accounts for the loading and noise contributions of the postamplifier and maximizes the signal-to-noise ratio of the total system. The high sensitivity of the dc SQUID is extended to high field NMR. A dc SQUID is used as a tuned radio-frequency amplifier to detect pulsed nuclear magnetic resonance at 32 MHz from a metal film in a 3.5 Tesla static field. A total system noise temperature of 11 K has been achieved, at a bath temperature of 4.2 K. The minimum number of nuclear Bohr magnetons observable from a free precession signal after a single pulse is about 2 {times} 10{sup 17} in a bandwidth of 25 kHz. In a separate experiment, a dc SQUID is used as a rf amplifier in a NQR experiment to observe a new resonance response mechanism. The net electric polarization of a NaClO{sub 3} crystal due to the precessing electric quadrupole moments of the Cl nuclei is detected at 30 MHz. The sensitivity of NMR and NQR spectrometers using dc SQUID amplifiers is compared to the sensitivity of spectrometers using conventional rf amplifiers. A SQUID-based spectrometer has a voltage sensitivity which is comparable to the best achieved by a FET-based spectrometer, at these temperatures and operating frequencies.

  14. /sup 13/C nuclear magnetic resonance studies of cardiac metabolism

    SciTech Connect

    Seeholzer, S.H.

    1985-01-01

    The last decade has witnessed the increasing use of Nuclear Magnetic Resonance (NMR) techniques for following the metabolic fate of compounds specifically labeled with /sup 13/C. The goals of the present study are: (1) to develop reliable quantitative procedures for measuring the /sup 13/C enrichment of specific carbon sites in compounds enriched by the metabolism of /sup 13/C-labeled substrates in rat heart, and (2) to use these quantitative measurements of fractional /sup 13/C enrichment within the context of a mathematical flux model describing the carbon flow through the TCA cycle and ancillary pathways, as a means for obtaining unknown flux parameters. Rat hearts have been perfused in vitro with various combinations of glucose, acetate, pyruvate, and propionate to achieve steady state flux conditions, followed by perfusion with the same substrates labeled with /sup 13/C in specific carbon sites. The hearts were frozen at different times after addition of /sup 13/C-labeled substrates and neutralized perchloric acid extracts were used to obtain high resolution proton-decoupled /sup 13/C NMR spectra at 90.55 MHz. The fractional /sup 13/C enrichment (F.E.) of individual carbon sites in different metabolites was calculated from the area of the resolved resonances after correction for saturation and nuclear Overhauser effects. These F.E. measurements by /sup 13/C NMR were validated by the analysis of /sup 13/C-/sup 1/H scalar coupling patterns observed in /sup 1/H NMR spectra of the extracted metabolites. The results obtained from perfusion of hearts glucose plus either (2-/sup 13/C) acetate or (3-/sup 13/C) pyruvate are similar to those obtained by previous investigators using /sup 14/C-labeled substrates.

  15. Nonequilibrium nuclear polarization and induced hyperfine and dipolar magnetic fields in semiconductor nanostructures

    NASA Astrophysics Data System (ADS)

    Ţifrea, Ionel; Flatté, Michael E.

    2011-10-01

    We investigate the dynamic nuclear polarization (DNP) caused by hyperfine coupling between nonequilibrium electronic spins and nuclear spins in semiconductor nanostructures. We derive the time and position dependence of the resulting hyperfine and dipolar magnetic fields. In GaAs quantum wells the induced nuclear spin polarization greatly exceeds the polarization of the electronic system that causes the DNP. The induced magnetic fields vary between tens of tesla for the electronic hyperfine field acting on nuclei, to hundreds of gauss for the nuclear hyperfine field acting on electrons, to a few gauss for the induced nuclear dipolar fields that act on both nuclei and electrons. The field strengths should be measurable via optically induced nuclear magnetic resonance or time-resolved Faraday rotation experiments. We discuss the implications of our calculations for low-dimensional semiconductor nanostructures.

  16. Nuclear composition of magnetized gamma-ray burst jets

    NASA Astrophysics Data System (ADS)

    Shibata, Sanshiro; Tominaga, Nozomu

    2015-06-01

    We investigate the fraction of metal nuclei in the relativistic jets of gamma-ray bursts associated with core-collapse supernovae. We simulate the fallback in jet-induced explosions with two-dimensional relativistic hydrodynamics calculations and the jet acceleration with steady, radial, relativistic magnetohydrodynamics calculations, and derive the detailed nuclear composition of the jet by post-processing calculation. We found that if the temperature at the jet launch site is above 4.7 × 109 K, quasi-statistical equilibrium is established and heavy nuclei are dissociated into light particles such as 4He during the acceleration of the jets. The criterion for the survival of metal nuclei is written in terms of the isotropic jet luminosity as L_j^iso ≲ 3.9 × 10^{50} ( R_i/107 cm)^2(1 + σi) erg s-1, where Ri and σi are the initial radius of the jets and the initial magnetization parameter, respectively. If the jet is initially dominated by radiation field (i.e., σi ≪ 1) and the isotropic luminosity is relatively high (L_j^iso ≳ 4 × 10^{52} erg s-1), the metal nuclei cannot survive in the jet. On the other hand, if the jet is mainly accelerated by magnetic field (i.e., σi ≫ 1), metal nuclei initially contained in the jet can survive without serious dissociation even in the case of a high-luminosity jet. If the jet contains metal nuclei, the dominant nuclei are 28Si, 16O, and 32S and the mean mass number can be ˜ 25.

  17. Advances in Nuclear Magnetic Resonance for Drug Discovery

    PubMed Central

    Powers, Robert

    2010-01-01

    Background Drug discovery is a complex and unpredictable endeavor with a high failure rate. Current trends in the pharmaceutical industry have exasperated these challenges and are contributing to the dramatic decline in productivity observed over the last decade. The industrialization of science by forcing the drug discovery process to adhere to assembly-line protocols is imposing unnecessary restrictions, such as short project time-lines. Recent advances in nuclear magnetic resonance are responding to these self-imposed limitations and are providing opportunities to increase the success rate of drug discovery. Objective/Method A review of recent advancements in NMR technology that have the potential of significantly impacting and benefiting the drug discovery process will be presented. These include fast NMR data collection protocols and high-throughput protein structure determination, rapid protein-ligand co-structure determination, lead discovery using fragment-based NMR affinity screens, NMR metabolomics to monitor in vivo efficacy and toxicity for lead compounds, and the identification of new therapeutic targets through the functional annotation of proteins by FAST-NMR. Conclusion NMR is a critical component of the drug discovery process, where the versatility of the technique enables it to continually expand and evolve its role. NMR is expected to maintain this growth over the next decade with advancements in automation, speed of structure calculation, in-cell imaging techniques, and the expansion of NMR amenable targets. PMID:20333269

  18. Updated methodology for nuclear magnetic resonance characterization of shales

    USGS Publications Warehouse

    Washburn, Kathryn E.; Birdwell, Justin E.

    2013-01-01

    Unconventional petroleum resources, particularly in shales, are expected to play an increasingly important role in the world’s energy portfolio in the coming years. Nuclear magnetic resonance (NMR), particularly at low-field, provides important information in the evaluation of shale resources. Most of the low-field NMR analyses performed on shale samples rely heavily on standard T1 and T2 measurements. We present a new approach using solid echoes in the measurement of T1 and T1–T2 correlations that addresses some of the challenges encountered when making NMR measurements on shale samples compared to conventional reservoir rocks. Combining these techniques with standard T1 and T2 measurements provides a more complete assessment of the hydrogen-bearing constituents (e.g., bitumen, kerogen, clay-bound water) in shale samples. These methods are applied to immature and pyrolyzed oil shale samples to examine the solid and highly viscous organic phases present during the petroleum generation process. The solid echo measurements produce additional signal in the oil shale samples compared to the standard methodologies, indicating the presence of components undergoing homonuclear dipolar coupling. The results presented here include the first low-field NMR measurements performed on kerogen as well as detailed NMR analysis of highly viscous thermally generated bitumen present in pyrolyzed oil shale.

  19. Water Permeability of Chlorella Cell Membranes by Nuclear Magnetic Resonance

    PubMed Central

    Stout, Darryl G.; Steponkus, Peter L.; Bustard, Larry D.; Cotts, Robert M.

    1978-01-01

    Measurement by two nuclear magnetic resonance (NMR) techniques of the mean residence time τa of water molecules inside Chlorella vulgaris (Beijerinck) var. “viridis” (Chodot) is reported. The first is the Conlon and Outhred (1972 Biochim Biophys Acta 288: 354-361) technique in which extracellular water is doped with paramagnetic Mn2+ ions. Some complications in application of this technique are identified as being caused by the affinity of Chlorella cell walls for Mn2+ ions which shortens the NMR relaxation times of intra- and extracellular water. The second is based upon observations of effects of diffusion on the spin echo of intra- and extracellular water. Echo attenuation of intracellular water is distinguished from that of extracellular water by the extent to which diffusive motion is restricted. Intracellular water, being restricted to the cell volume, suffers less echo attenuation. From the dependence of echo amplitude upon gradient strength at several values of echo time, the mean residence time of intracellular water can be determined. From the mean residence time of intracellular water, the diffusional water permeability coefficient of the Chlorella membrane is calculated to be 2.1 ± 0.4 × 10−3 cm sec−1. PMID:16660456

  20. Updated methodology for nuclear magnetic resonance characterization of shales

    NASA Astrophysics Data System (ADS)

    Washburn, Kathryn E.; Birdwell, Justin E.

    2013-08-01

    Unconventional petroleum resources, particularly in shales, are expected to play an increasingly important role in the world's energy portfolio in the coming years. Nuclear magnetic resonance (NMR), particularly at low-field, provides important information in the evaluation of shale resources. Most of the low-field NMR analyses performed on shale samples rely heavily on standard T1 and T2 measurements. We present a new approach using solid echoes in the measurement of T1 and T1-T2 correlations that addresses some of the challenges encountered when making NMR measurements on shale samples compared to conventional reservoir rocks. Combining these techniques with standard T1 and T2 measurements provides a more complete assessment of the hydrogen-bearing constituents (e.g., bitumen, kerogen, clay-bound water) in shale samples. These methods are applied to immature and pyrolyzed oil shale samples to examine the solid and highly viscous organic phases present during the petroleum generation process. The solid echo measurements produce additional signal in the oil shale samples compared to the standard methodologies, indicating the presence of components undergoing homonuclear dipolar coupling. The results presented here include the first low-field NMR measurements performed on kerogen as well as detailed NMR analysis of highly viscous thermally generated bitumen present in pyrolyzed oil shale.

  1. Distinguishing Carbonate Reservoir Pore Facies with Nuclear Magnetic Resonance Measurements

    SciTech Connect

    Genty, Coralie; Jensen, Jerry L. Ahr, Wayne M.

    2007-03-15

    Characterization of carbonate rocks may involve identifying the important pore types which are present. In the past, this task has required detailed petrographic analysis of many core samples. Here, we describe a method which uses nuclear magnetic resonance (NMR) measurements to reduce the amount of petrographic analysis needed for porosity typing of carbonate reservoir rocks.For a rock sample which has been measured with NMR, our method decomposes the log(T{sub 2}) spectrum into at most three Gaussian-shaped components and gives a set of nine parameters. Two characteristic quantities having geological significance are extracted from the nine parameters. Values of the two quantities are compared with a reference set, established from samples having both NMR and petrographic evaluations of porosity types. We use a Bayesian approach to the classification of the dominant porosity type.Tests of our method on 103 samples show a correct prediction in 60 to 90 percent of the samples. The lower success rate was obtained for samples with five porosity types from three fields; the higher success rate obtained with samples with three porosity types from one well. The use of geologically significant quantities extracted from the decomposition gives comparable success rate to those obtained using a standard, non-geological approach such as canonical variates.

  2. Discrete decoding based ultrafast multidimensional nuclear magnetic resonance spectroscopy

    SciTech Connect

    Wei, Zhiliang; Lin, Liangjie; Ye, Qimiao; Li, Jing; Cai, Shuhui; Chen, Zhong

    2015-07-14

    The three-dimensional (3D) nuclear magnetic resonance (NMR) spectroscopy constitutes an important and powerful tool in analyzing chemical and biological systems. However, the abundant 3D information arrives at the expense of long acquisition times lasting hours or even days. Therefore, there has been a continuous interest in developing techniques to accelerate recordings of 3D NMR spectra, among which the ultrafast spatiotemporal encoding technique supplies impressive acquisition speed by compressing a multidimensional spectrum in a single scan. However, it tends to suffer from tradeoffs among spectral widths in different dimensions, which deteriorates in cases of NMR spectroscopy with more dimensions. In this study, the discrete decoding is proposed to liberate the ultrafast technique from tradeoffs among spectral widths in different dimensions by focusing decoding on signal-bearing sites. For verifying its feasibility and effectiveness, we utilized the method to generate two different types of 3D spectra. The proposed method is also applicable to cases with more than three dimensions, which, based on the experimental results, may widen applications of the ultrafast technique.

  3. Nuclear Magnetic Resonance Spectroscopy-Based Identification of Yeast.

    PubMed

    Himmelreich, Uwe; Sorrell, Tania C; Daniel, Heide-Marie

    2017-01-01

    Rapid and robust high-throughput identification of environmental, industrial, or clinical yeast isolates is important whenever relatively large numbers of samples need to be processed in a cost-efficient way. Nuclear magnetic resonance (NMR) spectroscopy generates complex data based on metabolite profiles, chemical composition and possibly on medium consumption, which can not only be used for the assessment of metabolic pathways but also for accurate identification of yeast down to the subspecies level. Initial results on NMR based yeast identification where comparable with conventional and DNA-based identification. Potential advantages of NMR spectroscopy in mycological laboratories include not only accurate identification but also the potential of automated sample delivery, automated analysis using computer-based methods, rapid turnaround time, high throughput, and low running costs.We describe here the sample preparation, data acquisition and analysis for NMR-based yeast identification. In addition, a roadmap for the development of classification strategies is given that will result in the acquisition of a database and analysis algorithms for yeast identification in different environments.

  4. Two-dimensional nuclear magnetic resonance of quadrupolar systems

    SciTech Connect

    Wang, Shuanhu

    1997-09-01

    This dissertation describes two-dimensional nuclear magnetic resonance theory and experiments which have been developed to study quadruples in the solid state. The technique of multiple-quantum magic-angle spinning (MQMAS) is extensively reviewed and expanded upon in this thesis. Specifically, MQMAS is first compared with another technique, dynamic-angle spinning (DAS). The similarity between the two techniques allows us to extend much of the DAS work to the MQMAS case. Application of MQMAS to a series of aluminum containing materials is then presented. The superior resolution enhancement through MQMAS is exploited to detect the five- and six-coordinated aluminum in many aluminosilicate glasses. Combining the MQMAS method with other experiments, such as HETCOR, greatly expands the possibility of the use of MQMAS to study a large range of problems and is demonstrated in Chapter 5. Finally, the technique switching-angle spinning (SAS) is applied to quadrupolar nuclei to fully characterize a quadrupolar spin system in which all of the 8 NMR parameters are accurately determined. This dissertation is meant to demonstrate that with the combination of two-dimensional NMR concepts and new advanced spinning technologies, a series of multiple-dimensional NMR techniques can be designed to allow a detailed study of quadrupolar nuclei in the solid state.

  5. Nuclear magnetic resonance studies of bovine γB-crystallin

    NASA Astrophysics Data System (ADS)

    Thurston, George; Mills, Jeffrey; Michel, Lea; Mathews, Kaylee; Zanet, John; Payan, Angel; van Nostrand, Keith; Kotlarchyk, Michael; Ross, David; Wahle, Christopher; Hamilton, John

    Anisotropy of shape and/or interactions play an important role in determining the properties of concentrated solutions of the eye lens protein, γB-crystallin, including its liquid-liquid phase transition. We are studying γB anisotropic interactions with use of nuclear magnetic resonance (NMR) concentration- and temperature-dependent chemical shift perturbations (CSPs). We analyze two-dimensional heteronuclear spin quantum coherence (HSQC) spectra on backbone nitrogen and attached hydrogen nuclei for CSPs, up to 3 percent volume fraction. Cumulative distribution functions of the CSPs show a concentration and temperature-dependent spread. Many peaks that are highly shifted with either concentration or temperature are close (i) crystal intermolecular contacts (ii) locations of cataractogenic point mutations of a homologous human protein, human γD-crystallin, and (iii) charged amino-acid residues. We also discuss the concentration- and temperature-dependence of NMR and quasielastic light scattering measurements of rotational and translational diffusion of γB crystallin in solution, affected by interprotein attractions. Supported by NIH EY018249.

  6. Nuclear magnetic resonance proton imaging of bone pathology

    SciTech Connect

    Atlan, H.; Sigal, R.; Hadar, H.; Chisin, R.; Cohen, I.; Lanir, A.; Soudry, M.; Machtey, Y.; Schreiber, R.; Benmair, J.

    1986-02-01

    Thirty-two patients with diversified pathology were examined with a supraconductive NMR imager using spin echo with different TR and TE to obtain T1 and T2 weighted images. They included 20 tumors (12 primary, eight metastasis), six osteomyelitis, three fractures, two osteonecrosis, and one diffuse metabolic (Gaucher) disease. In all cases except for the stress fractures, the bone pathology was clearly visualized in spite of the normal lack of signal from the compact cortical bone. Nuclear magnetic resonance (NMR) imaging proved to be at least as sensitive as radionuclide scintigraphy but much more accurate than all other imaging procedures including computed tomography (CT) and angiography to assess the extension of the lesions, especially in tumors extended to soft tissue. This is due both to easy acquisition of sagittal and coronal sections and to different patterns of pathologic modifications of T1 and T2 which are beginning to be defined. It is hoped that more experience in clinical use of these patterns will help to discriminate between tumor extension and soft-tissue edema. We conclude that while radionuclide scintigraphy will probably remain the most sensitive and easy to perform screening test for bone pathology, NMR imaging, among noninvasive diagnostic procedures, appears to be at least as specific as CT. In addition, where the extension of the lesions is concerned, NMR imaging is much more informative than CT. In pathology of the spine, the easy visualization of the spinal cord should decrease the need for myelography.

  7. Nuclear magnetic resonance metabolomics of iron deficiency in soybean leaves.

    PubMed

    Lima, Marta R M; Diaz, Sílvia O; Lamego, Inês; Grusak, Michael A; Vasconcelos, Marta W; Gil, Ana M

    2014-06-06

    Iron (Fe) deficiency is an important agricultural concern that leads to lower yields and crop quality. A better understanding of the condition at the metabolome level could contribute to the design of strategies to ameliorate Fe-deficiency problems. Fe-sufficient and Fe-deficient soybean leaf extracts and whole leaves were analyzed by liquid (1)H nuclear magnetic resonance (NMR) and high-resolution magic-angle spinning NMR spectroscopy, respectively. Overall, 30 compounds were measurable and identifiable (comprising amino and organic acids, fatty acids, carbohydrates, alcohols, polyphenols, and others), along with 22 additional spin systems (still unassigned). Thus, metabolite differences between treatment conditions could be evaluated for different compound families simultaneously. Statistically relevant metabolite changes upon Fe deficiency included higher levels of alanine, asparagine/aspartate, threonine, valine, GABA, acetate, choline, ethanolamine, hypoxanthine, trigonelline, and polyphenols and lower levels of citrate, malate, ethanol, methanol, chlorogenate, and 3-methyl-2-oxovalerate. The data indicate that the main metabolic impacts of Fe deficiency in soybean include enhanced tricarboxylic acid cycle activity, enhanced activation of oxidative stress protection mechanisms and enhanced amino acid accumulation. Metabolites showing accumulation differences in Fe-starved but visually asymptomatic leaves could serve as biomarkers for early detection of Fe-deficiency stress.

  8. Nuclear magnetic resonance imaging of water content in the subsurface

    SciTech Connect

    J. Hendricks; T. Yao; A. Kearns

    1999-01-21

    Previous theoretical and experimental studies indicated that surface nuclear magnetic resonance (NMR) has the potential to provide cost-effective water content measurements in the subsurface and is a technology ripe for exploitation in practice. The objectives of this investigation are (a) to test the technique under a wide range of hydrogeological conditions and (b) to generalize existing NMR theories in order to correctly model NMR response from conductive ground and to assess properties of the inverse problem. Twenty-four sites with different hydrogeologic settings were selected in New Mexico and Colorado for testing. The greatest limitation of surface NMR technology appears to be the lack of understanding in which manner the NMR signal is influenced by soil-water factors such as pore size distribution, surface-to-volume ratio, paramagnetic ions dissolved in the ground water, and the presence of ferromagnetic minerals. Although the theoretical basis is found to be sound, several advances need to be made to make surface NMR a viable technology for hydrological investigations. There is a research need to investigate, under controlled laboratory conditions, how the complex factors of soil-water systems affect NMR relaxation times.

  9. Work in progress: nuclear magnetic resonance imaging of the gallbladder

    SciTech Connect

    Hricak, H.; Filly, R.A.; Margulis, A.R.; Moon, K.L.; Crooks, L.E.; Kaufman, L.

    1983-05-01

    A preliminary study of the relation between food intake and intensity of gallbladder bile on nuclear magnetic resonance (NMR) images was made. Twelve subjects (seven volunteers, five patients) were imaged following a minimum of 14 hours of fasting. Six of seven volunteers were reimaged one hour after stimulation by either a fatty meal or an alcoholic beverage. An additional seven patients were imaged two hours after a hospital breakfast. It was found that concentrated bile emits a high-intensity spin echo signal (SE), while hepatic bile in the gallbladder produces a low-intensity SE signal. Following ingestion of cholecystogogue, dilute hepatic bile settles on top of the concentrated bile, each emitting SE signals of different intensity. The average T1 value of concentrated bile was 594 msec, while the T1 vaue of dilute hepatic bile was 2,646 msec. The average T2 values were 104 msec for concentrated bile and 126 msec for dilute bile. The most likely cause for the different SE intensities of bile is the higher water content, and therefore longer T1 or T2 relaxation times, of hepatic bile. It is suggested that NMR imaging has the ability to provide physiological information about the gallbladder and that it may prove to be a simple and safe clinical test of gallbladder function.

  10. Proton nuclear magnetic resonance studies on brain edema

    SciTech Connect

    Naruse, S.; Horikawa, Y.; Tanaka, C.; Hirakawa, K.; Nishikawa, H.; Yoshizaki, K.

    1982-06-01

    The water in normal and edematous brain tissues of rats was studied by the pulse nuclear magnetic resonance (NMR) technique, measuring the longitudinal relaxation time (T1) and the transverse relaxation time (T2). In the normal brain, T1 and T2 were single components, both shorter than in pure water. Prolongation and separation of T2 into two components, one fast and one slow, were the characteristic findings in brain edema induced by both cold injury and triethyl tin (TET), although some differences between the two types of edema existed in the content of the lesion and in the degree of changes in T1 and T2 values. Quantitative analysis of T1 and T2 values in their time course relating to water content demonstrated that prolongation of T1 referred to the volume of increased water in tissues examined, and that two phases of T2 reflected the distribution and the content of the edema fluid. From the analysis of the slow component of T2 versus water content during edema formation, it was demonstrated that the increase in edema fluid was steady, and its content was constant during formation of TET-induced edema. On the contrary, during the formation of cold-injury edema, water-rich edema fluid increased during the initial few hours, and protein-rich edema fluid increased thereafter. It was concluded that proton NMR relaxation time measurements may provide new understanding in the field of brain edema research.

  11. Nuclear magnetic resonance imaging of the kidney: renal masses

    SciTech Connect

    Hricak, H.; Williams, R.D.; Moon, K.L. Jr.; Moss, A.A.; Alpers, C.; Crooks, L.E.; Kaufman, L.

    1983-06-01

    Fifteen patients with a variety of renal masses were examined by nuclear magnetic resonance (NMR), computed tomography, ultrasound, and intravenous urography. NMR clearly differentiated between simple renal cysts and other renal masses. On spin echo images, the simple renal cyst appeared as a round or slightly oval, homogeneous low-intensity mass with characteristically long T1 and T2 values. The thickness of the cyst wall was not measurable. The cyst had a smooth outer margin and a distict, sharp interface with normal parenchyma. Hemorrhagic cysts were seen as high-intensity lesions. Renal cell carcinomas displayed a wide range of intensity. The T1 and T2 values of the tumors were always different from those of the surrounding renal parenchyma. Tumor pseudocapsule was identified in four of five patients examined. All carcinomas were accurately staged by NMR and extension of the tumor thrombus into the inferior vena cava was demonstrated. The authors predict that if these preliminary results are confirmed by data from a larger number of patients, NMR will play a significant role in renal imaging.

  12. Monitoring iron mineralization processes using nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Keating, Kristina

    Proton nuclear magnetic resonance (NMR) measurements can be used to probe the molecular-scale physical and chemical environment of water in the pore space of geological materials. In geophysics, NMR relaxation measurements are used in to measure water content and estimate permeability in the top 100 m of Earth's surface. The goal of the research presented in this thesis is to determine if NMR can also be used in geophysical applications to monitor iron mineralization processes associated with contaminant remediation. The first part of the research presented in this thesis focuses on understanding the effect of iron mineral form and redox state on the NMR relaxation response of water in geologic material. Laboratory NMR measurements were made on Fe(III)-bearing minerals (ferrihydrite, lepidocrocite, goethite, and hematite), Fe(II)-bearing minerals (siderite, pyrite, and troilite), and a mixed valence iron-bearing mineral (magnetite). The results of these measurements show that the relaxation rate of water is strongly dependent on the mineral form of iron. Shown in the final section of this thesis are results from an experiment exploring temporal changes in the measured NMR relaxation rates during the reaction of ferrihydrite with aqueous Fe(II). These results show that NMR can be used to monitor temporal chemical changes in iron minerals. I conclude that this research shows that NMR indeed has the potential to be used as a tool for monitoring geochemical reactions associated with contaminant remediation.

  13. Conformational characterization of ceramides by nuclear magnetic resonance spectroscopy.

    PubMed Central

    Li, Li; Tang, Xiaoping; Taylor, K Grant; DuPré, Donald B; Yappert, M Cecilia

    2002-01-01

    Ceramide (Cer) has been identified as an active lipid second messenger in the regulation of cell growth, differentiation, and apoptosis. Its analog, dihydroceramide, without the 4 to 5 trans double bond in the sphingoid backbone lacks these biological effects. To establish the conformational features that distinguish ceramide from its analogs, nuclear magnetic resonance spectral data were acquired for diluted samples of ceramides (C2- and C18-Cer), dihydroceramide (C16-DHCer), and deoxydihydroceramide (C18-DODHCer). Our results suggest that in both C2- and C18-Cer, an H-bond network is formed in which the amide proton NH is donated to the OH groups on carbons C1 and C3 of the sphingosine backbone. Two tightly bound water molecules appear to stabilize this network by participating in flip-flop interactions with the hydroxyl groups. In DHCer, the lack of the trans double bond leads to a conformational distortion of this H-bonding motif. Without the critical double bond, the degree with which water molecules stabilize the H bonds between the two OH groups of the sphingolipid is reduced. This structural alteration might preclude the participation of DHCer in signaling-related interactions with cellular targets. PMID:11916863

  14. Multinuclear nuclear magnetic resonance spectroscopic study of cartilage proteoglycans

    SciTech Connect

    Lerner, L.

    1985-01-01

    Hyaline cartilage is a composite material whose major function is to withstand compression while retaining flexibility. Its mechanical properties are affected by tissue hydration and ionic composition. Models of the mechanical behavior of cartilage have incorporated certain assumptions about the interactions of the major components of cartilage: collagen, proteoglycans, water, and cations. To determine the validity of these assumption, the authors have used nuclear magnetic resonance spectroscopy (NMR). Two approaches have been used: (a) natural abundance carbon-13 NMR; and (b) NMR of sodium-23, potassium-39, magnesium-25, and calcium-43. Evidence from studies in intact tissues are reinforced by extensive measurements on solutions of proteoglycans and other relevant macromolecules. Based on the measurements of NMR relaxation rates and lineshapes reported here, it is concluded that neither sodium nor potassium interact strongly with bovine nasal proteoglycan aggregates or their substituent glycosaminoglycan chains in solution. Proteoglycans do bind magnesium and calcium. Therefore there is a qualitative difference between monovalent and divalent cations, which is not taken into account by polyelectrolyte models or models for the ionic dependence of mechanical properties. Cation binding to heparin, which has a higher charge density than cartilage proteoglycans, was also studied. The results presented here establish that heparin binds sodium, magnesium, and calcium.

  15. Segmental Isotopic Labeling of Proteins for Nuclear Magnetic Resonance

    PubMed Central

    Dongsheng, Liu; Xu, Rong; Cowburn, David

    2009-01-01

    Nuclear Magnetic Resonance (NMR) spectroscopy has emerged as one of the principle techniques of structural biology. It is not only a powerful method for elucidating the 3D structures under near physiological conditions, but also a convenient method for studying protein-ligand interactions and protein dynamics. A major drawback of macromolecular NMR is its size limitation caused by slower tumbling rates and greater complexity of the spectra as size increases. Segmental isotopic labeling allows specific segment(s) within a protein to be selectively examined by NMR thus significantly reducing the spectral complexity for large proteins and allowing a variety of solution-based NMR strategies to be applied. Two related approaches are generally used in the segmental isotopic labeling of proteins: expressed protein ligation and protein trans-splicing. Here we describe the methodology and recent application of expressed protein ligation and protein trans-splicing for NMR structural studies of proteins and protein complexes. We also describe the protocol used in our lab for the segmental isotopic labeling of a 50 kDa protein Csk (C-terminal Src Kinase) using expressed protein ligation methods. PMID:19632474

  16. Theoretical and experimental studies in nuclear magnetic resonance

    NASA Astrophysics Data System (ADS)

    Roehrich, Adrienne M.

    Nuclear magnetic resonance (NMR) is a tool used to probe the physical and chemical environments of specific atoms in molecules. This research explored small molecule analogues to biological materials to determine NMR parameters using ab initio computations, comparing the results with solid-state NMR measurements. Models, such as dimethyl phosphate (DMP) for oligonucleotides or CuCl for the active site of the protein azurin, represented computationally unwieldy macromolecules. 31P chemical shielding tensors were calculated for DMP as a function of torsion angles, as well as for the phosphate salts, ammonium dihydrogen phosphate (ADHP), diammonium hydrogen phosphate, and magnesium dihydrogen phosphate. The computational DMP work indicated a problem with the current standard 31P reference of 85% H3PO 4(aq.). Comparison of the calculations and experimental spectra for the phosphate salts indicated ADHP might be a preferable alternative as a solid state NMR reference for 31P. Experimental work included magic angle spinning experiments on powder samples using the UNL chemistry department's Bruker Avance 600 MHz NMR to collect data to determine chemical shielding anisotropies. For the quadrupolar nuclei of copper and scandium, the electric field gradient was calculated in diatomic univalent metal halides, allowing determination of the minimal level of theory necessary to compute NMR parameters for these nuclei.

  17. Updated methodology for nuclear magnetic resonance characterization of shales.

    PubMed

    Washburn, Kathryn E; Birdwell, Justin E

    2013-08-01

    Unconventional petroleum resources, particularly in shales, are expected to play an increasingly important role in the world's energy portfolio in the coming years. Nuclear magnetic resonance (NMR), particularly at low-field, provides important information in the evaluation of shale resources. Most of the low-field NMR analyses performed on shale samples rely heavily on standard T1 and T2 measurements. We present a new approach using solid echoes in the measurement of T1 and T1-T2 correlations that addresses some of the challenges encountered when making NMR measurements on shale samples compared to conventional reservoir rocks. Combining these techniques with standard T1 and T2 measurements provides a more complete assessment of the hydrogen-bearing constituents (e.g., bitumen, kerogen, clay-bound water) in shale samples. These methods are applied to immature and pyrolyzed oil shale samples to examine the solid and highly viscous organic phases present during the petroleum generation process. The solid echo measurements produce additional signal in the oil shale samples compared to the standard methodologies, indicating the presence of components undergoing homonuclear dipolar coupling. The results presented here include the first low-field NMR measurements performed on kerogen as well as detailed NMR analysis of highly viscous thermally generated bitumen present in pyrolyzed oil shale.

  18. Dynamic nuclear magnetic resonance field sensing with part-per-trillion resolution

    NASA Astrophysics Data System (ADS)

    Gross, Simon; Barmet, Christoph; Dietrich, Benjamin E.; Brunner, David O.; Schmid, Thomas; Pruessmann, Klaas P.

    2016-12-01

    High-field magnets of up to tens of teslas in strength advance applications in physics, chemistry and the life sciences. However, progress in generating such high fields has not been matched by corresponding advances in magnetic field measurement. Based mostly on nuclear magnetic resonance, dynamic high-field magnetometry is currently limited to resolutions in the nanotesla range. Here we report a concerted approach involving tailored materials, magnetostatics and detection electronics to enhance the resolution of nuclear magnetic resonance sensing by three orders of magnitude. The relative sensitivity thus achieved amounts to 1 part per trillion (10-12). To exemplify this capability we demonstrate the direct detection and relaxometry of nuclear polarization and real-time recording of dynamic susceptibility effects related to human heart function. Enhanced high-field magnetometry will generally permit a fresh look at magnetic phenomena that scale with field strength. It also promises to facilitate the development and operation of high-field magnets.

  19. Dynamic nuclear magnetic resonance field sensing with part-per-trillion resolution.

    PubMed

    Gross, Simon; Barmet, Christoph; Dietrich, Benjamin E; Brunner, David O; Schmid, Thomas; Pruessmann, Klaas P

    2016-12-02

    High-field magnets of up to tens of teslas in strength advance applications in physics, chemistry and the life sciences. However, progress in generating such high fields has not been matched by corresponding advances in magnetic field measurement. Based mostly on nuclear magnetic resonance, dynamic high-field magnetometry is currently limited to resolutions in the nanotesla range. Here we report a concerted approach involving tailored materials, magnetostatics and detection electronics to enhance the resolution of nuclear magnetic resonance sensing by three orders of magnitude. The relative sensitivity thus achieved amounts to 1 part per trillion (10(-12)). To exemplify this capability we demonstrate the direct detection and relaxometry of nuclear polarization and real-time recording of dynamic susceptibility effects related to human heart function. Enhanced high-field magnetometry will generally permit a fresh look at magnetic phenomena that scale with field strength. It also promises to facilitate the development and operation of high-field magnets.

  20. Dynamic nuclear magnetic resonance field sensing with part-per-trillion resolution

    PubMed Central

    Gross, Simon; Barmet, Christoph; Dietrich, Benjamin E.; Brunner, David O.; Schmid, Thomas; Pruessmann, Klaas P.

    2016-01-01

    High-field magnets of up to tens of teslas in strength advance applications in physics, chemistry and the life sciences. However, progress in generating such high fields has not been matched by corresponding advances in magnetic field measurement. Based mostly on nuclear magnetic resonance, dynamic high-field magnetometry is currently limited to resolutions in the nanotesla range. Here we report a concerted approach involving tailored materials, magnetostatics and detection electronics to enhance the resolution of nuclear magnetic resonance sensing by three orders of magnitude. The relative sensitivity thus achieved amounts to 1 part per trillion (10−12). To exemplify this capability we demonstrate the direct detection and relaxometry of nuclear polarization and real-time recording of dynamic susceptibility effects related to human heart function. Enhanced high-field magnetometry will generally permit a fresh look at magnetic phenomena that scale with field strength. It also promises to facilitate the development and operation of high-field magnets. PMID:27910860

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

    PubMed

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

    2016-12-07

    We present heteronuclear (19)F refocused CW (rCW) decoupling pulse sequences for solid-state magic-angle-spinning NMR applications. The decoupling sequences have been designed specifically to ensure suppression of the pertinent (13)C-(19)F dipolar coupling interactions while simultaneously suppressing strong anisotropic chemical shift as well as homonuclear (19)F-(19)F dipolar coupling effects as typically present in perfluorated compounds. In an extensive numerical and experimental analysis using a rigid, organic solid as a model compound, it becomes evident that the supercycled rCW schemes markedly improve the decoupling efficiency, leading to substantial enhancements in resolution and sensitivity when compared to previous state-of-the-art methods. Furthermore, considerable gains in robustness toward rf mismatch as well as offset in the radio-frequency carrier frequency are observed, all of which clearly render the new rCW schemes the methods of choice for (19)F decoupling in rigid, fluorinated compounds - which is further supported by a Floquet-based theoretical analysis.

  2. New Approaches to Quantum Computing using Nuclear Magnetic Resonance Spectroscopy

    SciTech Connect

    Colvin, M; Krishnan, V V

    2003-02-07

    The power of a quantum computer (QC) relies on the fundamental concept of the superposition in quantum mechanics and thus allowing an inherent large-scale parallelization of computation. In a QC, binary information embodied in a quantum system, such as spin degrees of freedom of a spin-1/2 particle forms the qubits (quantum mechanical bits), over which appropriate logical gates perform the computation. In classical computers, the basic unit of information is the bit, which can take a value of either 0 or 1. Bits are connected together by logic gates to form logic circuits to implement complex logical operations. The expansion of modern computers has been driven by the developments of faster, smaller and cheaper logic gates. As the size of the logic gates become smaller toward the level of atomic dimensions, the performance of such a system is no longer considered classical but is rather governed by quantum mechanics. Quantum computers offer the potentially superior prospect of solving computational problems that are intractable to classical computers such as efficient database searches and cryptography. A variety of algorithms have been developed recently, most notably Shor's algorithm for factorizing long numbers into prime factors in polynomial time and Grover's quantum search algorithm. The algorithms that were of only theoretical interest as recently, until several methods were proposed to build an experimental QC. These methods include, trapped ions, cavity-QED, coupled quantum dots, Josephson junctions, spin resonance transistors, linear optics and nuclear magnetic resonance. Nuclear magnetic resonance (NMR) is uniquely capable of constructing small QCs and several algorithms have been implemented successfully. NMR-QC differs from other implementations in one important way that it is not a single QC, but a statistical ensemble of them. Thus, quantum computing based on NMR is considered as ensemble quantum computing. In NMR quantum computing, the spins with

  3. Theoretical prediction of nuclear magnetic shieldings and indirect spin-spin coupling constants in 1,1-, cis-, and trans-1,2-difluoroethylenes

    SciTech Connect

    Nozirov, Farhod E-mail: farhod.nozirov@gmail.com; Stachów, Michał; Kupka, Teobald E-mail: farhod.nozirov@gmail.com

    2014-04-14

    A theoretical prediction of nuclear magnetic shieldings and indirect spin-spin coupling constants in 1,1-, cis- and trans-1,2-difluoroethylenes is reported. The results obtained using density functional theory (DFT) combined with large basis sets and gauge-independent atomic orbital calculations were critically compared with experiment and conventional, higher level correlated electronic structure methods. Accurate structural, vibrational, and NMR parameters of difluoroethylenes were obtained using several density functionals combined with dedicated basis sets. B3LYP/6-311++G(3df,2pd) optimized structures of difluoroethylenes closely reproduced experimental geometries and earlier reported benchmark coupled cluster results, while BLYP/6-311++G(3df,2pd) produced accurate harmonic vibrational frequencies. The most accurate vibrations were obtained using B3LYP/6-311++G(3df,2pd) with correction for anharmonicity. Becke half and half (BHandH) density functional predicted more accurate {sup 19}F isotropic shieldings and van Voorhis and Scuseria's τ-dependent gradient-corrected correlation functional yielded better carbon shieldings than B3LYP. A surprisingly good performance of Hartree-Fock (HF) method in predicting nuclear shieldings in these molecules was observed. Inclusion of zero-point vibrational correction markedly improved agreement with experiment for nuclear shieldings calculated by HF, MP2, CCSD, and CCSD(T) methods but worsened the DFT results. The threefold improvement in accuracy when predicting {sup 2}J(FF) in 1,1-difluoroethylene for BHandH density functional compared to B3LYP was observed (the deviations from experiment were −46 vs. −115 Hz)

  4. TANKS 18 AND 19-F STRUCTURAL FLOWABLE GROUT FILL MATERIAL EVALUATION AND RECOMMENDATIONS

    SciTech Connect

    Stefanko, D.; Langton, C.

    2011-11-01

    Cementitious grout will be used to close Tanks 18-F and 19-F. The functions of the grout are to: (1) physically stabilize the final landfill by filling the empty volume in the tanks with a non compressible material; (2) provide a barrier for inadvertent intrusion into the tank; (3) reduce contaminant mobility by (a) limiting the hydraulic conductivity of the closed tank and (b) reducing contact between the residual waste and infiltrating water; and (4) providing an alkaline, chemically reducing environment in the closed tank to control speciation and solubility of selected radionuclides. The objective of this work was to identify a single (all-in-one) grout to stabilize and isolate the residual radionuclides in the tank, provide structural stability of the closed tank and serve as an inadvertent intruder barrier. This work was requested by V. A. Chander, High Level Waste (HLW) Tank Engineering, in HLW-TTR-2011-008. The complete task scope is provided in the Task Technical and QA Plan, SRNL-RP-2011-00587 Revision 0. The specific objectives of this task were to: (1) Identify new admixtures and dosages for formulating a zero bleed flowable tank fill material selected by HLW Tank Closure Project personnel based on earlier tank fill studies performed in 2007. The chemical admixtures used for adjusting the flow properties needed to be updated because the original admixture products are no longer available. Also, the sources of cement and fly ash have changed, and Portland cements currently available contain up to 5 wt. % limestone (calcium carbonate). (2) Prepare and evaluate the placement, compressive strength, and thermal properties of the selected formulation with new admixture dosages. (3) Identify opportunities for improving the mix selected by HLW Closure Project personnel and prepare and evaluate two potentially improved zero bleed flowable fill design concepts; one based on the reactor fill grout and the other based on a shrinkage compensating flowable fill mix

  5. Liquid-state nuclear spin comagnetometers.

    PubMed

    Ledbetter, M P; Pustelny, S; Budker, D; Romalis, M V; Blanchard, J W; Pines, A

    2012-06-15

    We discuss nuclear spin comagnetometers based on ultralow-field nuclear magnetic resonance in mixtures of miscible solvents, each rich in a different nuclear spin. In one version thereof, Larmor precession of protons and 19F nuclei in a mixture of thermally polarized pentane and hexafluorobenzene is monitored via a sensitive alkali-vapor magnetometer. We realize transverse relaxation times in excess of 20 s and suppression of magnetic field fluctuations by a factor of 3400. We estimate it should be possible to achieve single-shot sensitivity of about 5×10(-9)  Hz, or about 5×10(-11)  Hz in ≈1 day of integration. In a second version, spin precession of protons and 129Xe nuclei in a mixture of pentane and hyperpolarized liquid xenon is monitored using superconducting quantum interference devices. Application to spin-gravity experiments, electric dipole moment experiments, and sensitive gyroscopes is discussed.

  6. 19F NMR analysis of the antimicrobial peptide PGLa bound to native cell membranes from bacterial protoplasts and human erythrocytes.

    PubMed

    Ieronimo, Marco; Afonin, Sergii; Koch, Katja; Berditsch, Marina; Wadhwani, Parvesh; Ulrich, Anne S

    2010-07-07

    (19)F NMR is a unique tool to examine the structure of fluorine-labeled peptides in their native cellular environment, due to an exquisite sensitivity and lack of natural abundance background. For solid-state NMR analysis, we isolated native membranes from erythrocyte ghosts and bacterial protoplasts and prepared them as macroscopically oriented samples. They showed a high purity and quality of alignment according to (31)P NMR, and the membrane-bound antimicrobial peptide PGLa could be detected by (19)F NMR. The characteristic fingerprint splitting of its (19)F reporter group indicated that the peptide helix binds to the native membranes in a surface alignment, albeit with a higher affinity in the prokaryotic than the eukaryotic system.

  7. Studies of Energy-Relevant Materials by Nuclear Magnetic Resonance

    NASA Astrophysics Data System (ADS)

    Cui, Jinfang

    In this thesis, we have used nuclear magnetic resonance (NMR) as a local probe to microscopically study three different families of energy-relevant complex materials, namely the 122 Fe-based superconductors Ca(Fe1-xCox)2As2, GeTe-based thermoelectric tellurides GeTe and detonation nanodiamond. In Chapter 3 and Chapter 4, we investigated the Co substitution effects on static and dynamic magnetic properties of the single-crystalline Ca(Fe 1-xCox)2As2 (x = 0, 0.023, 0.028, 0.033, 0.059) via 75As NMR and resistivity measurements. Robustness of the Fe magnetic moments was evidenced by only slight decreases of Hint, although T N is strongly suppressed with Co substitution in antiferromagnetic (AFM) state. In the paramagnetic (PM) state, the temperature dependence of Knight shift K for all crystals shows similar T-dependence of magnetic susceptibility chi. The spin fluctuations with the q = 0 components are suppressed with Delta/k B. On the other hand, the growth of the stripe-type AFM fluctuations with q = (pi, 0) or (0, pi) upon cooling in the PM state for all samples is evidenced by the T-dependence of (1/ T1Tchi). A pseudogap-like phenomenon, i.e., suppression of the AFM spin fluctuations, was discovered with decreasing temperature below a x-independent characteristic temperature T* ( 100 K) in samples with x ≥ 0.028. In addition, clear evidence for the coexistence and competition of the stripe-type antiferromagnetic and ferromagnetic (FM) spin correlations was given by modified Korringa ratio analysis in Chapter 4. In Chapter 5, we have carried out 125Te NMR measurements to study the electronic properties of Ge50Te50, Ag 2Ge48Te50 and Sb2Ge48Te 50. NMR shift K and 1/T1T of Ge50Te50 are nearly temperature independent at T < 50 K and both increase slightly with increasing temperature at high temperatures. A two-band model, where one band overlaps the Fermi level and the other band is separated from the Fermi level by an energy gap, has been used to explain these

  8. Novel nuclear magnetic resonance techniques for studying biological molecules

    SciTech Connect

    Laws, David Douglas

    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 13Ca, 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.

  9. Nuclear magnetic resonance data of C2H10OSi2

    NASA Astrophysics Data System (ADS)

    Mikhova, B. M.

    This document is part of Part 6 `Organic Metalloid Compounds' of Subvolume D 'Chemical Shifts and Coupling Constants for Carbon-13' of Landolt-Börnstein III/35 'Nuclear Magnetic Resonance Data', Group III 'Condensed Matter'.

  10. Nuclear magnetic resonance data of C8H24OSi4Te

    NASA Astrophysics Data System (ADS)

    Mikhova, B. M.

    This document is part of Part 6 `Organic Metalloid Compounds' of Subvolume D 'Chemical Shifts and Coupling Constants for Carbon-13' of Landolt-Börnstein III/35 'Nuclear Magnetic Resonance Data', Group III 'Condensed Matter'.

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

    SciTech Connect

    Goodson, Boyd McLean

    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.

  12. Developing hyperpolarized krypton-83 for nuclear magnetic resonance spectroscopy and magnetic resonance imaging

    NASA Astrophysics Data System (ADS)

    Cleveland, Zackary I.

    This dissertation discusses the production of highly nonequilibrium nuclear spin polarization, referred to as hyperpolarization or hp, in the nuclear spin I = 9/2 noble gas isotope krypton-83 using spin exchange optical pumping (SEOP). This nonequilibrium polarization yields nuclear magnetic resonance (NMR) signals that are enhanced three or more orders of magnitude above those of thermally polarized krypton and enables experiments that would otherwise be impossible. Krypton-83 possesses a nuclear electric quadrupole moment that dominates the longitudinal (T1) relaxation due to coupling of the quadrupole moment to fluctuating electric field gradients generated by distortions to the spherical symmetry of the electronic environment. Relaxation slows polarization buildup and limits the maximum signal intensity but makes krypton-83 a sensitive probe of its environment. The gas-phase krypton-83 longitudinal relaxation rate increases linearly with total gas density due to binary collisions. Density independent relaxation, caused by the formation of krypton-krypton van der Waals molecules and surface adsorption, also contributes to the observed rate. Buffer gases suppress van der Waals molecule mediated relaxation by breaking apart the weakly bound krypton dimers. Surface relaxation is gas composition independent and therefore more difficult to suppress. However, this relaxation mechanism makes hp krypton-83 sensitive to important surface properties including surface-to-volume ratio, surface chemistry, and surface temperature. The presence of surfaces with high krypton adsorption affinities (i.e. hydrophobic surfaces) accelerates the relaxation times and can produce T1 contrast in hp krypton-83 magnetic resonance imaging (MRI). Tobacco smoke deposited on surfaces generates strong T1 contrast allowing the observation of smoke deposition with spatial resolution. Conversely, water adsorption on surfaces significantly lengths the T1 times due competitive surface adsorption

  13. Magnetic susceptibility and neutron diffraction experiments on nuclear ordering in copper

    NASA Astrophysics Data System (ADS)

    Jyrkkio, Teppo

    Experimental curves of entropy and susceptibility versus temperature for copper nuclear spins down to the ordered state were obtained. Impurities and anomalous spin-lattice relaxation in copper at submilli-Kelvin temperatures were observed. Phase diagrams for spontaneous nuclear ordering in copper were derived. Nuclear antiferromagnetic ordering in copper was investigated. The feasibility of neutron diffraction experiments on ordered copper nuclei at nano-Kelvin temperature was studied. Neutron scattering experiments on nuclear magnets were carried out. Calibration and applications of polarized neutron thermometry at milli- and micro-Kelvin temperatures is described.Observation of nuclear antiferromagnetic order in copper by neutron diffraction at nano-Kelvin temparatures is reported.

  14. Constraints on low-mass WIMP interactions on 19F from PICASSO

    NASA Astrophysics Data System (ADS)

    Archambault, S.; Behnke, E.; Bhattacharjee, P.; Bhattacharya, S.; Dai, X.; Das, M.; Davour, A.; Debris, F.; Dhungana, N.; Farine, J.; Gagnebin, S.; Giroux, G.; Grace, E.; Jackson, C. M.; Kamaha, A.; Krauss, C.; Kumaratunga, S.; Lafrenière, M.; Laurin, M.; Lawson, I.; Lessard, L.; Levine, I.; Levy, C.; MacDonald, R. P.; Marlisov, D.; Martin, J.-P.; Mitra, P.; Noble, A. J.; Piro, M.-C.; Podviyanuk, R.; Pospisil, S.; Saha, S.; Scallon, O.; Seth, S.; Starinski, N.; Stekl, I.; Wichoski, U.; Xie, T.; Zacek, V.

    2012-05-01

    Recent results from the PICASSO dark matter search experiment at SNOLAB are reported. These results were obtained using a subset of 10 detectors with a total target mass of 0.72 kg of 19F and an exposure of 114 kgd. The low backgrounds in PICASSO allow recoil energy thresholds as low as 1.7 keV to be obtained which results in an increased sensitivity to interactions from Weakly Interacting Massive Particles (WIMPs) with masses below 10 GeV/c2. No dark matter signal was found. Best exclusion limits in the spin dependent sector were obtained for WIMP masses of 20 GeV/c2 with a cross section on protons of σpSD=0.032 pb (90% C.L.). In the spin independent sector close to the low mass region of 7 GeV/c2 favoured by CoGeNT and DAMA/LIBRA, cross sections larger than σpSI=1.41×10-4 pb (90% C.L.) are excluded.

  15. Determination of membrane immersion depth with O(2): a high-pressure (19)F NMR study.

    PubMed Central

    Prosser, R S; Luchette, P A; Westerman, P W; Rozek, A; Hancock, R E

    2001-01-01

    Oxygen is known to partition with an increasing concentration gradient toward the hydrophobic membrane interior. At partial pressures (P(O2)) of 100 Atm or more, this concentration gradient is sufficient to induce paramagnetic effects that depend sensitively on membrane immersion depth. This effect is demonstrated for the fluorine nucleus by depth-dependent paramagnetic shifts and spin-lattice relaxation rates, using a fluorinated detergent, CF3(CF(2))(5)C(2)H(4)-O-maltose (TFOM), reconstituted into a lipid bilayer model membrane system. To interpret the spin-lattice relaxation rates (R) in terms of a precise immersion depth, two specifically fluorinated cholesterol species (6-fluorocholesterol and 25-fluorocholesterol), whose membrane immersion depths were independently estimated, were studied by (19)F NMR. The paramagnetic relaxation rates, R, of the cholesterol species were then used to parameterize a Gaussian profile that directly relates R to immersion depth z. This same Gaussian curve could then be used to determine the membrane immersion depth of all six fluorinated chain positions of TFOM and of two adjacent residues of specifically fluorinated analogs of the antibacterial peptide indolicidin. The potential of this method for determination of immersion depth and topology of membrane proteins is discussed. PMID:11222301

  16. 1H and 19F NMR relaxation studies of fleroxacin with Micrococcus luteus.

    PubMed

    Waibel, Benjamin; Holzgrabe, Ulrike

    2007-04-11

    In order to investigate and characterize interaction processes between the fluoroquinolone fleroxacin and bacterial cells we used non-selective (all resonances are excited), selective (observed resonance is excited) spin-lattice relaxation rates and spin-spin relaxation measurements. The signals of three hydrogens at different moieties of the fleroxacin molecule were considered to get an insight in the complexation behavior. The enhancement of selective relaxation rates was observed with increasing fleroxacin concentrations and keeping the bacterial mass constant. The obtained relaxation rates of the affected hydrogens were analyzed via a Lineweaver-Burk-plot to determine the KD values. Furthermore, 19F NMR spectra were recorded and spin-spin relaxation rates (R2) were determined by a Carr-Purcell-Meiboom-Gill (CPMG) pulse sequence. Because of the dependency of the line width of NMR peaks on transversal relaxation time T2, we compared the line width at half-height at different fleroxacin concentrations in order to investigate the involvement of fluorine atoms in different positions in the complexation. All findings point to core quinolone moiety to be involved in the interaction with bacterial cells.

  17. Robust and efficient 19F heteronuclear dipolar decoupling using refocused continuous-wave rf irradiation

    NASA Astrophysics Data System (ADS)

    Vinther, Joachim M.; Khaneja, Navin; Nielsen, Niels Chr.

    2013-01-01

    Refocused continuous wave (rCW) decoupling is presented as an efficient and robust means to obtain well-resolved magic-angle-spinning solid-state NMR spectra of low-γ spins, such as 13C dipolar coupled to fluorine. The rCW decoupling sequences, recently introduced for 1H decoupling, are very robust towards large isotropic and anisotropic shift ranges as often encountered for 19F spins. In rCW decoupling, the so-called refocusing pulses inserted into the CW irradiation eliminate critical residual second- and third-order dipolar coupling and dipolar-coupling against chemical shielding anisotropy cross-terms in the effective Hamiltonian through time-reversal (i.e. refocusing). As important additional assets, the rCW decoupling sequences are robust towards variations in rf amplitudes, operational at low to high spinning speeds, and easy to set-up for optimal performance experimentally. These aspects are demonstrated analytically/numerically and experimentally in comparison to state-of-the-art decoupling sequences such as TPPM, SPINAL-64, and frequency-swept variants of these.

  18. Nuclear Spin Maser at Highly Stabilized Low Magnetic Field and Search for Atomic EDM

    SciTech Connect

    Yoshimi, A.; Asahi, K.; Inoue, T.; Uchida, M.; Hatakeyama, N.; Tsuchiya, M.; Kagami, S.

    2009-08-04

    A nuclear spin maser is operated at a low static field through an active feedback scheme based on an optical nuclear spin detection and succeeding spin control by a transverse field application. The frequency stability of this optical-coupling spin maser is improved by installation of a low-noise current source for a solenoid magnet producing a static magnetic field in the maser operation. Experimental devices for application of the maser to EDM experiment are being developed.

  19. Optically Pumped Nuclear Magnetic Resonance in the Quantum Hall Regimes

    NASA Astrophysics Data System (ADS)

    Barrett, Sean E.

    1998-03-01

    Optical pumping enables the direct detection of the nuclear magnetic resonance signal of ^71Ga nuclei located in an electron doped GaAs quantum well.footnote S. E. Barrett et al., Phys. Rev. Lett. 72, 1368 (1994) This OPNMR technique was previously used to measure the Knight shift (K_S)footnote S. E. Barrett et al., Phys. Rev. Lett. 74, 5112 (1995) and spin-lattice relaxation time (T_1)footnote R. Tycko et al., Science 268, 1460 (1995) near Landau level filling ν=1, which provided the first experimental support for the theoretical predictionsfootnote S. L. Sondhi et al., Phys. Rev. B 47, 16419 (1993); H. A. Fertig et al., Phys. Rev. B 50, 11018 (1994) that the charged excitations of the ν = 1 ground state are novel spin textures called skyrmions. We have recently demonstrated that OPNMR is possible in fields up to B=12 Tesla, and temperatures down to T= 0.3 K, making it a viable new probe of the Fractional Quantum Hall Regime. In this talk we will present our latest OPNMR measurements near Landau level filling ν=1/3, which include the first direct measurement of the electron spin polarization at ν=1/3. The spin polarization drops as the filling factor is varied away from ν=1/3, indicating that the quasiparticles and quasiholes are not fully spin-polarized. We will also show how the NMR lineshape away from ν=1/3 changes dramatically at low temperatures, which is due to slowing of the electron dynamics, and a reduction in the motional narrowing of the NMR line. The current understanding of these results will be discussed.

  20. Nuclear magnetic resonance studies of macroscopic morphology and dynamics

    SciTech Connect

    Barrall, Geoffrey Alden

    1995-09-01

    Nuclear magnetic resonance techniques are traditionally used to study molecular level structure and dynamics with a noted exception in medically applied NMR imaging (MRI). In this work, new experimental methods and theory are presented relevant to the study of macroscopic morphology and dynamics using NMR field gradient techniques and solid state two-dimensional exchange NMR. The goal in this work is not to take some particular system and study it in great detail, rather it is to show the utility of a number of new and novel techniques using ideal systems primarily as a proof of principle. By taking advantage of the analogy between NMR imaging and diffraction, one may simplify the experiments necessary for characterizing the statistical properties of the sample morphology. For a sample composed of many small features, e.g. a porous medium, the NMR diffraction techniques take advantage of both the narrow spatial range and spatial isotropy of the sample`s density autocorrelation function to obtain high resolution structural information in considerably less time than that required by conventional NMR imaging approaches. The time savings of the technique indicates that NMR diffraction is capable of finer spatial resolution than conventional NMR imaging techniques. Radio frequency NMR imaging with a coaxial resonator represents the first use of cylindrically symmetric field gradients in imaging. The apparatus as built has achieved resolution at the micron level for water samples, and has the potential to be very useful in the imaging of circularly symmetric systems. The study of displacement probability densities in flow through a random porous medium has revealed the presence of features related to the interconnectedness of the void volumes. The pulsed gradient techniques used have proven successful at measuring flow properties for time and length scales considerably shorter than those studied by more conventional techniques.

  1. A Multidisciplinary Approach to High Throughput Nuclear Magnetic Resonance Spectroscopy

    PubMed Central

    Pourmodheji, Hossein; Ghafar-Zadeh, Ebrahim; Magierowski, Sebastian

    2016-01-01

    Nuclear Magnetic Resonance (NMR) is a non-contact, powerful structure-elucidation technique for biochemical analysis. NMR spectroscopy is used extensively in a variety of life science applications including drug discovery. However, existing NMR technology is limited in that it cannot run a large number of experiments simultaneously in one unit. Recent advances in micro-fabrication technologies have attracted the attention of researchers to overcome these limitations and significantly accelerate the drug discovery process by developing the next generation of high-throughput NMR spectrometers using Complementary Metal Oxide Semiconductor (CMOS). In this paper, we examine this paradigm shift and explore new design strategies for the development of the next generation of high-throughput NMR spectrometers using CMOS technology. A CMOS NMR system consists of an array of high sensitivity micro-coils integrated with interfacing radio-frequency circuits on the same chip. Herein, we first discuss the key challenges and recent advances in the field of CMOS NMR technology, and then a new design strategy is put forward for the design and implementation of highly sensitive and high-throughput CMOS NMR spectrometers. We thereafter discuss the functionality and applicability of the proposed techniques by demonstrating the results. For microelectronic researchers starting to work in the field of CMOS NMR technology, this paper serves as a tutorial with comprehensive review of state-of-the-art technologies and their performance levels. Based on these levels, the CMOS NMR approach offers unique advantages for high resolution, time-sensitive and high-throughput bimolecular analysis required in a variety of life science applications including drug discovery. PMID:27294925

  2. Advances in Theory of Solid-State Nuclear Magnetic Resonance

    PubMed Central

    Mananga, Eugene S.; Moghaddasi, Jalil; Sana, Ajaz; Akinmoladun, Andrew; Sadoqi, Mostafa

    2015-01-01

    Recent advances in theory of solid state nuclear magnetic resonance (NMR) such as Floquet-Magnus expansion and Fer expansion, address alternative methods for solving a time-dependent linear differential equation which is a central problem in quantum physics in general and solid-state NMR in particular. The power and the salient features of these theoretical approaches that are helpful to describe the time evolution of the spin system at all times are presented. This review article presents a broad view of manipulations of spin systems in solid-state NMR, based on milestones theories including the average Hamiltonian theory and the Floquet theory, and the approaches currently developing such as the Floquet-Magnus expansion and the Fer expansion. All these approaches provide procedures to control and describe the spin dynamics in solid-state NMR. Applications of these theoretical methods to stroboscopic and synchronized manipulations, non-synchronized experiments, multiple incommensurated frequencies, magic-angle spinning samples, are illustrated. We also reviewed the propagators of these theories and discussed their convergences. Note that the FME is an extension of the popular Magnus Expansion and Average Hamiltonian Theory. It aims is to bridge the AHT to the Floquet Theorem but in a more concise and efficient formalism. Calculations can then be performed in a finite-dimensional Hilbert space instead of an infinite dimensional space within the so-called Floquet theory. We expected that the FME will provide means for more accurate and efficient spin dynamics simulation and for devising new RF pulse sequence. PMID:26878063

  3. A Multidisciplinary Approach to High Throughput Nuclear Magnetic Resonance Spectroscopy.

    PubMed

    Pourmodheji, Hossein; Ghafar-Zadeh, Ebrahim; Magierowski, Sebastian

    2016-06-09

    Nuclear Magnetic Resonance (NMR) is a non-contact, powerful structure-elucidation technique for biochemical analysis. NMR spectroscopy is used extensively in a variety of life science applications including drug discovery. However, existing NMR technology is limited in that it cannot run a large number of experiments simultaneously in one unit. Recent advances in micro-fabrication technologies have attracted the attention of researchers to overcome these limitations and significantly accelerate the drug discovery process by developing the next generation of high-throughput NMR spectrometers using Complementary Metal Oxide Semiconductor (CMOS). In this paper, we examine this paradigm shift and explore new design strategies for the development of the next generation of high-throughput NMR spectrometers using CMOS technology. A CMOS NMR system consists of an array of high sensitivity micro-coils integrated with interfacing radio-frequency circuits on the same chip. Herein, we first discuss the key challenges and recent advances in the field of CMOS NMR technology, and then a new design strategy is put forward for the design and implementation of highly sensitive and high-throughput CMOS NMR spectrometers. We thereafter discuss the functionality and applicability of the proposed techniques by demonstrating the results. For microelectronic researchers starting to work in the field of CMOS NMR technology, this paper serves as a tutorial with comprehensive review of state-of-the-art technologies and their performance levels. Based on these levels, the CMOS NMR approach offers unique advantages for high resolution, time-sensitive and high-throughput bimolecular analysis required in a variety of life science applications including drug discovery.

  4. Advances in Theory of Solid-State Nuclear Magnetic Resonance.

    PubMed

    Mananga, Eugene S; Moghaddasi, Jalil; Sana, Ajaz; Akinmoladun, Andrew; Sadoqi, Mostafa

    Recent advances in theory of solid state nuclear magnetic resonance (NMR) such as Floquet-Magnus expansion and Fer expansion, address alternative methods for solving a time-dependent linear differential equation which is a central problem in quantum physics in general and solid-state NMR in particular. The power and the salient features of these theoretical approaches that are helpful to describe the time evolution of the spin system at all times are presented. This review article presents a broad view of manipulations of spin systems in solid-state NMR, based on milestones theories including the average Hamiltonian theory and the Floquet theory, and the approaches currently developing such as the Floquet-Magnus expansion and the Fer expansion. All these approaches provide procedures to control and describe the spin dynamics in solid-state NMR. Applications of these theoretical methods to stroboscopic and synchronized manipulations, non-synchronized experiments, multiple incommensurated frequencies, magic-angle spinning samples, are illustrated. We also reviewed the propagators of these theories and discussed their convergences. Note that the FME is an extension of the popular Magnus Expansion and Average Hamiltonian Theory. It aims is to bridge the AHT to the Floquet Theorem but in a more concise and efficient formalism. Calculations can then be performed in a finite-dimensional Hilbert space instead of an infinite dimensional space within the so-called Floquet theory. We expected that the FME will provide means for more accurate and efficient spin dynamics simulation and for devising new RF pulse sequence.

  5. A proposed direct measurement of cross section at Gamow window for key reaction 19F(p,α) 16O in Asymptotic Giant Branch stars with a planned accelerator in CJPL

    NASA Astrophysics Data System (ADS)

    He, JianJun; Xu, ShiWei; Ma, ShaoBo; Hu, Jun; Zhang, LiYong; Fu, ChangBo; Zhang, NingTao; Lian, Gang; Su, Jun; Li, YunJu; Yan, ShengQuan; Shen, YangPing; Hou, SuQing; Jia, BaoLu; Zhang, Tao; Zhang, XiaoPeng; Guo, Bing; Kubono, Shigeru; Liu, WeiPing

    2016-05-01

    In 2014, the National Natural Science Foundation of China (NSFC) approved the Jinping Underground Nuclear Astrophysics laboratory (JUNA) project, which aims at direct cross-section measurements of four key stellar nuclear reactions right down to the Gamow windows. In order to solve the observed fluorine overabundances in Asymptotic Giant Branch (AGB) stars, measuring the key 19F(p,α)16O reaction at effective burning energies (i.e., at Gamow window) is established as one of the scientific research sub-projects. The present paper describes this sub-project in details, including motivation, status, experimental setup, yield and background estimation, aboveground test, as well as other relevant reactions.

  6. Double-tuned single coil probe for nuclear magnetic resonance spectrometer

    SciTech Connect

    McKay, R.A.

    1984-05-01

    A double-tuned single coil probe for a nuclear magnetic resonance spectrometer having improved sensitivity is described comprising a double-tuned circuit means in which the low frequency irradiation is fed to a transmission line through an inductor means. The double-tuned circuit means of the invention may be remotely disposed from the magnetic field which results in greater sensitivity.

  7. Electronic and nuclear motion and their couplings in the presence of a magnetic field

    NASA Astrophysics Data System (ADS)

    Schmelcher, P.; Cederbaum, L. S.; Meyer, H.-D.

    1988-12-01

    The performance of an adiabatic separation of electronic and nuclear motion in the presence of a magnetic field is examined, and it is shown that the diagonal term of the nonadiabatic coupling elements must be added to the nuclear equation of motion in the Born-Oppenheimer (BO) approximation. The screened BO approximation is described which is particularly suited to describe the adiabatic separation of electronic and nuclear degrees of freedom in a magnetic field. A new interpretation of the well-known gauge-centering is presented. The results are of interest in connection with the studies of white dwarfs and neutron stars.

  8. MEMS-Based Force-Detected Nuclear Magnetic Resonance (FDNMR) Spectrometer

    NASA Technical Reports Server (NTRS)

    Lee, Choonsup; Butler, Mark C.; Elgammal, Ramez A.; George, Thomas; Hunt, Brian; Weitekamp, Daniel P.

    2006-01-01

    Nuclear Magnetic Resonance (NMR) spectroscopy allows assignment of molecular structure by acquiring the energy spectrum of nuclear spins in a molecule, and by interpreting the symmetry and positions of resonance lines in the spectrum. As such, NMR has become one of the most versatile and ubiquitous spectroscopic methods. Despite these tremendous successes, NMR experiments suffer from inherent low sensitivity due to the relatively low energy of photons in the radio frequency (rt) region of the electromagnetic spectrum. Here, we describe a high-resolution spectroscopy in samples with diameters in the micron range and below. We have reported design and fabrication of force-detected nuclear magnetic resonance (FDNMR).

  9. MEMS-Based Force-Detected Nuclear Magnetic Resonance (FDNMR) Spectrometer

    NASA Technical Reports Server (NTRS)

    Lee, Choonsup; Butler, Mark C.; Elgammal, Ramez A.; George, Thomas; Hunt, Brian; Weitekamp, Daniel P.

    2006-01-01

    Nuclear Magnetic Resonance (NMR) spectroscopy allows assignment of molecular structure by acquiring the energy spectrum of nuclear spins in a molecule, and by interpreting the symmetry and positions of resonance lines in the spectrum. As such, NMR has become one of the most versatile and ubiquitous spectroscopic methods. Despite these tremendous successes, NMR experiments suffer from inherent low sensitivity due to the relatively low energy of photons in the radio frequency (rt) region of the electromagnetic spectrum. Here, we describe a high-resolution spectroscopy in samples with diameters in the micron range and below. We have reported design and fabrication of force-detected nuclear magnetic resonance (FDNMR).

  10. GET-SERF, a new gradient encoded SERF experiment for the trivial edition of 1H-19F couplings.

    PubMed

    Di Pietro, Maria Enrica; Aroulanda, Christie; Merlet, Denis

    2013-09-01

    A new spatially encoded heteronuclear (1)H-(19)F selective refocusing NMR experiment (GET-SERF) is proposed. This sequence allows editing in one single 2D experiment all couplings between a selected fluorine site and all the proton nuclei of the molecule. Its efficiency is illustrated in the case of diflunisal, a difluorinated anti-inflammatory drug, in isotropic and anisotropic media.

  11. Fluorinated Carbohydrates as Lectin Ligands: 19F-Based Direct STD Monitoring for Detection of Anomeric Selectivity

    PubMed Central

    Ribeiro, João P.; Diercks, Tammo; Jiménez-Barbero, Jesús; André, Sabine; Gabius, Hans-Joachim; Cañada, Francisco Javier

    2015-01-01

    The characterization of the binding of reducing carbohydrates present as mixtures of anomers in solution to a sugar recepor (lectin) poses severe difficulties. In this situation, NMR spectroscopy enables the observation of signals for each anomer in the mixture by applying approaches based on ligand observation. Saturation transfer difference (STD) NMR allows fast and efficient screening of compound mixtures for reactivity to a receptor. Owing to the exceptionally favorable properties of 19F in NMR spectroscopy and the often complex 1H spectra of carbohydrates, 19F-containing sugars have the potential to be turned into versatile sensors for recognition. Extending the recently established 1H → 1H STDre19F-NMR technique, we here demonstrate its applicability to measure anomeric selectivity of binding in a model system using the plant lectin concanavalin A (ConA) and 2-deoxy-2-fluoro-d-mannose. Indeed, it is also possible to account for the mutual inhibition between the anomers on binding to the lectin by means of a kinetic model. The monitoring of 19F-NMR signal perturbation disclosed the relative activities of the anomers in solution and thus enabled the calculation of their binding affinity towards ConA. The obtained data show a preference for the α anomer that increases with temperature. This experimental approach can be extended to others systems of biomedical interest by testing human lectins with suitably tailored glycan derivatives. PMID:26580665

  12. Fluorinated Carbohydrates as Lectin Ligands: (19)F-Based Direct STD Monitoring for Detection of Anomeric Selectivity.

    PubMed

    Ribeiro, João P; Diercks, Tammo; Jiménez-Barbero, Jesús; André, Sabine; Gabius, Hans-Joachim; Cañada, Francisco Javier

    2015-11-13

    The characterization of the binding of reducing carbohydrates present as mixtures of anomers in solution to a sugar recepor (lectin) poses severe difficulties. In this situation, NMR spectroscopy enables the observation of signals for each anomer in the mixture by applying approaches based on ligand observation. Saturation transfer difference (STD) NMR allows fast and efficient screening of compound mixtures for reactivity to a receptor. Owing to the exceptionally favorable properties of (19)F in NMR spectroscopy and the often complex ¹H spectra of carbohydrates, (19)F-containing sugars have the potential to be turned into versatile sensors for recognition. Extending the recently established ¹H → ¹H STDre(19)F-NMR technique, we here demonstrate its applicability to measure anomeric selectivity of binding in a model system using the plant lectin concanavalin A (ConA) and 2-deoxy-2-fluoro-d-mannose. Indeed, it is also possible to account for the mutual inhibition between the anomers on binding to the lectin by means of a kinetic model. The monitoring of (19)F-NMR signal perturbation disclosed the relative activities of the anomers in solution and thus enabled the calculation of their binding affinity towards ConA. The obtained data show a preference for the α anomer that increases with temperature. This experimental approach can be extended to others systems of biomedical interest by testing human lectins with suitably tailored glycan derivatives.

  13. Novel detection schemes of nuclear magnetic resonance and magnetic resonance imaging: applications from analytical chemistry to molecular sensors.

    PubMed

    Harel, Elad; Schröder, Leif; Xu, Shoujun

    2008-01-01

    Nuclear magnetic resonance (NMR) is a well-established analytical technique in chemistry. The ability to precisely control the nuclear spin interactions that give rise to the NMR phenomenon has led to revolutionary advances in fields as diverse as protein structure determination and medical diagnosis. Here, we discuss methods for increasing the sensitivity of magnetic resonance experiments, moving away from the paradigm of traditional NMR by separating the encoding and detection steps of the experiment. This added flexibility allows for diverse applications ranging from lab-on-a-chip flow imaging and biological sensors to optical detection of magnetic resonance imaging at low magnetic fields. We aim to compare and discuss various approaches for a host of problems in material science, biology, and physics that differ from the high-field methods routinely used in analytical chemistry and medical imaging.

  14. Noncyclic geometric quantum computation in a nuclear-magnetic-resonance system

    SciTech Connect

    Wang, Z. S.; Liu, G. Q.; Ji, Y. H.

    2009-05-15

    A scheme is proposed to include both cyclic and noncyclic geometric quantum computations in nuclear-magnetic-resonance system by the invariant theory. By controlling magnetic field and arbitrary parameters in the invariant operator, the phases accumulated in the entangling quantum gates for single- and two-qubit systems are pure geometric phases. Thus, fault tolerance may occur in some critical magnetic field parameters for either cyclic or noncyclic evolution by differently choosing for gate time.

  15. Nuclear magnetic resonance at millitesla fields using a zero-field spectrometer.

    PubMed

    Tayler, Michael C D; Sjolander, Tobias F; Pines, Alexander; Budker, Dmitry

    2016-09-01

    We describe new analytical capabilities for nuclear magnetic resonance (NMR) experiments in which signal detection is performed with chemical resolution (via spin-spin J couplings) in the zero to ultra-low magnetic field region, below 1μT. Using magnetic fields in the 100μT to 1mT range, we demonstrate the implementation of conventional NMR pulse sequences with spin-species selectivity.

  16. Development and applications of NMR (nuclear magnetic resonance) in low fields and zero field

    SciTech Connect

    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.

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

    NASA Astrophysics Data System (ADS)

    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

  18. Microstructure of Wet Cement Pastes: a Nuclear Magnetic Resonance Study

    NASA Astrophysics Data System (ADS)

    Jehng, Jyh-Yuar

    1995-01-01

    Nuclear magnetic resonance relaxation analysis has been applied to interpret the evolution of microstructure in a cement paste during hydration. The work in this thesis has yielded a better understanding of the geometric and physical characterization of porous materials, and specifically cement pastes. A basic understanding of the wet-dry and freeze-thaw processes of cement pastes has been developed. The pore structure evolution has been studied by the suppression of the freezing temperature of water and compared with relaxation analysis performed at room temperature. Both methods consistently show that hydrating cement pastes have two principal components in their size distribution. Firstly, in situ measurements have been made of the water consumption, the total specific surface area, and pore water size distribution as a function of hydration time. The amount of evaporable water in the pore space can be determined from the magnitude of the NMR signal, and the NMR relaxation times provide a measure of the characteristic pore sizes. Drying studies have been performed to determine the surface spin-spin relaxation time. The NMR results on evolution of cement pore structure with hydration clearly show five different stages. The water consumption was determined to be a linear function of the logarithm of hydration time over a wide range during which the total surface area of the wet gel remains constant. These experiments support a model of capillary and gel pores in the cement paste and provide strong evidence of a stable dense-gel structure. Secondly, supercooling and thawing point depression of confined water has been studied systematically. The depression of the freezing point of liquid water confined within a pore was found to be dependent on the pore size with capillary pore water freezing at 240 K and the remaining gel pore water freezing over a temperature range extending to as low as 160 K. Finally, an important application of NMR has been developed to monitor

  19. Drug-specific [sup 19]F NMR and dynamic [sup 18]F PET imaging of the cytostatic agent 5-fluorouracil

    SciTech Connect

    Bellemann, M.E.; Brix, G.; Haberkorn, U.; Ostertag, H.J.; Lorenz, W.J. )

    1994-12-01

    The spatial distribution of the antineoplastic agent 5-fluorouracil (5-FU) has been mapped both with [sup 19]F NMR and [sup 18]F PET imaging techniques. For [sup 19]F NMR imaging of 5-FU and its major catabolite [alpha]-fluoro-[beta]-alanine (FBAL), a fast gradient-echo pulse sequence was employed. A chemical-shift selective saturation pulse was used to suppress either the 5-FU or the FBAL resonance before the other component of the [sup 19]F NMR spectrum was images. This approach yielded selective 5-FU and FBAL NMR images free of chemical-shift artifacts in readout and slice-selection direction. In phantom experiments, [sup 19]F 5-FU and FBAL images with a spatial resolution of 12.5 x 12.5 x 20 mm[sup 3] were obtained in 32 min from model solutions with drug and catabolite concentrations similar to those estimated in animals and patients undergoing i.v. chemotherapy with 5-FU. The biodistribution of 5-[[sup 18]F]FU in rats shortly after administration of the drug demonstrated the good vascularization of the transplanted tumors. The metabolic turnover of the cytostatic agent started about 10--20 min p.i. and was predominant in the tumor and liver tissue. The rapid adjustment of the [sup 18]F metabolite concentrations in the transplanted tumors to a steady state provides evidence of anabolic tumor activity, which supports the hypothesis of 5-FU trapping in malignant cells based on [sup 19]F NMR spectroscopy data. The high uptake of 5-[[sup 18]F]FU in the liver, on the other hand, mainly reflects the catabolization of 5-FU to the noncytotoxic FBAL, which leads to a reduced bioavailability of the drug.

  20. Impact of Zeolite Transferred from Tank 19F to Tank 18F on DWPF Vitrification of Sludge Batch 3

    SciTech Connect

    Jantzen, C.M.

    2004-01-07

    The Defense Waste Processing Facility (DWPF) is planning to initiate vitrification of Sludge Batch 3 (SB3) in combination with Sludge Batch 2 (SB2) in the spring of 2004. The contents of Sludge Batch 3 will be a mixture of the heel remaining from Sludge Batch 1B, sludge from Tank 7F (containing coal, sand, and sodium oxalate), and sludge materials from Tank 18F. The sludge materials in Tank 18F contain part of a mound of zeolitic material transferred there from Tank 19F. This mound was physically broken up and transfers were made from Tank 19F to Tank 18F for vitrification into SB3. In addition, excess Pu and Am/Cm materials were transferred to Tank 51H to be processed through the DWPF as part of SB3. Additional Pu material and a Np stream from the Canyons are also planned to be added to SB3 before processing of this batch commences at DWPF. The primary objective of this task was to assess the impacts of the excess zeolite mound material in Tank 19F on the predicted glass and processing properties of interest when the zeolite becomes part of SB3. The two potential impacts of the Tank 19F zeolite mound on DWPF processing relates to (1) the samples taken for determination of the acceptability of a macrobatch of DWPF feed and (2) the achievable waste loading. The potential effects of the large size of the zeolite particles found in the Tank 19F solids, as reported in this study, are considered minimal for processing of SB3 in DWPF. Other findings about the zeolite conversion mechanism via a process of Ostwald ripening are discussed in the text and in the conclusions.

  1. First Measurement of the 19F(α, p)22Ne Reaction at Energies of Astrophysical Relevance

    NASA Astrophysics Data System (ADS)

    Pizzone, R. G.; D’Agata, G.; La Cognata, M.; Indelicato, I.; Spitaleri, C.; Blagus, S.; Cherubini, S.; Figuera, P.; Grassi, L.; Guardo, G. L.; Gulino, M.; Hayakawa, S.; Kshetri, R.; Lamia, L.; Lattuada, M.; Mijatović, T.; Milin, M.; Miljanić D., Đ.; Prepolec, L.; Rapisarda, G. G.; Romano, S.; Sergi, M. L.; Skukan, N.; Soić, N.; Tokić, V.; Tumino, A.; Uroić, M.

    2017-02-01

    The observational 19F abundance in stellar environments systematically exceeds the predicted one, thus representing one of the unsolved challenges for stellar modeling. It is therefore clear that further investigation is needed in this field. In this work, we focus our attention on the measurement of the {}19{{F}}{(α ,p)}22{Ne} reaction in the astrophysical energy range, between 0.2 and 0.8 MeV (far below the Coulomb barrier, 3.8 MeV), as it represents the main destruction channel in He-rich environments. The lowest energy at which this reaction has been studied with direct measurements is ∼0.66 MeV, covering only the upper tail of the Gamow window, causing the reaction-rate evaluation to be based on extrapolation. To investigate lower energies, the {}19{{F}}{(α ,p)}22{Ne} reaction has been studied by means of the Trojan horse method, applied to the quasi-free {}6{Li}{{(}19{{F}},{p}22{Ne})}2{{H}} reaction at E beam = 6 MeV. The indirect cross section of the {}19{{F}}{(α ,p)}22{Ne} reaction at energies ≲1 MeV was extracted, fully covering the astrophysical region of interest and overlapping existing direct data for normalization. Several resonances have been detected for the first time inside the Gamow window. The reaction rate has been calculated, showing an increase up to a factor of 4 with respect to the literature at astrophysical temperatures. This might lead to potential major astrophysical implications.

  2. Characterization of solid polymer dispersions of active pharmaceutical ingredients by 19F MAS NMR and factor analysis.

    PubMed

    Urbanova, Martina; Brus, Jiri; Sedenkova, Ivana; Policianova, Olivia; Kobera, Libor

    2013-01-01

    In this contribution the ability of (19)F MAS NMR spectroscopy to probe structural variability of poorly water-soluble drugs formulated as solid dispersions in polymer matrices is discussed. The application potentiality of the proposed approach is demonstrated on a moderately sized active pharmaceutical ingredient (API, Atorvastatin) exhibiting extensive polymorphism. In this respect, a range of model systems with the API incorporated in the matrix of polvinylpyrrolidone (PVP) was prepared. The extent of mixing of both components was determined by T(1)((1)H) and T(1ρ)((1)H) relaxation experiments, and it was found that the API forms nanosized domains. Subsequently it was found out that the polymer matrix induces two kinds of changes in (19)F MAS NMR spectra. At first, this is a high-frequency shift reaching 2-3 ppm which is independent on molecular structure of the API and which results from the long-range polarization of the electron cloud around (19)F nucleus induced by electrostatic fields of the polymer matrix. At second, this is broadening of the signals and formation of shoulders reflecting changes in molecular arrangement of the API. To avoid misleading in the interpretation of the recorded (19)F MAS NMR spectra, because both the contributions act simultaneously, we applied chemometric approach based on multivariate analysis. It is demonstrated that factor analysis of the recorded spectra can separate both these spectral contributions, and the subtle structural differences in the molecular arrangement of the API in the nanosized domains can be traced. In this way (19)F MAS NMR spectra of both pure APIs and APIs in solid dispersions can be directly compared. The proposed strategy thus provides a powerful tool for the analysis of new formulations of fluorinated pharmaceutical substances in polymer matrices.

  3. Characterization of solid polymer dispersions of active pharmaceutical ingredients by 19F MAS NMR and factor analysis

    NASA Astrophysics Data System (ADS)

    Urbanova, Martina; Brus, Jiri; Sedenkova, Ivana; Policianova, Olivia; Kobera, Libor

    In this contribution the ability of 19F MAS NMR spectroscopy to probe structural variability of poorly water-soluble drugs formulated as solid dispersions in polymer matrices is discussed. The application potentiality of the proposed approach is demonstrated on a moderately sized active pharmaceutical ingredient (API, Atorvastatin) exhibiting extensive polymorphism. In this respect, a range of model systems with the API incorporated in the matrix of polvinylpyrrolidone (PVP) was prepared. The extent of mixing of both components was determined by T1(1H) and T1ρ(1H) relaxation experiments, and it was found that the API forms nanosized domains. Subsequently it was found out that the polymer matrix induces two kinds of changes in 19F MAS NMR spectra. At first, this is a high-frequency shift reaching 2-3 ppm which is independent on molecular structure of the API and which results from the long-range polarization of the electron cloud around 19F nucleus induced by electrostatic fields of the polymer matrix. At second, this is broadening of the signals and formation of shoulders reflecting changes in molecular arrangement of the API. To avoid misleading in the interpretation of the recorded 19F MAS NMR spectra, because both the contributions act simultaneously, we applied chemometric approach based on multivariate analysis. It is demonstrated that factor analysis of the recorded spectra can separate both these spectral contributions, and the subtle structural differences in the molecular arrangement of the API in the nanosized domains can be traced. In this way 19F MAS NMR spectra of both pure APIs and APIs in solid dispersions can be directly compared. The proposed strategy thus provides a powerful tool for the analysis of new formulations of fluorinated pharmaceutical substances in polymer matrices.

  4. Optically rewritable patterns of nuclear magnetization in gallium arsenide.

    PubMed

    King, Jonathan P; Li, Yunpu; Meriles, Carlos A; Reimer, Jeffrey A

    2012-06-26

    The control of nuclear spin polarization is important to the design of materials and algorithms for spin-based quantum computing and spintronics. Towards that end, it would be convenient to control the sign and magnitude of nuclear polarization as a function of position within the host lattice. Here we show that, by exploiting different mechanisms for electron-nuclear interaction in the optical pumping process, we are able to control and image the sign of the nuclear polarization as a function of distance from an irradiated GaAs surface. This control is achieved using a crafted combination of light helicity, intensity and wavelength, and is further tuned via use of NMR pulse sequences. These results demonstrate all-optical creation of micron scale, rewritable patterns of positive and negative nuclear polarization in a bulk semiconductor without the need for ferromagnets, lithographic patterning techniques, or quantum-confined structures.

  5. Development of a 700 MHz low-/high- temperature superconductor nuclear magnetic resonance magnet: Test results and spatial homogeneity improvement

    PubMed Central

    Hahn, S.; Bascuñán, J.; Lee, H.; Bobrov, E. S.; Kim, W.; Iwasa, Y.

    2010-01-01

    For the first time in nuclear magnetic resonance (NMR) magnet development, a magnet configuration comprising an insert wound with high-temperature superconductor (HTS) and a background-field magnet wound with low-temperature superconductor (LTS) has been proven viable for NMR magnets. This new LTS/HTS magnet configuration opens the way for development of 1 GHz and above NMR magnets. Specifically, a 700 MHz LTS/HTS NMR magnet (LH700), consisting of a 600 MHz LTS magnet (L600) and a 100 MHz HTS insert (H100), has been designed, built, and successfully tested, and its magnetic field characteristics were measured and analyzed. A field homogeneity of 172 ppm in a cylindrical mapping volume of 17 mm diameter by 30 mm long was measured at 692 MHz and corresponding 1H NMR signal with 1.9 kHz half-width was captured. Two techniques, room-temperature and ferromagnetic shimming, were analytically examined to investigate if they would be effective for further improving spatial field homogeneity of the LH700. PMID:18315337

  6. Development of a 700 MHz low-/high- temperature superconductor nuclear magnetic resonance magnet: test results and spatial homogeneity improvement.

    PubMed

    Hahn, S; Bascuñán, J; Lee, H; Bobrov, E S; Kim, W; Iwasa, Y

    2008-02-01

    For the first time in nuclear magnetic resonance (NMR) magnet development, a magnet configuration comprising an insert wound with high-temperature superconductor (HTS) and a background-field magnet wound with low-temperature superconductor (LTS) has been proven viable for NMR magnets. This new LTS/HTS magnet configuration opens the way for development of 1 GHz and above NMR magnets. Specifically, a 700 MHz LTS/HTS NMR magnet (LH700), consisting of a 600 MHz LTS magnet (L600) and a 100 MHz HTS insert (H100), has been designed, built, and successfully tested, and its magnetic field characteristics were measured and analyzed. A field homogeneity of 172 ppm in a cylindrical mapping volume of 17 mm diameter by 30 mm long was measured at 692 MHz and corresponding 1H NMR signal with 1.9 kHz half-width was captured. Two techniques, room-temperature and ferromagnetic shimming, were analytically examined to investigate if they would be effective for further improving spatial field homogeneity of the LH700.

  7. Phenylboronic acid-based (19)F MRI probe for the detection and imaging of hydrogen peroxide utilizing its large chemical-shift change.

    PubMed

    Nonaka, Hiroshi; An, Qi; Sugihara, Fuminori; Doura, Tomohiro; Tsuchiya, Akira; Yoshioka, Yoshichika; Sando, Shinsuke

    2015-01-01

    Herein, we report on a new (19)F MRI probe for the detection and imaging of H2O2. Our designed 2-fluorophenylboronic acid-based (19)F probe promptly reacted with H2O2 to produce 2-fluorophenol via boronic acid oxidation. The accompanying (19)F chemical-shift change reached 31 ppm under our experimental conditions. Such a large chemical-shift change allowed for the imaging of H2O2 by (19)F chemical-shift-selective MRI.

  8. Solid state nuclear magnetic resonance investigations of advanced energy materials

    NASA Astrophysics Data System (ADS)

    Bennett, George D.

    In order to better understand the physical electrochemical changes that take place in lithium ion batteries and asymmetric hybrid supercapacitors solid state nuclear magnetic resonance (NMR) spectroscopy has been useful to probe and identify changes on the atomic and molecular level. NMR is used to characterize the local environment and investigate the dynamical properties of materials used in electrochemical storage devices (ESD). NMR investigations was used to better understand the chemical composition of the solid electrolyte interphase which form on the negative and positive electrodes of lithium batteries as well as identify the breakdown products that occur in the operation of the asymmetric hybrid supercapacitors. The use of nano-structured particles in the development of new materials causes changes in the electrical, structural and other material properties. NMR was used to investigate the affects of fluorinated and non fluorinated single wall nanotubes (SWNT). In this thesis three experiments were performed using solid state NMR samples to better characterize them. The electrochemical reactions of a lithium ion battery determine its operational profile. Numerous means have been employed to enhance battery cycle life and operating temperature range. One primary means is the choice and makeup of the electrolyte. This study focuses on the characteristics of the solid electrolyte interphase (SEI) that is formed on the electrodes surface during the charge discharge cycle. The electrolyte in this study was altered with several additives in order to determine the influence of the additives on SEI formation as well as the intercalation and de-intercalation of lithium ions in the electrodes. 7Li NMR studies where used to characterize the SEI and its composition. Solid state NMR studies of the carbon enriched acetonitrile electrolyte in a nonaqueous asymmetric hybrid supercapacitor were performed. Magic angle spinning (MAS) coupled with cross polarization NMR

  9. Force-detected nuclear magnetic resonance: recent advances and future challenges.

    PubMed

    Poggio, M; Degen, C L

    2010-08-27

    We review recent efforts to detect small numbers of nuclear spins using magnetic resonance force microscopy. Magnetic resonance force microscopy (MRFM) is a scanning probe technique that relies on the mechanical measurement of the weak magnetic force between a microscopic magnet and the magnetic moments in a sample. Spurred by the recent progress in fabricating ultrasensitive force detectors, MRFM has rapidly improved its capability over the last decade. Today it boasts a spin sensitivity that surpasses conventional, inductive nuclear magnetic resonance detectors by about eight orders of magnitude. In this review we touch on the origins of this technique and focus on its recent application to nanoscale nuclear spin ensembles, in particular on the imaging of nanoscale objects with a three-dimensional (3D) spatial resolution better than 10 nm. We consider the experimental advances driving this work and highlight the underlying physical principles and limitations of the method. Finally, we discuss the challenges that must be met in order to advance the technique towards single nuclear spin sensitivity-and perhaps-to 3D microscopy of molecules with atomic resolution.

  10. Non-invasive imaging of transplanted human neural stem cells and ECM scaffold remodeling in the stroke-damaged rat brain by 19F- and diffusion-MRI

    PubMed Central

    Bible, Ellen; Dell’Acqua, Flavio; Solanky, Bhavana; Balducci, Anthony; Crapo, Peter; Badylak, Stephen F.; Ahrens, Eric T.; Modo, Michel

    2012-01-01

    Transplantation of human neural stem cells (hNSCs) is emerging as a viable treatment for stroke related brain injury. However, intraparenchymal grafts do not regenerate lost tissue, but rather integrate into the host parenchyma without significantly affecting the lesion cavity. Providing a structural support for the delivered cells appears important for cell based therapeutic approaches. The non-invasive monitoring of therapeutic methods would provide valuable information regarding therapeutic strategies but remains a challenge. Labeling transplanted cells with metal-based 1H-magnetic resonance imaging (MRI) contrast agents affects the visualization of the lesion cavity. Herein, we demonstrate that a 19F-MRI contrast agent can adequately monitor the distribution of transplanted cells, whilst allowing an evaluation of the lesion cavity and the formation of new tissue on 1H-MRI scans. Twenty percent of cells labeled with the 19F-agent were of host origin, potentially reflecting the re-uptake of label from dead transplanted cells. Both T2- and diffusion-weighted MRI scans indicated that transplantation of hNSCs suspended in a gel form of a xenogeneic extracellular matrix (ECM) bioscaffold resulted in uniformly distributed cells throughout the lesion cavity. However, diffusion MRI indicated that the injected materials did not yet establish diffusion barriers (i.e. cellular network, fiber tracts) normally found within striatal tissue. The ECM bioscaffold therefore provides an important support to hNSCs for the creation of de novo tissue and multi-nuclei MRI represents an adept method for the visualization of some aspects of this process. However, significant developments of both the transplantation paradigm, as well as regenerative imaging, are required to successfully create new tissue in the lesion cavity and to monitor this process non-invasively. PMID:22244696

  11. Orientation of the antimicrobial peptide PGLa in lipid membranes determined from 19F-NMR dipolar couplings of 4-CF3-phenylglycine labels.

    PubMed

    Glaser, Ralf W; Sachse, Carsten; Dürr, Ulrich H N; Wadhwani, Parvesh; Ulrich, Anne S

    2004-05-01

    A highly sensitive solid state (19)F-NMR strategy is described to determine the orientation and dynamics of membrane-associated peptides from specific fluorine labels. Several analogues of the antimicrobial peptide PGLa were synthesized with the non-natural amino acid 4-trifluoromethyl-phenylglycine (CF(3)-Phg) at different positions throughout the alpha-helical peptide chain. A simple 1-pulse (19)F experiment allows the simultaneous measurement of both the anisotropic chemical shift and the homonuclear dipolar coupling within the rotating CF(3)-group in a macroscopically oriented membrane sample. The value and sign of the dipolar splitting determines the tilt of the CF(3)-rotational axis, which is rigidly attached to the peptide backbone, with respect to the external magnetic field direction. Using four CF(3)-labeled peptide analogues (with L-CF(3)-Phg at Ile9, Ala10, Ile13, and Ala14) we confirmed that PGLa is aligned at the surface of lipid membranes with its helix axis perpendicular to the bilayer normal at a peptide:lipid ratio of 1:200. We also determined the azimuthal rotation angle of the helix, which agrees well with the orientation expected from its amphiphilic character. Peptide analogues with a D-CF(3)-Phg label resulting from racemization of the amino acid during synthesis were separately collected by HPLC. Their spectra provide additional information about the PGLa structure and orientation but allow only to discriminate qualitatively between multiple solutions. The structural and functional characterization of the individual CF(3)-labeled peptides by circular dichroism and antimicrobial assays showed only small effects for our four substitutions on the hydrophobic face of the helix, but a significant disturbance was observed in a fifth analogue where Ala8 on the hydrophilic face had been replaced. Even though the hydrophobic CF(3)-Phg side chain cannot be utilized in all positions, it allows highly sensitive NMR measurements over a wide range of

  12. Radiofrequency Coil Designs For Nuclear Magnetic Resonance Zeuciviatographic Imaging

    NASA Astrophysics Data System (ADS)

    Bernardo, M. L.; Cohen, A. J.; Lauterbur, P. C.

    1982-11-01

    The requirements for spatial uniformity of the radio-frequency magnetic field used in three-dimensional MAR imaging are discussed and an improved winding distribution for a saddle-shaped single transmitter-receiver coil has been developed and tested by computer simulation of the rf mag-netic field pattern. The use of flat local or "surface" coils for NMR imaging is also proposed. A. method for correcting such images for the apparent spin density differences caused by the extreme rf magnetic field nonuniformity has been developed and tested with phantoms and images of the human back.

  13. Fluorinated Amino-Derivatives of the Sesquiterpene Lactone, Parthenolide, as 19F NMR Probes in Deuterium-Free Environments

    PubMed Central

    Woods, James R.; Mo, Huaping; Bieberich, Andrew A.; Alavanja, Tanja; Colby, David A.

    2011-01-01

    The design, synthesis, and biological activity of fluorinated amino-derivatives of the sesquiterpene lactone, parthenolide, are described. A fluorinated aminoparthenolide analogue with biological activity similar to the parent natural product was discovered, and its X-ray structure was obtained. This lead compound was then studied using 19F NMR in the presence and absence of glutathione to obtain additional mechanism of action data, and it was found that the aminoparthenolide eliminates amine faster in the presence of glutathione than in the absence of glutathione. The exact changes in concentrations of fluorinated compound and amine were quantified by a concentration-reference method using 19F NMR; a major benefit of applying this strategy is that no deuterated solvents or internal standards are required to obtain accurate concentrations. These mechanistic data with glutathione may contribute to the conversion of the amino-derivative to parthenolide, the active pharmacological agent, in glutathione-rich cancer cells. PMID:22029741

  14. Nuclear resonance reflection of synchrotron radiation from thin dysprosium films with different types of magnetic ordering

    NASA Astrophysics Data System (ADS)

    Andreeva, M. A.; Antropov, N. O.; Baulin, R. A.; Kravtsov, E. A.; Ryabukhina, M. V.; Yakunina, E. M.; Ustinov, V. V.

    2016-12-01

    Epitaxial thin films of dysprosium have been successfully synthesized by the method of high-vacuum magnetron sputtering and their structure and magnetic properties have been investigated. The opportunity of the nuclear resonance scattering for the investigation of nanostructures containing 161Dy has been considered; the specific features of the spectra of nuclear resonance reflectivity from the films have been analyzed on the energy and time scales at different orientations of the magnetic hyperfine field. The simulation of the angular dependences of nuclear resonance reflectivity for the case of spiral ordering in periodic structures containing 161Dy has been carried out. It has been shown that these dependences make it possible to uniquely determine the period of magnetic ordering.

  15. Nuclear magnetic resonance detection and spectroscopy of single proteins using quantum logic.

    PubMed

    Lovchinsky, I; Sushkov, A O; Urbach, E; de Leon, N P; Choi, S; De Greve, K; Evans, R; Gertner, R; Bersin, E; Müller, C; McGuinness, L; Jelezko, F; Walsworth, R L; Park, H; Lukin, M D

    2016-02-19

    Nuclear magnetic resonance spectroscopy is a powerful tool for the structural analysis of organic compounds and biomolecules but typically requires macroscopic sample quantities. We use a sensor, which consists of two quantum bits corresponding to an electronic spin and an ancillary nuclear spin, to demonstrate room temperature magnetic resonance detection and spectroscopy of multiple nuclear species within individual ubiquitin proteins attached to the diamond surface. Using quantum logic to improve readout fidelity and a surface-treatment technique to extend the spin coherence time of shallow nitrogen-vacancy centers, we demonstrate magnetic field sensitivity sufficient to detect individual proton spins within 1 second of integration. This gain in sensitivity enables high-confidence detection of individual proteins and allows us to observe spectral features that reveal information about their chemical composition.

  16. Characteristics of spectrum registration of condensed medium by the method of nuclear-magnetic resonance in a weak field

    NASA Astrophysics Data System (ADS)

    Davydov, V. V.; Myazin, N. S.; Velichko, E. N.

    2017-07-01

    The characteristics of signal registration of nuclear-magnetic resonance in a weak magnetic field from a small volume of an investigated medium have been considered. The consideration of the characteristics revealed in a new developed design of a magnetic system for a compact nuclear-magnetic spectrometer, and also in the NMR-signal registration method allows significant extension of the possibility to use the phenomenon of nuclear-magnetic resonance for the study of condensed medium in an express mode. The experimental results of different media studies have been presented.

  17. Method of Continuous Variation: Characterization of Alkali Metal Enolates Using 1H and 19F NMR Spectroscopies

    PubMed Central

    2015-01-01

    The method of continuous variation in conjunction with 1H and 19F NMR spectroscopies was used to characterize lithium and sodium enolates solvated by N,N,N′,N′-tetramethylethyldiamine (TMEDA) and tetrahydrofuran (THF). A strategy developed using lithium enolates was then applied to the more challenging sodium enolates. A number of sodium enolates solvated by TMEDA or THF afford exclusively tetramers. Evidence suggests that TMEDA chelates sodium on cubic tetramers. PMID:24915602

  18. Orientation of fluorinated cholesterol in lipid bilayers analyzed by 19F tensor calculation and solid-state NMR.

    PubMed

    Matsumori, Nobuaki; Kasai, Yusuke; Oishi, Tohru; Murata, Michio; Nomura, Kaoru

    2008-04-09

    6-F-cholesterol was reported to exhibit biological and interfacial properties similar to unmodified cholesterol. We have also found that 6-F-cholesterol mimicked the cholesterol activity observed in the systems of amphotericin B and lipid rafts. However, to use 6-F-cholesterol as a molecular probe to explore molecular recognition in membranes, it is indispensable to have detailed knowledge of the dynamic and orientation properties of the molecule in membrane environments. In this paper, we present the molecular orientation of 6-F-cholesterol (30 mol %) in dimyristoylphosphatidylcholine (DMPC) bilayers revealed by combined use of 19F chemical shift anisotropy (CSA), 2H NMR, and C-F rotational echo double resonance (REDOR) experiments. The axis of rotation of 6-F-cholesterol was shown to be in a similar direction to that of cholesterol in DMPC bilayers, which is almost parallel to the long axis of the molecular frame. The molecular order parameter of 6-F-cholesterol was determined to be ca. 0.85, which is within the range of reported values of cholesterol. These findings suggest that the dynamic properties of 6-F-cholesterol in DMPC are quite similar to those of unmodified cholesterol; therefore, the introduction of a fluorine atom at C6 has virtually no effect on cholesterol dynamics in membranes. In addition, this study demonstrates the practical utility of theoretical calculations for determining the 19F CSA principal axes, which would be extremely difficult to obtain experimentally. The combined use of quantum calculations and solid-state 19F NMR will make it possible to apply the orientation information of 19F CSA tensors to membrane systems.

  19. Solubilization of flurbiprofen within non-ionic Tween 20 surfactant micelles: a 19F and 1H NMR study.

    PubMed

    Saveyn, Pieter; Cocquyt, Ellen; Zhu, Wuxin; Sinnaeve, Davy; Haustraete, Katrien; Martins, José C; Van der Meeren, Paul

    2009-07-14

    The solubilization of the poorly water soluble anti-inflammatory drug flurbiprofen in non-ionic Tween 20 surfactant micellar solutions was studied by both (19)F and (1)H NMR spectroscopy in an acidic environment. These non-destructive techniques allowed us to investigate the effect of temperature cycling in situ. Using (19)F NMR, an increased solubilisation capacity was observed as the temperature increased. This effect became more pronounced above the cloud point, which was reduced by more than 30 degrees C in the presence of an excess of flurbiprofen. Upon clouding, peak splitting was observed in the (19)F spectrum, which indicates that two pools of solubilised flurbiprofen exist that are in slow exchange on the NMR frequency timescale. The clouding and solubilization processes were found to be reversible, albeit with slow kinetics. Based on chemical shift differences of both Tween 20 and flurbiprofen, as well as NOESY experiments, the flurbiprofen was found to be accumulated within the palisade layer of the Tween 20 micelles.

  20. Multimodal Perfluorocarbon Nanoemulsions for 19F MRI, Ultrasonography, and Catalysis of MRgFUS-Mediated Drug Delivery

    NASA Astrophysics Data System (ADS)

    Rapoport, N.; Nam, K.-H.; Christensen, D. A.; Kennedy, A. M.; Parker, D. L.; Payne, A. H.; Todd, N.; Shea, J. E.; Scaife, C. L.

    2011-09-01

    Perfluorocarbon nanoemulsions can target lipophilic therapeutic agents to solid tumors and simultaneously provide for monitoring nanocarrier biodistribution via ultrasonography and/or 19F MRI. In the first generation of block copolymer stabilized perfluorocarbon nanoemulsions, perfluoropentane (PFP) was used as the droplet forming compound. Although manifesting excellent therapeutic and ultrasound imaging properties, PFP nanoemulsions were unstable at storage, difficult to handle, and underwent droplet-to-bubble transition upon injection that was hard to control. To solve the above problems, perfluoro-15-crown-5-ether (PFCE) was used as a core forming compound in the second generation of block copolymer stabilized perfluorocarbon nanoemulsions. In the present paper, acoustic, imaging, and therapeutic properties of unloaded and paclitaxel (PTX) loaded PFCE nanoemulsions are reported. The size of paclitaxel-loaded PFCE nanodroplets (300 nm to 500 nm depending on emulsification conditions) favors their passive accumulation in tumor tissue. PFCE nanodroplets manifest both ultrasound and 19F MR contrast properties, which allows the use of multimodal imaging to monitor nanodroplet biodistribution. Ultrasonography and 19F MRI produced consistent results on nanodroplet biodistribution. Sonication with 1-MHz therapeutic ultrasound triggered reversible droplet-to-bubble transition in PFCE nanoemulsions. Microbubbles formed by acoustic vaporization underwent stable cavitation. In a pilot study on ultrasound-mediated therapy of a large breast cancer tumor, paclitaxel-loaded PFCE nanoemulsions combined with 1-MHz ultrasound (MI≥1.75) showed excellent therapeutic properties. Anticipated mechanisms of the observed effects are discussed.

  1. Catalysis of nuclear reactions in hydrogen in a strong magnetic field

    NASA Astrophysics Data System (ADS)

    Khersonskii, V. K.

    1986-10-01

    Calculations are made of the probabilities of nuclear reactions in HD(+), D2(+), and DT(+) molecular ions in a strong magnetic field. It is shown, that as the field intensity increases from 10 to the 12th to 10 to the 13 G, the probabilities of the nuclear reactions increase by ten orders of magnitude. The calculations allow for the effect of the vibrational-rotational state of the molecules on the reaction probabilities.

  2. Diamond-nitrogen-vacancy electronic and nuclear spin-state anticrossings under weak transverse magnetic fields

    NASA Astrophysics Data System (ADS)

    Clevenson, Hannah; Chen, Edward H.; Dolde, Florian; Teale, Carson; Englund, Dirk; Braje, Danielle

    2016-08-01

    We report on detailed studies of electronic and nuclear spin states in the diamond-nitrogen-vacancy (NV) center under weak transverse magnetic fields. We numerically predict and experimentally verify a previously unobserved NV hyperfine level anticrossing (LAC) occurring at bias fields of tens of gauss—two orders of magnitude lower than previously reported LACs at ˜500 and ˜1000 G axial magnetic fields. We then discuss how the NV ground-state Hamiltonian can be manipulated in this regime to tailor the NV's sensitivity to environmental factors and to map into the nuclear spin state.

  3. Nuclear magnetic resonance micro-imaging in the investigation of plant cell metabolism.

    PubMed

    Köckenberger, W

    2001-04-01

    Micro-imaging based on nuclear magnetic resonance offers the possibility to map metabolites in plant tissues non-invasively. Major metabolites such as sucrose and amino acids can be observed with high spatial resolution. Stable isotope tracers, such as (13)C-labelled metabolites can be used to measure the in vivo conversion rates in a metabolic network. This review summarizes the different nuclear magnetic resonance micro-imaging techniques that are available to obtain spatially resolved information on metabolites in plants. A short general introduction into NMR imaging techniques is provided. Particular emphasis is given to the difficulties encountered when NMR micro-imaging is applied to plant systems.

  4. Anomalous hyperfine coupling and nuclear magnetic relaxation in Weyl semimetals

    NASA Astrophysics Data System (ADS)

    Okvátovity, Zoltán; Simon, Ferenc; Dóra, Balázs

    2016-12-01

    The electron-nuclear hyperfine interaction shows up in a variety of phenomena including, e.g., NMR studies of correlated states and spin decoherence effects in quantum dots. Here we focus on the hyperfine coupling and the NMR spin relaxation time T1 in Weyl semimetals. Since the density of states in Weyl semimetals varies with the square of the energy around the Weyl point, a naive power counting predicts a 1 /T1T ˜E4 scaling, with E the maximum of temperature (T ) and chemical potential. By carefully investigating the hyperfine interaction between nuclear spins and Weyl fermions, we find that while its spin part behaves conventionally, its orbital part diverges unusually, with the inverse of the energy around the Weyl point. Consequently, the nuclear spin relaxation rate scales in a graphenelike manner as 1 /T1T ˜E2ln(E /ω0) , with ω0 the nuclear Larmor frequency. This allows us to identify an effective hyperfine coupling constant, which is tunable by gating or doping. This is relevant for the decoherence effect in spintronics devices and double quantum dots, where hyperfine coupling is the dominant source of spin-blockade lifting.

  5. Hybrid quantum magnetic-field sensor with an electron spin and a nuclear spin in diamond

    NASA Astrophysics Data System (ADS)

    Matsuzaki, Yuichiro; Shimo-Oka, Takaaki; Tanaka, Hirotaka; Tokura, Yasuhiro; Semba, Kouichi; Mizuochi, Norikazu

    2016-11-01

    Recently, magnetic-field sensors based on an electron spin of a nitrogen vacancy center in diamond have been studied both from an experimental and theoretical point of view. This system provides a nanoscale magnetometer, and it is possible to detect a precession of a single spin. In this paper, we propose a sensor consisting of an electron spin and a nuclear spin in diamond. Although the electron spin has a reasonable interaction strength with magnetic field, the coherence time of the spin is relatively short. On the other hand, the nuclear spin has a longer lifetime while the spin has a negligible interaction with magnetic fields. We show that, through the combination of such two different spins via the hyperfine interaction, it is possible to construct a magnetic-field sensor with the sensitivity far beyond that of previous sensors using just a single electron spin.

  6. Nuclear magnetic resonance apparatus having semitoroidal rf coil for use in topical NMR and NMR imaging

    DOEpatents

    Fukushima, Eiichi; Roeder, Stephen B. W.; Assink, Roger A.; Gibson, Atholl A. V.

    1986-01-01

    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, so as to enable NMR measurements to be taken from selected regions inside an object, particularly including 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 interaction of the electric field with the sample.

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

    PubMed

    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.

  8. Zero and Ultra-Low-Field Nuclear Magnetic Resonance Spectroscopy Via Optical Magnetometry

    NASA Astrophysics Data System (ADS)

    Blanchard, John Woodland

    Nuclear magnetic resonance (NMR) is among the most powerful analytical tools available to the chemical and biological sciences for chemical detection, characterization, and structure elucidation. NMR experiments are usually performed in large magnetic fields in order to maximize sensitivity and increase chemical shift resolution. However, the high magnetic fields required for conventional NMR necessitate large, immobile, and expensive superconducting magnets, limiting the use of the technique. New hyperpolarization and non-inductive detection methods have recently allowed for NMR measurements in the inverse regime of extremely low magnetic fields. Whereas a substantial body of research has been conducted in the high-field regime, taking advantage of the efficient coherent control afforded by a spectroscopy dominated by coupling to the spectrometer, the zero- and ultra-low-field (ZULF) regime has remained mostly unexplored. In this dissertation, we investigate the applicability of ZULF-NMR as a novel spectroscopic technique complimentary to high-field NMR. In particular, we consider various aspects of the ZULF-NMR experiment and the dynamics of nuclear spins under various local spin coupling Hamiltonians. We first survey zero-field NMR experiments on systems dominated by the electron-mediated indirect spin-spin coupling (J-coupling). The resulting J-spectra permit precision measurement of chemically relevant information due to the exquisite sensitivity of J-couplings to subtle changes in molecular geometry and electronic structure. We also consider the effects of weak magnetic fields and residual dipolar couplings in anisotropic media, which encode information about nuclear magnetic moments and geometry, and further resolve topological ambiguities by lifting degeneracies. By extending the understanding of the interactions that contribute to ZULF-NMR spectra, this work represents a significant advancement towards a complete description of zero- and ultra

  9. Nuclear magnetic resonance in sedimentary rocks: Effect of proton desorption rate

    NASA Astrophysics Data System (ADS)

    Mendelson, Kenneth S.

    1982-09-01

    In a discussion of nuclear magnetic resonance of protons in the pore fluid of sedimentary rocks, Cohen and Mendelson assumed that the desorption rate of protons from the rock surface is much faster than the relaxation rate of the magnetization for protons on the surface. In the present paper it is shown that this assumption is not necessary and conditions are established under which the analysis of Cohen and Mendelson is valid.

  10. Nuclear Magnetic Resonance Signature of the Spin-Nematic Phase in LiCuVO4 at High Magnetic Fields

    NASA Astrophysics Data System (ADS)

    Orlova, A.; Green, E. L.; Law, J. M.; Gorbunov, D. I.; Chanda, G.; Krämer, S.; Horvatić, M.; Kremer, R. K.; Wosnitza, J.; Rikken, G. L. J. A.

    2017-06-01

    We report a V 51 nuclear magnetic resonance investigation of the frustrated spin-1 /2 chain compound LiCuVO4 , performed in pulsed magnetic fields and focused on high-field phases up to 56 T. For the crystal orientations H ∥c and H ∥b , we find a narrow field region just below the magnetic saturation where the local magnetization remains uniform and homogeneous, while its value is field dependent. This behavior is the first microscopic signature of the spin-nematic state, breaking spin-rotation symmetry without generating any transverse dipolar order, and is consistent with theoretical predictions for the LiCuVO4 compound.

  11. Design and development of a novel nuclear magnetic resonance detection for the gas phase ions by magnetic resonance acceleration technique

    NASA Astrophysics Data System (ADS)

    Fuke, K.; Tona, M.; Fujihara, A.; Sakurai, M.; Ishikawa, H.

    2012-08-01

    Nuclear magnetic resonance (NMR) technique is a well-established powerful tool to study the physical and chemical properties of a wide range of materials. However, presently, NMR applications are essentially limited to materials in the condensed phase. Although magnetic resonance was originally demonstrated in gas phase molecular beam experiments, no application to gas phase molecular ions has yet been demonstrated. Here, we present a novel principle of NMR detection for gas phase ions based on a "magnetic resonance acceleration" technique and describe the design and construction of an apparatus which we are developing. We also present an experimental technique and some results on the formation and manipulation of cold ion packets in a strong magnetic field, which are the key innovations to detect NMR signal using the present method. We expect this novel method to lead new realm for the study of mass-selected gas-phase ions with interesting applications in both fundamental and applied sciences.

  12. Nuclear magnetic resonance linewidth and spin diffusion in {sup 29}Si isotopically controlled silicon

    SciTech Connect

    Hayashi, Hiroshi; Itoh, Kohei M.; Vlasenko, Leonid S.

    2008-10-15

    A nuclear magnetic resonance (NMR) study was performed with n-type silicon single crystals containing {sup 29}Si isotope abundance f ranges from 1.2% to 99.2%. The nuclear spin diffusion coefficient D has been determined from the linewidth of significantly enhanced {sup 29}Si NMR signals utilizing a developed dynamic nuclear polarization (DNP) method. The {sup 29}Si NMR linewidth depends linearly on f, at least when f<10%, and approaches {proportional_to}f{sup 1/2} dependence when f>50%. The estimated {sup 29}Si nuclear spin diffusion time T{sub sd} between phosphorus atoms used for DNP is more than ten times shorter than the nuclear polarization time T{sub 1}{sup p} of {sup 29}Si nuclei around phosphorus. Therefore, the regime of 'rapid spin diffusion' is realized in the DNP experiments.

  13. Manipulation of the nuclear spin ensemble in a quantum dot with chirped magnetic resonance pulses.

    PubMed

    Munsch, Mathieu; Wüst, Gunter; Kuhlmann, Andreas V; Xue, Fei; Ludwig, Arne; Reuter, Dirk; Wieck, Andreas D; Poggio, Martino; Warburton, Richard J

    2014-09-01

    The nuclear spins in nanostructured semiconductors play a central role in quantum applications. The nuclear spins represent a useful resource for generating local magnetic fields but nuclear spin noise represents a major source of dephasing for spin qubits. Controlling the nuclear spins enhances the resource while suppressing the noise. NMR techniques are challenging: the group III and V isotopes have large spins with widely different gyromagnetic ratios; in strained material there are large atom-dependent quadrupole shifts; and nanoscale NMR is hard to detect. We report NMR on 100,000 nuclear spins of a quantum dot using chirped radiofrequency pulses. Following polarization, we demonstrate a reversal of the nuclear spin. We can flip the nuclear spin back and forth a hundred times. We demonstrate that chirped NMR is a powerful way of determining the chemical composition, the initial nuclear spin temperatures and quadrupole frequency distributions for all the main isotopes. The key observation is a plateau in the NMR signal as a function of sweep rate: we achieve inversion at the first quantum transition for all isotopes simultaneously. These experiments represent a generic technique for manipulating nanoscale inhomogeneous nuclear spin ensembles and open the way to probe the coherence of such mesoscopic systems.

  14. Dynamical in situ nuclear-magnetic-resonance tensile apparatus

    NASA Astrophysics Data System (ADS)

    Hackelöer, H. J.; Kanert, O.; Tamler, H.; De Hosson, J. Th. M.

    1983-03-01

    A combination of a servohydraulic tensile machine and NMR pulse spectrometer is described enabling nuclear-spin relaxation rates to be recorded simultaneously with stress-strain data incorporating tension as well as compression of nonmetallic as well as of metallic samples. The data of the mechanical system are as follows: Maximum load: 5000 N; minimum deformation speed: 10 μm s-1, maximum deformation speed: 3×105 μm s-1; deformation stroke: digitally controlled between 1 and 8×103 μm; bandwidth: dc to 1 kHz; resolution: 2-4 μm; temperature conditions of the sample: from 80 to 570 K. The operation and performance of the system is described by means of experiments observing nuclear-spin relaxation rates which are induced by the movement of dislocations due to the finite deformation rate of the sample.

  15. Low Field Nuclear Magnetic Resonance (NMR) using SQUIDs

    NASA Astrophysics Data System (ADS)

    Burghoff, Martin

    2007-03-01

    Using a high resolution SQUID system in a magnetically highly shielded room, we measured the precession of 1H nuclei of liquid benzene, distilled water, and chloroform in magnetic fields around a microTesla. We found that the NMR lines of these liquids are in the range of a few hundred milliHertz and increase linearly with the detection field over a Larmor frequency range of two orders of magnitude. The slope is attributed to the inhomogeneity of the detection field and enables the extrapolation of the natural line width to zero magnetic field. For this limit, where any molecular motion is fast with respect to the Larmor frequency, the natural resonance line widths of benzene, chloroform and distilled water were determined to be 120 mHz, 150 mHz, and 170 mHz, respectively. In low magnetic fields, chemical shift and homonuclear coupling become negligible. All that remains as a source of a spectral structure is pure J-coupling between nuclei of different gyromagnetic ratio. We studied pure J-coupling between methylene protons and fluorine nuclei of trifluorethanol and between methyl protons and phosphorus in trimethylphosphate at detection fields from 0.5 microTesla to 4 microTesla. This corresponds to a variation of d=J(H,F)/(f(H)-f(F)) from 8 to 1 and of d=J(H,P)/(f(H)-f(P)) from 0.8 to 0.08, respectively. At very low fields, i.e. at d=8, the spectra of trifluorethanol exhibited only one single resonance line with an irregular structure. With increasing field, more and more individual lines were revealed. For trimethylphosphate, d=0.08 represents the transition to the weak coupling regime. In addition, we employed a 304 SQUID vector magnetometer system for the recording of the magnetic field generated by water protons in two adjacent sample tubes precessing about a magnetic field of a microTesla. From the spatially resolved data, positions and moments of the samples were calculated, yielding a reconstructed moving image of the two precessing magnetic dipoles.

  16. Nuclear magnetic resonance multiwindow analysis of proton local fields and magnetization distribution in natural and deuterated mouse muscle.

    PubMed Central

    Peemoeller, H; Pintar, M M

    1979-01-01

    The proton free-induction decays, spin-spin relaxation times, local fields in the rotating frame, and spin-lattice relaxation times in the laboratory and rotating frames, in natural and fully deuterated mouse muscle, are reported. Measurements were taken above and below freezing temperature and at two time windows on the free-induction decay. A comparative analysis show that the magnetization fractions deduced from the different experiments are in good agreement. The main conclusion is that the resolution of the (heterogeneous) muscle nuclear magnetic resonance (NMR) response is improved by the multiwindow analysis. PMID:262554

  17. The effects of nuclear magnetic resonance on patients with cardiac pacemakers

    SciTech Connect

    Pavlicek, W.; Geisinger, M.; Castle, L.; Borkowski, G.P.; Meaney, T.F.; Bream, B.L.; Gallagher, J.H.

    1983-04-01

    The effect of nuclear magnetic resonance (NMR) imaging on six representative cardiac pacemakers was studied. The results indicate that the threshold for initiating the asynchronous mode of a pacemaker is 17 gauss. Radiofrequency levels are present in an NMR unit and may confuse or possibly inhibit demand pacemakers, although sensing circuitry is normally provided with electromagnetic interference discrimination. Time-varying magnetic fields can generate pulse amplitudes and frequencies to mimic cardiac activity. A serious limitation in the possibility of imaging a patient with a pacemaker would be the alteration of normal pulsing parameters due to time-varying magnetic fields.

  18. Exact two-component relativistic theory for nuclear magnetic resonance parameters.

    PubMed

    Sun, Qiming; Liu, Wenjian; Xiao, Yunlong; Cheng, Lan

    2009-08-28

    An exact two-component (X2C) relativistic theory for nuclear magnetic resonance parameters is obtained by first a single block-diagonalization of the matrix representation of the Dirac operator in a magnetic-field-dependent basis and then a magnetic perturbation expansion of the resultant two-component Hamiltonian and transformation matrices. Such a matrix formulation is not only simple but also general in the sense that the various ways of incorporating the field dependence can be treated in a unified manner. The X2C dia- and paramagnetic terms agree individually with the corresponding four-component ones up to machine accuracy for any basis.

  19. Nuclear conversion theory: molecular hydrogen in non-magnetic insulators

    PubMed Central

    Ghiglieno, Filippo

    2016-01-01

    The hydrogen conversion patterns on non-magnetic solids sensitively depend upon the degree of singlet/triplet mixing in the intermediates of the catalytic reaction. Three main ‘symmetry-breaking’ interactions are brought together. In a typical channel, the electron spin–orbit (SO) couplings introduce some magnetic excitations in the non-magnetic solid ground state. The electron spin is exchanged with a molecular one by the electric molecule–solid electron repulsion, mixing the bonding and antibonding states and affecting the molecule rotation. Finally, the magnetic hyperfine contact transfers the electron spin angular momentum to the nuclei. Two families of channels are considered and a simple criterion based on the SO coupling strength is proposed to select the most efficient one. The denoted ‘electronic’ conversion path involves an emission of excitons that propagate and disintegrate in the bulk. In the other denoted ‘nuclear’, the excited electron states are transients of a loop, and the electron system returns to its fundamental ground state. The described model enlarges previous studies by extending the electron basis to charge-transfer states and ‘continui’ of band states, and focuses on the broadening of the antibonding molecular excited state by the solid conduction band that provides efficient tunnelling paths for the hydrogen conversion. After working out the general conversion algebra, the conversion rates of hydrogen on insulating and semiconductor solids are related to a few molecule–solid parameters (gap width, ionization and affinity potentials) and compared with experimental measures. PMID:27703681

  20. The Complexation of the Na(super +) by 18-Crown-6 Studied via Nuclear Magnetic Resonance

    ERIC Educational Resources Information Center

    Peters, Steven J.; Stevenson, Cheryl D.

    2004-01-01

    A student friendly experiment that teaches several important concepts of modern nuclear magnetic resonance (NMR), like multinuclear capabilities, the NMR time scale, and time-averaged signals, is described along with some important concepts of thermo chemical equilibria. The mentioned experiment involves safe and inexpensive compounds, such as…

  1. Analyses of cocondensation of melamine and urea through formaldehyde with carbon 13 nuclear magnetic resonance spectroscopy

    Treesearch

    Tomita Bunchiro; Chung-Yun Hse

    1995-01-01

    The 13C-NMR (carbon 13 nuclear magnetic resonance) spectra of urea-formaldehyde (UF) resins, melamine-formaldehyde (MF) resins, and melamine-urea-formaldehyde (MUF) cocondensed resins synthesized under various conditions were taken with a frequency of 75 MHz. The main purpose was to investigate whether or not the occurrences of cocondensation...

  2. Analysis of cocondensation of melamine and urea through formaldehyde with carbon 13 nuclear magnetic resonance spectroscopy

    Treesearch

    Bunichiro Tomita; Chung-Yun Hse

    1995-01-01

    The 13C-NMR (carbon 13 nuclear magnetic resonance) spectra of urea-formaldehyde (UF) resins, melamine-formaldehyde (MF) resins, and melamine-urea-formaldehyde (MUF) cocondensed resins synthesized under various conditions were taken with a frequency of 75 MHz. The main purpose was to investigate whether or not the occurrences of cocondensation...

  3. An Accessible Two-Dimensional Solution Nuclear Magnetic Resonance Experiment on Human Ubiquitin

    ERIC Educational Resources Information Center

    Rovnyak, David; Thompson, Laura E.

    2005-01-01

    Solution-state nuclear magnetic resonance (NMR) is an invaluable tool in structural and molecular biology research, but may be underutilized in undergraduate laboratories because instrumentation for performing structural studies of macromolecules in aqueous solutions is not yet widely available for use in undergraduate laboratories. We have…

  4. MEMS-based force-detected nuclear magnetic resonance spectrometer for in situ planetary exploration

    NASA Technical Reports Server (NTRS)

    George, T.; Leskowitz, G.; Madsen, L.; Weitekamp, D.; Tang, W.

    2000-01-01

    Nuclear Magnetic resonance (NMR) is a well-known spectroscopic technique used by chemists and is especially powerful in detecting the presence of water and distinguishing between arbitrary physisorbed and chemisorbed states. This ability is of particular importance in the search for extra-terrestrial life on planets such as Mars.

  5. Quantitative Analysis of Nail Polish Remover Using Nuclear Magnetic Resonance Spectroscopy Revisited

    ERIC Educational Resources Information Center

    Hoffmann, Markus M.; Caccamis, Joshua T.; Heitz, Mark P.; Schlecht, Kenneth D.

    2008-01-01

    Substantial modifications are presented for a previously described experiment using nuclear magnetic resonance (NMR) spectroscopy to quantitatively determine analytes in commercial nail polish remover. The revised experiment is intended for a second- or third-year laboratory course in analytical chemistry and can be conducted for larger laboratory…

  6. Quantitative nuclear magnetic resonance to measure body composition in infants and children

    USDA-ARS?s Scientific Manuscript database

    Quantitative Nuclear Magnetic Resonance (QMR) is being used in human adults to obtain measures of total body fat (FM) with high precision. The current study assessed a device specially designed to accommodate infants and children between 3 and 50 kg (EchoMRI-AH™). Body composition of 113 infants and...

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

    SciTech Connect

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

    2016-06-14

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

  8. An Accessible Two-Dimensional Solution Nuclear Magnetic Resonance Experiment on Human Ubiquitin

    ERIC Educational Resources Information Center

    Rovnyak, David; Thompson, Laura E.

    2005-01-01

    Solution-state nuclear magnetic resonance (NMR) is an invaluable tool in structural and molecular biology research, but may be underutilized in undergraduate laboratories because instrumentation for performing structural studies of macromolecules in aqueous solutions is not yet widely available for use in undergraduate laboratories. We have…

  9. Structural Isomer Identification via NMR: A Nuclear Magnetic Resonance Experiment for Organic, Analytical, or Physical Chemistry.

    ERIC Educational Resources Information Center

    Szafran, Zvi

    1985-01-01

    Background information, procedures used, and typical results obtained are provided for an experiment that examines the ability of nuclear magnetic resonance (NMR) to distinguish between structural isomers via resonance multiplicities and chemical shifts. Reasons for incorporating the experiment into organic, analytical, or physical chemistry…

  10. Hepatic Metabolism of Perfluorinated Carboxylic Acids and Polychlorotrifluoroethylene: A Nuclear Magnetic Resonance Investigation in Vivo

    DTIC Science & Technology

    1992-01-24

    metabolism of perfluorooctanoic acid (PFOA) and perfluorodecanoic acid (PFDA) in rats. These studies are now complete and a manuscript was submitted to...SUBTITLE S. FUNDING NUMBERS Hepatic Metabolism of Perfluorinated Carboxylic Acids and Polychlorotrifluoroethylene: A Nuclear Magnetic Resonance...describes recent results of studies designed to investigate the metabolic effects of perfluoro- carboxylic acids on liver carbohydrate and high-energy

  11. Interaction between adrenaline and dibenzo-18-crown-6: Electrochemical, nuclear magnetic resonance, and theoretical study

    NASA Astrophysics Data System (ADS)

    Yu, Zhang-Yu; Liu, Tao; Wang, Xue-Liang

    2014-12-01

    The interaction between adrenaline (Ad) and dibenzo-18-crown-6 (DB18C6) was studied by cyclic voltammetry, nuclear magnetic resonance spectroscopy, and the theoretical calculations, respectively. The results show that DB18C6 will affect the electron transfer properties of Ad. DB18C6 can form stable supramolecular complexes with Ad through ion-dipole and hydrogen bond interactions.

  12. Exploration of the Use of Nuclear Magnetic Resonance for the Study of Ricin Toxicity in Cells

    DTIC Science & Technology

    2009-04-01

    ricin. 15. SUBJECT TERMS 3T3 Cells Ricinus communis Cell Toxicity Nuclear Magnetic Resonance NMR Ricin 16. SECURITY CLASSIFICATION OF: a. REPORT u...Ricin Preparation. The Ricin communis agglutinin II (ricin) stock solution was prepared by dialyzing ricin (Vector Laboratories, Burlingame, CA

  13. A Noninvasive Method to Study Regulation of Extracellular Fluid Volume in Rats Using Nuclear Magnetic Resonance

    EPA Science Inventory

    Time-domain nuclear magnetic resonance (TD-NMR)-based measurement of body composition of rodents is an effective method to quickly and repeatedly measure proportions of fat, lean, and fluid without anesthesia. TD-NMR provides a measure of free water in a living animal, termed % f...

  14. Quantitative Analysis of Nail Polish Remover Using Nuclear Magnetic Resonance Spectroscopy Revisited

    ERIC Educational Resources Information Center

    Hoffmann, Markus M.; Caccamis, Joshua T.; Heitz, Mark P.; Schlecht, Kenneth D.

    2008-01-01

    Substantial modifications are presented for a previously described experiment using nuclear magnetic resonance (NMR) spectroscopy to quantitatively determine analytes in commercial nail polish remover. The revised experiment is intended for a second- or third-year laboratory course in analytical chemistry and can be conducted for larger laboratory…

  15. A Noninvasive Method to Study Regulation of Extracellular Fluid Volume in Rats Using Nuclear Magnetic Resonance

    EPA Science Inventory

    Time-domain nuclear magnetic resonance (TD-NMR)-based measurement of body composition of rodents is an effective method to quickly and repeatedly measure proportions of fat, lean, and fluid without anesthesia. TD-NMR provides a measure of free water in a living animal, termed % f...

  16. The Complexation of the Na(super +) by 18-Crown-6 Studied via Nuclear Magnetic Resonance

    ERIC Educational Resources Information Center

    Peters, Steven J.; Stevenson, Cheryl D.

    2004-01-01

    A student friendly experiment that teaches several important concepts of modern nuclear magnetic resonance (NMR), like multinuclear capabilities, the NMR time scale, and time-averaged signals, is described along with some important concepts of thermo chemical equilibria. The mentioned experiment involves safe and inexpensive compounds, such as…

  17. In vivo imaging of the rat anatomy with nuclear magnetic resonance.

    PubMed

    Hansen, G; Crooks, L E; Davis, P; De Groot, J; Herfkens, R; Margulis, A R; Gooding, C; Kaufman, L; Hoenninger, J; Arakawa, M; McRee, R; Watts, J

    1980-09-01

    Live rats were imaged by nuclear magnetic resonance (NMR). These images demonstrated fine detail and high object contrast. Motion artifacts are not apparent in 4-minute images, and major blood vessels are demonstrated as regions of low signal intensity because of blood flow. Selective contrast enhancement is possible by varying NMR imager accumulation parameters.

  18. Time domain-nuclear magnetic resonance study of chars from southern hardwoods

    Treesearch

    Thomas Elder; Nicole Labbe; David Harper; Timothy Rials

    2006-01-01

    Chars from the thermal degradation of silver maple (Acer saccharinum), red maple (Acer rubrum), sugar maple (Acer saccharum), and white oak (Quercus spp.), performed at temperatures from 250 to 350 oC, were examined using time domain-nuclear magnetic resonance...

  19. Structural Isomer Identification via NMR: A Nuclear Magnetic Resonance Experiment for Organic, Analytical, or Physical Chemistry.

    ERIC Educational Resources Information Center

    Szafran, Zvi

    1985-01-01

    Background information, procedures used, and typical results obtained are provided for an experiment that examines the ability of nuclear magnetic resonance (NMR) to distinguish between structural isomers via resonance multiplicities and chemical shifts. Reasons for incorporating the experiment into organic, analytical, or physical chemistry…

  20. Effect of 1. 5 tesla nuclear magnetic resonance imaging scanner on implanted permanent pacemakers

    SciTech Connect

    Hayes, D.L.; Holmes, D.R. Jr.; Gray, J.E.

    1987-10-01

    Patients with a permanent pacemaker are currently restricted from diagnostic nuclear magnetic resonance (NMR) imaging because of potential adverse effects on the pacemaker by the magnet. Previous work has shown that NMR imaging will result in asynchronous pacing of the pulse generator within a given distance of the magnet. The radiofrequency signal generated by the system may also result in rapid cardiac pacing, which may have deleterious effects. This study utilized a 1.5 tesla unit in an in vivo laboratory animal to evaluate the unit's effects on eight different pulse generators from two manufacturers. All pacemakers functioned in an asynchronous mode when placed within a certain distance of the magnet. In addition, transient reed switch inhibition was observed. Seven of the eight pulse generators paced rapidly when exposed to the radiofrequency signal and there was a dramatic decrease in arterial blood pressure. Whether effective rapid cardiac pacing would occur could not be predicted before exposure to the magnetic resonance unit. Nuclear magnetic resonance imaging with high magnetic fields in patients with a pacemaker should continue to be avoided until the mechanism of the rapid cardiac pacing can be further delineated and either predicted or prevented.

  1. Relativistic effects on the nuclear magnetic shielding in the MF (M=Cu, Ag, Au) series

    SciTech Connect

    David, Jorge; Restrepo, Albeiro

    2007-11-15

    Relativistic effects on the nuclear magnetic shielding {sigma}(M) of the series of diatomics MF (M=Cu, Ag, Au) are calculated and analyzed using the Dirac-Hartree-Fock (DHF) method in the random phase approximation (RPA). Significant differences due to relativistic effects on the shielding constant {sigma}(M) are found in this series of atoms. The high electronegativity of the fluorine atom works in conjunction with the spin-orbit coupling to increase the calculated value for {sigma}(Au). An unusually large diamagnetic contribution to the shielding constant is observed. Nonrelativistic nuclear magnetic shielding [{sigma}{sup NR}(M)] shows very good linear correlation with the nuclear charge (Z) of the metal, while the relativistic shielding [{sigma}{sup rel}(M)] varies as Z{sup 2.26}.

  2. Optically detected nuclear magnetic resonance in n-GaAs using an on-chip microcoil

    NASA Astrophysics Data System (ADS)

    Chen, Y. S.; Huang, J.; Reuter, D.; Ludwig, A.; Wieck, A. D.; Bacher, G.

    2011-02-01

    Optically detected nuclear magnetic resonance (NMR) with micrometer resolution is demonstrated in n-GaAs using an on-chip microcoil. To trace the Overhauser field, the electron Larmor frequency is monitored via time-resolved magneto-optical Kerr rotation. Sweeping the frequency of the rf magnetic field induced by an on-chip microscale current loop, nuclear spin depolarization is achieved for each isotope species. The experimental data indicate an impact of a local quadrupole field, most likely caused by ionized donors, on the amplitude and linewidth of the NMR spectrum. By applying rf pulse sequences, the Rabi oscillation of A75s nuclear spins is obtained with an effective dephasing time of ˜200 μs.

  3. Electrically detected nuclear magnetic resonance in GaAs/AlGaAs-based quantum point contacts

    NASA Astrophysics Data System (ADS)

    Keane, Zachary; Godfrey, Matthew; Burke, Adam; Chen, Jason; Fricke, Sebastian; Klochan, Oleh; Micolich, Adam; Beere, Harvey; Ritchie, Dave; Trunov, Kirill; Reuter, Dirk; Wieck, Andreas; Hamilton, Alex

    2011-03-01

    Nuclear magnetic resonance (NMR) is a well-known technique with widespread applications in physics, chemistry and medicine. Conventional NMR studies use inductive coils to detect the magnetic field produced by precessing nuclear spins; this approach requires on the order of 1012 spins for detection. Recently, resistive detection of NMR through the hyperfine interaction has been demonstrated with electrons in mesoscopic 2- and 1-dimensional devices based on high-quality GaAs/AlGaAs heterostructures. These studies are typically sensitive to 108 spins, enabling NMR on much smaller sample volumes. Holes are predicted to have much weaker nuclear spin coupling than electrons, which could be relevant to the emerging fields of spintronics and quantum information processing. We present a preliminary comparison between the magnitude of the NMR signal in electron and hole quantum point contacts.

  4. Damage dosimetry and embrittlement monitoring of nuclear pressure vessels in real time by magnetic properties measurement

    SciTech Connect

    Stubbins, J.F.; Ougouag, A.M.; Williams, J.G.

    1992-07-01

    The objective of this project is to develop a technique for real-time monitoring of neutron dose and of the onset and progression of embrittlement in operating nuclear pressure vessels. The technique relies on the measurement of magnetic properties of steel and other magnetic materials which are extremely sensitive to radiation-induced properties changes. The approach being developed here is innovative and unique. It promises to be readily applicable to all existing and planned reactor structures. The significance of this program is that it addresses a major concern in the operation of existing nuclear pressure vessels. The development of microscopic defect clusters during irradiation in the nuclear pressure vessel beltline region leads to an increase in material yield strength and a concomitant decrease in ductility, or ability to absorb energy in fracture (i.e. fracture toughness). This decrease in fracture toughness is alarming since it may impair the ability of the pressure vessel to resist fracture during unusual loading situations.

  5. Remote detection of nuclear magnetic resonance with an anisotropic magnetoresistive sensor.

    PubMed

    Verpillat, F; Ledbetter, M P; Xu, S; Michalak, D J; Hilty, C; Bouchard, L-S; Antonijevic, S; Budker, D; Pines, A

    2008-02-19

    We report the detection of nuclear magnetic resonance (NMR) using an anisotropic magnetoresistive (AMR) sensor. A "remote-detection" arrangement was used in which protons in flowing water were prepolarized in the field of a superconducting NMR magnet, adiabatically inverted, and subsequently detected with an AMR sensor situated downstream from the magnet and the adiabatic inverter. AMR sensing is well suited for NMR detection in microfluidic "lab-on-a-chip" applications because the sensors are small, typically on the order of 10 mum. An estimate of the sensitivity for an optimized system indicates that approximately 6 x 10(13) protons in a volume of 1,000 mum(3), prepolarized in a 10-kG magnetic field, can be detected with a signal-to-noise ratio of 3 in a 1-Hz bandwidth. This level of sensitivity is competitive with that demonstrated by microcoils in superconducting magnets and with the projected sensitivity of microfabricated atomic magnetometers.

  6. Structural analysis of strained quantum dots using nuclear magnetic resonance.

    PubMed

    Chekhovich, E A; Kavokin, K V; Puebla, J; Krysa, A B; Hopkinson, M; Andreev, A D; Sanchez, A M; Beanland, R; Skolnick, M S; Tartakovskii, A I

    2012-10-01

    Strained semiconductor nanostructures can be used to make single-photon sources, detectors and photovoltaic devices, and could potentially be used to create quantum logic devices. The development of such applications requires techniques capable of nanoscale structural analysis, but the microscopy methods typically used to analyse these materials are destructive. NMR techniques can provide non-invasive structural analysis, but have been restricted to strain-free semiconductor nanostructures because of the significant strain-induced quadrupole broadening of the NMR spectra. Here, we show that optically detected NMR spectroscopy can be used to analyse individual strained quantum dots. Our approach uses continuous-wave broadband radiofrequency excitation with a specially designed spectral pattern and can probe individual strained nanostructures containing only 1 × 10(5) quadrupole nuclear spins. With this technique, we are able to measure the strain distribution and chemical composition of quantum dots in the volume occupied by the single confined electron. The approach could also be used to address problems in quantum information processing such as the precise control of nuclear spins in the presence of strong quadrupole effects.

  7. Matrix decompositions of two-dimensional nuclear magnetic resonance spectra.

    PubMed

    Havel, T F; Najfeld, I; Yang, J X

    1994-08-16

    Two-dimensional NMR spectra are rectangular arrays of real numbers, which are commonly regarded as digitized images to be analyzed visually. If one treats them instead as mathematical matrices, linear algebra techniques can also be used to extract valuable information from them. This matrix approach is greatly facilitated by means of a physically significant decomposition of these spectra into a product of matrices--namely, S = PAPT. Here, P denotes a matrix whose columns contain the digitized contours of each individual peak or multiple in the one-dimensional spectrum, PT is its transpose, and A is an interaction matrix specific to the experiment in question. The practical applications of this decomposition are considered in detail for two important types of two-dimensional NMR spectra, double quantum-filtered correlated spectroscopy and nuclear Overhauser effect spectroscopy, both in the weak-coupling approximation. The elements of A are the signed intensities of the cross-peaks in a double quantum-filtered correlated spectrum, or the integrated cross-peak intensities in the case of a nuclear Overhauser effect spectrum. This decomposition not only permits these spectra to be efficiently simulated but also permits the corresponding inverse problems to be given an elegant mathematical formulation to which standard numerical methods are applicable. Finally, the extension of this decomposition to the case of strong coupling is given.

  8. Methods of, and apparatus for, proton decoupling in nuclear magnetic resonance spectroscopy

    SciTech Connect

    Vatis, D.; Bottomley, P.A.; Foster, T.H.

    1987-07-21

    This patent describes an apparatus for providing a radio-frequency signal having at least one selected one of (1) first specie decoupling and (2) nuclear Overhauser enhancement effect, upon a second nuclei specie in a sample in a nuclear magnetic resonance (NMR) experiment, comprising: means for providing a radio-frequency (RF) signal at a center frequency substantially equal to the Larmor frequency of a first specie, different from the second nuclear specie, in the sample; means for modulating the amplitude of the RF signal with a time-dependent sinc (..omega../sub O/t) signal waveform; means for adjusting at least one selected one of (1) the amplitude of the modulated radio-frequency signal and (2) the instantaneous center frequency, across a range of frequencies related to a chemical shift spectrum ..omega../sub O/ of the first specie; and means for applying the adjusted signal to the sample to cause at least one selected one of (1) minimization of the coupling of the first nuclear specie to, and (2) nuclear Overhauser enhancement of, magnetic resonance spectroscopy response signals provided by the second nuclear specie.

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

    SciTech Connect

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

    2015-06-21

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

  10. Spinodal instabilities and the distillation effect in nuclear matter under strong magnetic fields

    SciTech Connect

    Rabhi, A.; Providencia, C.; Providencia, J. Da

    2009-01-15

    We study the effect of strong magnetic fields, of the order of 10{sup 18}-10{sup 19} G, on the instability region of nuclear matter at subsaturation densities. Relativistic nuclear models both with constant couplings and with density-dependent parameters are considered. It is shown that a strong magnetic field can have large effects on the instability regions giving rise to bands of instability and wider unstable regions. As a consequence, we predict larger transition densities at the inner edge of the crust of compact stars with strong magnetic fields. The direction of instability gives rise to a very strong distillation effect if the last Landau level is only partially filled. However, for almost completed Landau levels, an antidistillation effect may occur.

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

    PubMed

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

    2015-06-21

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

  12. Table of nuclear magnetic dipole and electric quadrupole moments

    SciTech Connect

    Stone, N.J. . E-mail: n.stone1@physics.oxford.ac.uk

    2005-05-01

    The table is a compilation of experimental measurements of static magnetic dipole and electric quadrupole moments of ground states and excited states of atomic nuclei throughout the periodic table. To aid identification of the states, their excitation energy, half-life, spin, and parity are given, along with a brief indication of the method and any reference standard used in the particular measurement. The literature search covers the period to late 2004. Many of the entries prior to 1988 follow those in Raghavan [At. Data Nucl. Data Tables 42 (1989) 189].

  13. [Nuclear magnetic resonance tomography of the temporomandibular joint].

    PubMed

    König, H; Spitzer, W J

    1986-05-01

    Because of its position, the temporomandibular joint is difficult to demonstrate by conventional radiological methods. Even the use of complex methods, such as arthro-tomography or CT, does not result in the satisfactory demonstration of the soft tissues and, in particular, of the articular disc. Magnetic resonance was carried out in 24 patients; it was possible to differentiate functional from morphological changes in the cartilage and these are discussed. Measurements were carried out during progressive opening of the mouth. This permits direct demonstration of reversible and irreversible cartilage displacement and of other changes in the joint and cartilages.

  14. NbF5 and TaF5: Assignment of 19F NMR resonances and chemical bond analysis from GIPAW calculations

    NASA Astrophysics Data System (ADS)

    Biswal, Mamata; Body, Monique; Legein, Christophe; Sadoc, Aymeric; Boucher, Florent

    2013-11-01

    The 19F isotropic chemical shifts (δiso) of two isomorphic compounds, NbF5 and TaF5, which involve six nonequivalent fluorine sites, have been experimentally determined from the reconstruction of 1D 19F MAS NMR spectra. In parallel, the corresponding 19F chemical shielding tensors have been calculated using the GIPAW method for both experimental and DFT-optimized structures. Furthermore, the [M4F20] units of NbF5 and TaF5 being held together by van der Waals interactions, the relevance of Grimme corrections to the DFT optimization processes has been evaluated. However, the semi-empirical dispersion correction term introduced by such a method does not show any significant improvement. Nonetheless, a complete and convincing assignment of the 19F NMR lines of NbF5 and TaF5 is obtained, ensured by the linearity between experimental 19F δiso values and calculated 19F isotropic chemical shielding σiso values. The effects of the geometry optimizations have been carefully analyzed, confirming among other matters, the inaccuracy of the experimental structure of NbF5. The relationships between the fluorine chemical shifts, the nature of the fluorine atoms (bridging or terminal), the position of the terminal ones (opposite or perpendicular to the bridging ones), the fluorine charges, the ionicity and the length of the M-F bonds have been established. Additionally, for three of the 19F NMR lines of NbF5, distorted multiplets, arising from 1J-coupling and residual dipolar coupling between the 19F and 93Nb nuclei, were simulated yielding to values of 93Nb-19F 1J-coupling for the corresponding fluorine sites.

  15. Evaluation of radio frequency microcoils as nuclear magnetic resonance detectors in low-homogeneity high-field superconducting magnets

    NASA Astrophysics Data System (ADS)

    Wright, A. C.; Neideen, T. A.; Magin, R. L.; Norcross, J. A.

    1998-11-01

    We describe here experiments evaluating the performance of solenoidal radio frequency probes having submillimeter dimensions (microcoils) as detectors for liquid nuclear magnetic resonance (NMR) in very low-homogeneity (100 ppm/cm) magnetic fields. Performance is based on the measured H2O linewidth. A series of solenoidal microcoils having sample volumes 8, 53, and 593 nl were filled with distilled H2O and evaluated for smallest obtainable unshimmed NMR spectral linewidths in a vertical bore superconducting magnet, stabilized at 5.9 T (1H frequency=250 MHz). The smallest microcoil (472 μm diameter) gave a smallest H2O linewidth of 525 Hz, 25 times smaller than that from a standard 5.7 mm probe. Linewidth increased approximately as the square root of sample volume. For comparison, shimmed H2O linewidths using the same microcoils in a high-homogeneity (0.1 ppm/cm) NMR magnet were also measured. Shimmed linewidths in the high-homogeneity magnet were two orders of magnitude smaller and exhibited a similar dependence on volume. The results demonstrate that by using microcoils the volume over which the polarizing magnetic field must meet a specified homogeneity can be significantly reduced, which would be advantageous for smaller, less expensive NMR systems.

  16. Nuclear magnetic resonance relaxation and diffusion in the presence of internal gradients: the effect of magnetic field strength.

    PubMed

    Mitchell, J; Chandrasekera, T C; Johns, M L; Gladden, L F; Fordham, E J

    2010-02-01

    It is known that internal magnetic field gradients in porous materials, caused by susceptibility differences at the solid-fluid interfaces, alter the observed effective Nuclear Magnetic Resonance transverse relaxation times T2,eff. The internal gradients scale with the strength of the static background magnetic field B0. Here, we acquire data at various magnitudes of B0 to observe the influence of internal gradients on T2-T2 exchange measurements; the theory discussed and observations made are applicable to any T2-T2 analysis of heterogeneous materials. At high magnetic field strengths, it is possible to observe diffusive exchange between regions of local internal gradient extrema within individual pores. Therefore, the observed exchange pathways are not associated with pore-to-pore exchange. Understanding the significance of internal gradients in transverse relaxation measurements is critical to interpreting these results. We present the example of water in porous sandstone rock and offer a guideline to determine whether an observed T2,eff relaxation time distribution reflects the pore size distribution for a given susceptibility contrast (magnetic field strength) and spin echo separation. More generally, we confirm that for porous materials T1 provides a better indication of the pore size distribution than T2,eff at high magnetic field strengths (B0>1 T), and demonstrate the data analysis necessary to validate pore size interpretations of T2,eff measurements.

  17. Magnetization transfer modes in scalar-coupled spin systems investigated by selective two-dimensional nuclear magnetic resonance exchange experiments

    NASA Astrophysics Data System (ADS)

    Di Bari, Lorenzo; Kowalewski, Jozef; Bodenhausen, Geoffrey

    1990-12-01

    Longitudinal nuclear magnetic relaxation in coupled two-spin systems is discussed in terms of magnetization transfer modes, a generalization of the magnetization modes commonly used in the discussion of one-dimensional NMR relaxation experiments. The symmetry properties of the transfer modes and their relationship to the elements of the usual Redfield relaxation matrix are discussed. Experimental strategies for measuring the amplitudes of the transfer modes are discussed and various selective two-dimensional exchange (``soft-NOESY'') methods are proposed. Experimental data are presented for Exifone, a small organic molecule, and the auto- and cross-correlation spectral densities, the magnitudes of the proton chemical shift anisotropies, and the strengths of the dipolar interaction are derived from the spectra.

  18. Synthesis and conformational analysis of a simplified inositol-model of the Streptococcus pneumoniae 19F capsular polysaccharide repeating unit.

    PubMed

    Catelani, Giorgio; D'Andrea, Felicia; Guazzelli, Lorenzo; Griselli, Alessio; Testi, Nicola; Chiacchio, Maria Assunta; Legnani, Laura; Toma, Lucio

    2017-04-18

    Carbohydrate mimics have been studied for a long time as useful sugar substitutes, both in the investigation of biological events and in the treatment of sugar-related diseases. Here we report further evaluation of the capabilities of inositols as carbohydrate substitutes. The conformational features of an inositol-model of a simplified repeating unit corresponding to the capsular polysaccharide of Streptococcus pneumoniae 19F has been evaluated by computational analysis, and compared to the native repeating unit. The inositol mimic was synthesized, and its experimental spectroscopic data allowed for verification of the theoretical results. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Detection and differentiation of neutral organic compounds by 19F NMR with a tungsten calix[4]arene imido complex.

    PubMed

    Zhao, Yanchuan; Swager, Timothy M

    2013-12-18

    Fluorinated tungsten calix[4]arene imido complexes were synthesized and used as receptors to detect and differentiate neutral organic compounds. It was found that the binding of specific neutral organic molecules to the tungsten centers induces an upfield shift of the fluorine atom appended on the arylimido group, the extent of which is highly dependent on electronic and steric properties. We demonstrate that the specific bonding and size-selectivity of calix[4]arene tungsten-imido complex combined with (19)F NMR spectroscopy is a powerful new method for the analysis of complex mixtures.

  20. Rapid acquisition of 1H and 19F NMR experiments for direct and competition ligand-based screening.

    PubMed

    Dalvit, Claudio; Gossert, Alvar D; Coutant, Jérôme; Piotto, Martial

    2011-04-01

    Direct and competition ligand-based NMR experiments are often used in the screening of chemical fragment libraries against a protein target due to the high relative sensitivity of NMR for protein-binding events. A plethora of NMR methods has been proposed for this purpose. Two of these techniques are the (19)F T(2) filter and the (1)H selective T(2) filter experiments. Modifications of the pulse sequences of these experiments have resulted in a ∼2-fold reduction in the experiment time thus allowing an increase in the screening throughput and making NMR an attractive technique for screening large compound collections. Copyright © 2011 John Wiley & Sons, Ltd.