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Sample records for nitrogen-14 nqr nmr

  1. Methyl quantum tunneling and nitrogen-14 NQR NMR studies using a SQUID magnetic resonance spectrometer

    SciTech Connect

    Black, Bruce Elmer

    1993-07-01

    Nuclear Magnetic Resonance (NMR) and Nuclear Quadrupole Resonance (NQR) techniques have been very successful in obtaining molecular conformation and dynamics information. Unfortunately, standard NMR and NQR spectrometers are unable to adequately detect resonances below a few megahertz due to the frequency dependent sensitivity of their Faraday coil detectors. For this reason a new spectrometer with a dc SQUID (Superconducting Quantum Interference Device) detector, which has no such frequency dependence, has been developed. Previously, this spectrometer was used to observe 11B and 27Al NQR resonances. The scope of this study was increased to include 23Na, 51V, and 55Mn NQR transitions. Also, a technique was presented to observe 14N NQR resonances through cross relaxation of the nitrogen polarization to adjacent proton spins. When the proton Zeeman splitting matches one nitrogen quadrupoler transition the remaining two 14N transitions can be detected by sweeping a saturating rf field through resonance. Additionally, simultaneous excitation of two nitrogen resonances provides signal enhancement which helps to connect transitions from the same site. In this way, nitrogen-14 resonances were observed in several amino acids and polypeptides. This spectrometer has also been useful in the direct detection of methyl quantum tunneling splittings at 4.2 K. Tunneling, frequencies of a homologous series of carboxylic acids were measured and for solids with equivalent crystal structures, an exponential correlation between the tunneling frequency and the enthalpy of fusion is observed. This correlation provides information about the contribution of intermolecular interactions to the energy barrier for methyl rotation.

  2. Nitrogen-14 NQR Study of Energetic Materials

    DTIC Science & Technology

    1982-09-01

    Army Research Office Research Triangle Park North Carolina 27709 Contract No. DAAG-29-79-0025 I Submitted by: BLOCK ENGINEERING Division of Bio-Rad...NQR Lines C-i F APPENDIX D Princeton Applied Research Interface D-1 References R-1 BLOCK 󈨑 7T - %. LIST OF TABLES Tables Page 2.2-I Lorentzian FID and...as can be seen by the seemingly incongruous pairing of v and v + lines in Figure 3.1-1. In fact, it will be shown that the chemical inequivalence of "o

  3. Nitrogen-14 nuclear quadrupole resonance (NQR): dramatic sensitivity enhancement by large and fast temperature lowering.

    PubMed

    Ferrari, Maude; Retournard, Alain; Canet, Daniel

    2007-10-01

    We have observed that, when going rapidly from ambient temperature down to liquid nitrogen temperature, the nitrogen-14 NQR signal (for transitions involving the m=0 spin state, nitrogen-14 being a quadrupolar nucleus of spin I=1) is increased by a factor of ca. 10(2). While Boltzmann statistics cannot explain this enhancement, the strong temperature dependence of the quadrupolar interaction is very likely to be at the origin of this phenomenon. Indeed, the quadrupolar Hamiltonian becomes time dependent and is prone to induce transitions toward the spin state associated with m=0. Its binding and slow relaxing properties result in a durable increased population and consequently in an increased intensity of NQR lines originating from the state m=0.

  4. Some nitrogen-14 NMR studies in solids

    SciTech Connect

    Pratum, T.K.

    1983-11-01

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

  5. Nanoscale NMR and NQR with Nitrogen Vacancy Centers

    NASA Astrophysics Data System (ADS)

    Urbach, Elana; Lovchinsky, Igor; Sanchez-Yamagishi, Javier; Choi, Soonwon; Bylinskii, Alexei; Dwyer, Bo; Andersen, Trond; Sushkov, Alex; Park, Hongkun; Lukin, Mikhail

    2016-05-01

    Nuclear quadrupole resonance (NQR) is a powerful tool which is used to detect quadrupolar interaction in nuclear spins with I > 1/2. Conventional NQR and NMR technology, however, rely on measuring magnetic fields from a macroscopic number of spins. Extending NMR and NQR techniques to the nanoscale could allow us to learn structural information about interesting materials and biomolecules. We present recent progress on using Nitrogen-Vacancy (NV) centers in diamond to perform room temperature nanoscale NMR and NQR spectroscopy on small numbers of nuclear spins in hexagonal boron nitride.

  6. Fourier transform zero field NMR and NQR

    SciTech Connect

    Zax, D.B.

    1984-09-01

    The characterization of the structural and chemical properties of matter, particularly in disordered condensed phases, is a difficult process. Few analytical methods work effectively on polycrystalline or amorphous solids. In many systems the chemical shifts measured by traditional high resolution solid state NMR methods are insufficiently sensitive or the information contained in the dipole-dipole couplings is more important. In these cases Fourier transform zero field magnetic resonance may make an important contribution. Zero field NMR and NQR is the subjecti of this thesis.

  7. Fourier transform zero field NMR and NQR

    SciTech Connect

    Zax, D.B.

    1985-01-01

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

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

    PubMed

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

    2011-04-01

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

  9. NMR and NQR study of the thermodynamically stable quasicrystals

    SciTech Connect

    Shastri, A.

    1995-02-10

    {sup 27}Al and {sup 61,65}Cu NMR measurements are reported for powder samples of stable AlCuFe and AlCuRu icosahedral quasicrystals and their crystalline approximants, and for a AlPdMn single grain quasicrystal. Furthermore, {sup 27}Al NQR spectra at 4.2 K have been observed in the AlCuFe and AlCuRu samples. From the quadrupole perturbed NMR spectra at different magnetic fields, and from the zero field NQR spectra, a wide distribution of local electric field gradient (EFG) tensor components and principal axis system orientations was found at the Al site. A model EFG calculation based on a 1/1 AlCuFe approximant was successful in explaining the observed NQR spectra. It is concluded that the average local gradient is largely determined by the p-electron wave function at the Al site, while the width of the distribution is due to the lattice contribution to the EFG. Comparison of {sup 63}Cu NMR with {sup 27}Al NMR shows that the EFG distribution at the two sites is similar, but that the electronic contribution to the EFG is considerably smaller at the Cu site, in agreement with a more s-type wave function of the conduction electrons.

  10. SQUID detected NMR and NQR. Superconducting Quantum Interference Device.

    PubMed

    Augustine, M P; TonThat, D M; Clarke, J

    1998-03-01

    The dc Superconducting QUantum Interference Device (SQUID) is a sensitive detector of magnetic flux, with a typical flux noise of the order 1 muphi0 Hz(-1/2) at liquid helium temperatures. Here phi0 = h/2e is the flux quantum. In our NMR or NQR spectrometer, a niobium wire coil wrapped around the sample is coupled to a thin film superconducting coil deposited on the SQUID to form a flux transformer. With this untuned input circuit the SQUID measures the flux, rather than the rate of change of flux, and thus retains its high sensitivity down to arbitrarily low frequencies. This feature is exploited in a cw spectrometer that monitors the change in the static magnetization of a sample induced by radio frequency irradiation. Examples of this technique are the detection of NQR in 27Al in sapphire and 11B in boron nitride, and a level crossing technique to enhance the signal of 14N in peptides. Research is now focused on a SQUID-based spectrometer for pulsed NQR and NMR, which has a bandwidth of 0-5 MHz. This spectrometer is used with spin-echo techniques to measure the NQR longitudinal and transverse relaxation times of 14N in NH4ClO4, 63+/-6 ms and 22+/-2 ms, respectively. With the aid of two-frequency pulses to excite the 359 kHz and 714 kHz resonances in ruby simultaneously, it is possible to obtain a two-dimensional NQR spectrum. As a third example, the pulsed spectrometer is used to study NMR spectrum of 129Xe after polariza-tion with optically pumped Rb. The NMR line can be detected at frequencies as low as 200 Hz. At fields below about 2 mT the longitudinal relaxation time saturates at about 2000 s. Two recent experiments in other laboratories have extended these pulsed NMR techniques to higher temperatures and smaller samples. In the first, images were obtained of mineral oil floating on water at room temperature. In the second, a SQUID configured as a thin film gradiometer was used to detect NMR in a 50 microm particle of 195Pt at 6 mT and 4.2 K.

  11. Investigation of structural information for boron-rich solids and aluminates via NMR and NQR studies

    SciTech Connect

    Lee, D.

    1991-01-01

    Along with NMR, Nuclear Quadrupole Resonance (NQR) has become important recently for obtaining structural information from oxide glasses. The NQR studies prove in this thesis that they provide more accurate structural information than the NMR studies have done. This study presents boron and aluminum NMR, and NQR studies for some borate glasses and compounds, icosahedral boron-rich solids, some crystalline aluminosilicates. Various borates were employed to acquire structural information as well as to determine the quadrupole parameters (the quadrupole coupling constant Qcc and the asymmetry parameter {eta}) using NQR under a guidance of NMR or vice versa. By NQR a previously unknown boron site was observed for vitreous Li{sub 2}O{center dot}B{sub 2}O{sub 3}. The NMR and NQR studies were performed on some icosachedral boron-rich solids: {alpha}-rhombohedral boron (B{sub 12}), {beta}-boron (B{sub 105}) and boron carbide (B{sub 12}C{sub 3}). Three different forms of crystalline aluminosilicate (Al{sub 2}SiO{sub 5}) were studied by NQR. The NQR study yielded more accurate values of the quadrupole parameters for {sup 27}Al than the previous NMR single crystal study did.

  12. Quadrupole coupling parameters and structural aspects of crystalline and amorphous solids by NMR and NQR

    SciTech Connect

    Mao, Degen.

    1991-01-01

    NMR and NQR techniques were combined to obtain the quadrupole coupling constant (Qcc) and asymmetry parameter ({eta}) and extract structural information for several borate, gallate, and metavanadate compounds and glasses. {sup 71}Ga and {sup 69}Ga NMR was used to study crystalline {beta}-Ga{sub 2}O{sub 3} and several gallate glasses. Quadrupole parameters were acquired for GaO{sub 6} and GaO{sub 4} units in {beta}-Ga{sub 2}O{sub 3} by the computer simulation of the NMR powder patterns. A sensitive CW NQR spectrometer was built to detect NQR resonances below 2 MHz. The spectrometer includes a modified Robinson oscillator-detector, a new bi-symmetric square wave Zeeman modulator and a computerized data acquisition system. {sup 51}V (I = 7/2) NQR resonances below 850 kHz were detected for several metavanadates at both room temperature and liquid nitrogen temperature. Two methods, Zeeman perturbed NQR powder pattern and {sup 10}B NQR, can be employed to obtain both Qcc and {eta}. With a double coil tank circuit design, pure {sup 11}B NQR was used to determine the fraction of borons in BO{sub 3} and BO{sub 4} configurations in hydrated zinc borates. {sup 11}B NMR and NQR were also used to study lead borate glasses.

  13. Localized 5f antiferromagnetism in cubic UIn3 : I115n-NMR/NQR study

    NASA Astrophysics Data System (ADS)

    Sakai, Hironori; Kambe, Shinsaku; Tokunaga, Yo; Chudo, Hiroyuki; Tokiwa, Yoshifumi; Aoki, Dai; Haga, Yoshinori; Ōnuki, Yoshichika; Yasuoka, Hiroshi

    2009-03-01

    I115n nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements have been performed on an antiferromagnet UIn3 with the cubic AuCu3 -type structure. The NQR frequency (νQ) and Knight shift (K) of I115n in UIn3 have been estimated in the paramagnetic state from NMR experiments under applied field. The perpendicular component of transferred hyperfine coupling constant (A⊥) has been deduced from scaled behavior of K to the static susceptibility (χ) . Under zero field, the observation of the NQR spectrum has led to an estimated νQ of 11.8 MHz at 90 K. The temperature variation in the NQR relaxation rates (1/T1) far above the Néel temperature TN=88K approaches a constant value, which indicates a localized nature for the 5f electrons in this system. On the other hand, in the antiferromagnetically ordered state at 4 K (well below TN ), the I115n -NMR spectrum has been scanned over frequencies ranging from ˜20 to ˜70MHz under zero applied field. From the analysis of the NMR spectrum, we propose that the most plausible direction of antiferromagnetic U moments may be ⟨110⟩ among the possible orientations of ⟨100⟩ , ⟨110⟩ , or ⟨111⟩ .

  14. Zero field NMR and NQR with selective pulses and indirect detection

    SciTech Connect

    Millar, J.M.; Thayer, A.M.; Bielecki, A.; Zax, D.B.; Pines, A.

    1985-08-01

    Zero field NMR and NQR spectra are obtained by the application of dc magnetic field pulses to a demagnetized sample. Pulsed dc fields allow for selective excitation of isotopic species and provide a means for coherent manipulation of the spin system in zero field. Using these selective pulses and level crossing techniques, indirect detection of a quadrupolar nucleus may be accomplished via protons without obtaining the proton background signal in the NQR spectrum. Experimental results from a variety of /sup 1/H, /sup 2/H, and /sup 14/N homo- and heteronuclear systems are presented as an illustration of these techniques.

  15. 75As, 63Cu NMR and NQR characterization of selected arsenic minerals.

    PubMed

    Lehmann-Horn, J A; Miljak, D G; Bastow, T J

    2013-01-01

    The direct measurement and identification of solid state arsenic phases using (75)As NMR is made difficult by the simultaneous conditions of large quadrupole moment and low coordination symmetry in many compounds. However, specific arsenic minerals can efficiently be detected and discriminated via nuclear quadrupolar resonance (NQR). We report on the first NMR and NQR measurements in the natural minerals enargite (Cu3AsS4), niccolite (NiAs), arsenopyrite (FeAsS) and loellingite (FeAs2). The NQR frequencies have been determined from both high-field NMR powder patterns and via zero-field frequency sweeps. Density functional theory (DFT) based ab initio calculations support the experimental results. The compounds studied here are common in terms of the known set of As-containing minerals. They are sometimes encountered in the context of base metal or gold mining. The study represents a significant addition to the list of arsenic minerals that can now be detected with NQR techniques. © 2013 Elsevier Inc. All rights reserved.

  16. Low-frequency NMR and NQR with a dc SQUID amplifier

    SciTech Connect

    Fan, Nong-Qiang.

    1990-11-01

    A sensitive Fourier-transform spectrometer based on a dc SQUID (Superconducting QUantum Interference Device) has been developed for the direct detection of nuclear magnetic resonance (NMR) in zero applied magnetic field and pure nuclear quadrupole resonance (NQR) at low frequencies. The motivation to detect zero field NMR and NQR is to provide a new high resolution spectroscopy technique at frequencies below 200 kHz to study ultra-weak interactions in chemicals and materials. By comparing the sensitivity of a SQUID amplifier with that of a conventional semiconductor amplifier, it is shown that a SQUID amplifier is essential for the direct detection of low frequency resonant signals. The spectrometer has a frequency response extending from about 10 to 200 kHz, and a recovery time (after the magnetic pulse is removed) of about 50 {mu}s. The spectrometer is used to detect NMR spectra from Pt and Cu metal powders in a magnetic field of 6 mtesla, and NQR spectra from {sup 2}D in a tunneling methyl group and {sup 14}N in NH{sub 4}ClO{sub 4}. Finally, the zero field NMR spectrum from a quantum tunneling methyl group is calculated. 25 refs., 34 figs., 2 tabs.

  17. Sb-NMR/NQR studies of heavy fermion system YbRhSb

    NASA Astrophysics Data System (ADS)

    Kishimoto, Yasuki; Awai, Yosiki; Kotegawa, Hisashi; Tou, Hideki; Muro, Yuji; Nakamura, Koji; Sera, Masafumi; Takabatake, Toshiro

    2017-04-01

    We report a study of 121Sb nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) in a Yb-based heavy fermion system YbRhSb using a single crystal. Sharp 121Sb-NMR lines were observed for each crystal axis for B‖a,b,c. From comparison with observed Sb-NMR spectra and numerical simulations, electric field gradient (EFG) parameters and Knight shift parameters are obtained at 10 K. The obtained quadrupole frequency, asymmetry parameter, isotropic Knight shift and anisotropic principal values of Knight shift tensors are νQ = 18.8 MHz, η =0.2,\\text{\\hspace{0.17em}}{K}{iso}≈ 0.6 % , and ({K}\\text{ax}x,{K}\\text{ax}y,{K}\\text{ax}z)≈ (-3.5,4.1,-0.6) % , respectively. We also succeeded in observing 121Sb-NQR signals at around 19.5 and 37 MHz, which are reproduced by the nuclear quadrupole Hamiltonian with νQ = 18.8 MHz and η = 0.2. We mention the relation between the anisotropy of the Knight shift and magnetic susceptibility. Our NMR/NQR results suggest that the weak ferromagnetism in YbRhSb is ascribed to a canted antiferromagnetic state.

  18. Structure-activity study of thiazides by magnetic resonance methods (NQR, NMR, EPR) and DFT calculations.

    PubMed

    Latosińska, J N

    2005-01-01

    The paper presents a comprehensive analysis of the relationship between the electronic structure of thiazides and their biological activity. The compounds of interest were studied in solid state by the resonance methods nuclear quadrupole resonance (NQR), nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) and quantum chemistry (ab inito and DFT) methods. Detailed parallel analysis of the spectroscopic parameters such as quadrupole coupling constant (QCC) NQR chemical shift (delta), chemical shift anisotropy (CSA), asymmetry parameter (eta), NMR and hyperfine coupling constant (A), EPR was performed and the electronic effects (polarisation and delocalisation) were revealed and compared. Biological activity of thiazides has been found to depend on many factors, but mainly on the physico-chemical properties whose assessment was possible on the basis of electron density determination in the molecules performed by experimental and theoretical methods.

  19. Improving resolution in proton solid-state NMR by removing nitrogen-14 residual dipolar broadening

    NASA Astrophysics Data System (ADS)

    Stein, Robin S.; Elena, Bénédicte; Emsley, Lyndon

    2008-06-01

    Residual dipolar coupling between quadrupolar and other nuclei under MAS has not usually been thought to be important in high field NMR spectroscopy. We show that coupling to 14N broadens 1H lineshapes significantly even at 11.7 T, and that we can decouple 14N from 1H during 1H homonuclear decoupling to successfully improve 1H resolution. The method used for decoupling is the application of evenly spaced pulses to the quadrupolar nucleus.

  20. Quadrupole interactions: NMR, NQR, and in between from a single viewpoint.

    PubMed

    Bain, Alex D

    2017-03-01

    Nuclear spins with quantum numbers >1/2 can interact with a static magnetic field, or a local electric field gradient, to produce quantized energy levels. If the magnetic field interaction dominates, we are doing nuclear magnetic resonance (NMR). If the interaction of the nuclear electric quadrupole with electric field gradients is much stronger, this is nuclear quadrupole resonance (NQR). The two are extremes of a continuum, as the ratio of one interaction to the other changes. In this work, we look at this continuum from a single, unified viewpoint based on a Liouville-space approach: the direct method. This method does not require explicit operators and their commutators, unlike Hamiltonian methods. We derive both the quadrupole-perturbed NMR solution and also the Zeeman-perturbed NQR results. Furthermore, we examine the polarization of these signals, because this is different between pure NMR and pure NQR spectroscopy. Spin 3/2 is the focus here, but the approach is perfectly general and can be applied to any spin. Copyright © 2016 John Wiley & Sons, Ltd.

  1. NMR and NQR studies of URu2Si2 and isostructural nonmagnetic references

    NASA Astrophysics Data System (ADS)

    Emi, Naoya; Hamabata, Ryosuke; Koyama, Takehide; Ueda, Koichi; Mito, Takeshi; Kohori, Yoh; Matsumoto, Yuji; Haga, Yoshinori; Yamamoto, Etsuji; Fisk, Zachary

    2017-06-01

    The non-f compound ThRu2Si2 has been studied as an isostructural nonmagnetic reference for URu2Si2 using nuclear magnetic resonance (NMR) measurement. The temperature dependences of Knight shifts measured by 29Si-NMR and 99Ru-NMR are independent of temperature. The results are consistent with data previously reported on the susceptibility. 101Ru-NQR frequency 101 ν Q was also estimated from the 99Ru-NMR measurement. 101 ν Q of ThRu2Si2 is close to that of URu2Si2, especially at high temperatures, suggesting that U ions in URu2Si2 are in a nearly tetravalent state.

  2. 93Nb- and 27Al-NMR/NQR studies of the praseodymium based PrNb2Al20

    NASA Astrophysics Data System (ADS)

    Kubo, Tetsuro; Kotegawa, Hisashi; Tou, Hideki; Higashinaka, Ryuji; Nakama, Akihiro; Aoki, Yuji; Sato, Hideyuki

    2015-03-01

    We report a study of 93Nb- and 27Al-nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) in a praseodymium based compound PrNb2Al20. The observed NMR line at around 3 T and 30 K shows a superposition of typical powder patterns of one Nb signal and at least two Al signals. 93Nb-NMR line could be reproduced by using the previously reported NQR frequency νQ ≊ 1.8MHz and asymmetry parameter η ≊ 0 [Kubo T et al 2014 JPS Conf. Proc. 3 012031]. From 27Al-NMR/NQR, NQR parameters are obtained to be νQ,A ≊ 1.53 MHz, and ηA ≊ 0.20 for the site A, and νQ,B ≊ 2.28 MHz, and ηB ≊ 0.17 for the site B. By comparing this result with the previous 27Al-NMR study of PrT2Al20 (T = Ti, V) [Tokunaga Y et al 2013 Phys. Rev. B 88 085124], these two Al site are assigned to the two of three crystallographycally inequivalent Al sites.

  3. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1990-01-01

    The primary intent of our study is to investigate the magnetic character of copper-cobalt catalysts and examine the relation between catalytic and magnetic properties of the catalyst. The results reported in the previous report on the zerofield NMR spectra of a series of Cu/Co catalysts have been a serious concern due to the number of high frequency lines observed which did not fit the expected pattern. To further investigate this discrepancy, we have prepared again several catalysts in our laboratory and scanned the NMR/NQR spectra and studied the magnetization characteristics at Howard University during the Summer 1990. Two undergraduate physics majors made the magnetization studies using the vibration sample magnetometer system. 13 refs., 2 figs., 3 tabs.

  4. Solid-state NMR/NQR and first-principles study of two niobium halide cluster compounds.

    PubMed

    Perić, Berislav; Gautier, Régis; Pickard, Chris J; Bosiočić, Marko; Grbić, Mihael S; Požek, Miroslav

    2014-01-01

    Two hexanuclear niobium halide cluster compounds with a [Nb6X12](2+) (X=Cl, Br) diamagnetic cluster core, have been studied by a combination of experimental solid-state NMR/NQR techniques and PAW/GIPAW calculations. For niobium sites the NMR parameters were determined by using variable Bo field static broadband NMR measurements and additional NQR measurements. It was found that they possess large positive chemical shifts, contrary to majority of niobium compounds studied so far by solid-state NMR, but in accordance with chemical shifts of (95)Mo nuclei in structurally related compounds containing [Mo6Br8](4+) cluster cores. Experimentally determined δiso((93)Nb) values are in the range from 2,400 to 3,000 ppm. A detailed analysis of geometrical relations between computed electric field gradient (EFG) and chemical shift (CS) tensors with respect to structural features of cluster units was carried out. These tensors on niobium sites are almost axially symmetric with parallel orientation of the largest EFG and the smallest CS principal axes (Vzz and δ33) coinciding with the molecular four-fold axis of the [Nb6X12](2+) unit. Bridging halogen sites are characterized by large asymmetry of EFG and CS tensors, the largest EFG principal axis (Vzz) is perpendicular to the X-Nb bonds, while intermediate EFG principal axis (Vyy) and the largest CS principal axis (δ11) are oriented in the radial direction with respect to the center of the cluster unit. For more symmetrical bromide compound the PAW predictions for EFG parameters are in better correspondence with the NMR/NQR measurements than in the less symmetrical chlorine compound. Theoretically predicted NMR parameters of bridging halogen sites were checked by (79/81)Br NQR and (35)Cl solid-state NMR measurements. Copyright © 2014 Elsevier Inc. All rights reserved.

  5. Zero-field NMR and NQR studies of magnetically ordered state in charge-ordered EuPtP

    NASA Astrophysics Data System (ADS)

    Koyama, T.; Maruyama, T.; Ueda, K.; Mito, T.; Mitsuda, A.; Umeda, M.; Sugishima, M.; Wada, H.

    2015-03-01

    EuPtP undergoes two valence transitions and has two kinds of valence states of Eu ions at low temperatures. In the charge-ordered state, this compound shows an antiferromagnetic order ascribed to magnetic divalent Eu ions. We investigated the antiferromagnetically ordered state of EuPtP by nuclear magnetic resonance (NMR) measurement and nuclear quadrupole resonance (NQR) measurement in a zero external magnetic field. The observed 153Eu NMR signals of a magnetic divalent state and Eu,153151 NQR signals of a nonmagnetic trivalent state clearly demonstrate that the spins order in the hexagonal basal plane and the internal magnetic field is not canceled out, even at the Eu3 + layers which are in the middle of magnetic Eu2 + layers. In addition, the observation of 31P and 195Pt NMR spectra allowed us to discuss a possible magnetic structure. We also evaluated the nuclear quadrupole frequencies for both Eu2 + and Eu3 + ion states.

  6. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1990-01-01

    The primary objective of the project is to investigate the magnetic nature of the higher alcohol synthesis catalyst-Cu/Co supported on specific supports: chromia and titania with and without an alkali metal promoter, and examine the relations between catalytic ad magnetic properties. The preliminary attempts made with cobalt/copper ratio 5:8, and high metal loading in the 30--50% range showed neither copper NQR signals nor cobalt NMR signals. This leads us to believe that in the samples examined, both cobalt and copper were in the oxidic form (CoO, Co{sub 3}O{sub 4}, CuO) or copper was completely reduced while cobalt remained as an oxide. This third possibility was the formation of different spinels AB{sub 2}O{sub 4} of copper and cobalt with titanium. The final questions was the appropriateness and effectiveness of the closed system reduction procedure. 8 refs., 2 tabs.

  7. Studies of Ga NMR and NQR in SrGa4

    NASA Astrophysics Data System (ADS)

    Niki, H.; Higa, N.; Nakamura, S.; Kuroshima, H.; Toji, T.; Yogi, M.; Nakamura, A.; Hedo, M.; Nakama, T.; Ōnuki, Y.; Harima, H.

    2015-04-01

    In order to microscopically investigate the properties in SrGa4, the Ga NMR measurements of a powder sample were carried out. The Ga NMR spectra corresponding to Ga(I) and Ga(II) sites are obtained. The NMR spectra of 69&71Ga (a nuclear spin I = 3/2) in the powder sample of SrGa4 do not take a typical powder pattern caused by the NQR interaction, but take the spectra consisting of three well resolved resonance-lines, which indicates that the nonuniform distribution of crystal orientation in the powder sample occurs because of the magnetic anisotropy. From the analysis of the Ga NMR spectrum, it is found that the ab-plane of the crystal is parallel to the external magnetic field, which would be attributed to the anisotropy of the magnetic susceptibility with the easy axis parallel to the ab-plane. This result is also confirmed by the 69Ga NQR in SrGa4. The Knight shifts of the 69Ga(I) and 69Ga(II) shift slightly to the negative side with decreasing temperature due to the core polarization of the d-electrons. The values of the Knight shift of the 69Ga(I) and 69Ga(II) are 0.01 and -0.11 % at 4.2 K, and 0.09 and -0.08 % at 300 K, respectively. The values of the 1/ T 1 T of the NMR of both 69Ga(I) and 69Ga(II) are almost constant between 4.2 and 100 K, whose values are 1.5 s -1 K -1 at 69Ga(I) and 0.12 s -1 K -1 at 69Ga(II), while the 1/ T 1 T slightly increase above 100K with increasing temperature. The value of T 1 of 69Ga(I) is one order of magnitude less than that of 69Ga(II).

  8. 35Cl NQR and 1H NMR Studies of Molecular Motions in Guanidinium Salt of Chloroacetic Acid

    NASA Astrophysics Data System (ADS)

    Zdanowska-Fnjczek, Maria; Grottel, Małgorzata; Jakubas, Ryszard

    1998-07-01

    Multinuclear NQR and NMR techniques have been applied in order to study the molecular dynamics in [C(NH2)3](ClH2CCOO). The 35Cl NQR frequency was measured over a wide range of temperature. The experimental results were described by using the theories of Bayer and Brown which take into account the torsional oscillations of the CClH2 -group of the anion. A study of the proton NMR second moment as well as relaxation times T1, and T1p performed in a wide temperature range revealed an onset of the guanidinium cation reorientation around its two-fold symmetry axis. Activation parameters for this motion were determined.

  9. Ab initio DFT study of bisphosphonate derivatives as a drug for inhibition of cancer: NMR and NQR parameters.

    PubMed

    Aghabozorg, Hussein; Sohrabi, Beheshteh; Mashkouri, Sara; Aghabozorg, Hamid Reza

    2012-03-01

    DFT computations were carried out to characterize the (17)Oand (2)H electric field gradient, EFG, in various bisphosphonate derivatives. The computations were performed at the B3LYP level with 6-311++G (d,P) standard basis set. Calculated EFG tensors were used to determine the (17)O and (2)H nuclear quadrupole coupling constant, χ and asymmetry parameter, η. For better understanding of the bonding and electronic structure of bisphosphonates, isotropic and anisotropic NMR chemical shieldings were calculated for the (13)C, (17)O and (31)P nuclei using GIAO method for the optimized structure of intermediate bisphosphonates at B3LYP level of theory using 6-311++G (d, p) basis set. The results showed that various substituents have a strong effect on the nuclear quadrupole resonance (NQR) parameters (χ, η) of (17)O in contrast with (2)H NQR parameters. The NMR and NQR parameters were studied in order to find the correlation between electronic structure and the activity of the desired bisphosphonates. In addition, the effect of substitutions on the bisphosphonates polarity was investigated. Molecular polarity was determined via the DFT calculated dipole moment vectors and the results showed that substitution of bromine atom on the ring would increase the activity of bisphosphonates.

  10. Unconventional Pairing States in Heavy-Fermion Superconductors Studied by the NQR/NMR Experiments

    NASA Astrophysics Data System (ADS)

    Kitaoka, Yoshio; Mukuda, Hidekazu; Yashima, Mitsuharu; Harada, Atsushi

    2007-05-01

    We review the studies on the unconventional superconducting pairing states and their relevance with magnetism in the f-electron derived heavy-fermion (HF) systems by means of nuclear-magnetic-resonance (NMR) and nuclear-quadrupole-resonance (NQR). These studies have unraveled a rich variety of the phenomena in the ground state of HF systems. In this article, we address an intimate relationship between the onset of strong-coupling superconductivity (SC) and critical magnetic fluctuations emerging in the vicinity of quantum critical point (QCP). Furthermore, we focus on the novel phase diagram of the HF antiferromagnet CeRhIn5 under pressure which is characterized by the tetracritical point separating the pure antiferromagnetism (AFM) phase, the AFM+SC uniformly coexisting phase, and the paramagnetic SC phase. A comparison is also presented on the AFM+SC uniformly coexisting phase in high-temperature superconductors as the function of carrier doping. As a consequence, we raise a question; Do we need a bosonic glue to pair electrons in these superconductors? Finally, we address a possible origin of the novel SC in the itinerant ferromagnet UGe2, which is mediated by ferromagnetic spin-density fluctuations relevant with the first-order transition inside the ferromagnetic states.

  11. Structural and dynamic characterization of solid furosemide polymorphs by NQR and NMR methods

    NASA Astrophysics Data System (ADS)

    Wolfenson, A.; Pérez, S. C.; Zuriaga, Mariano J.; Garnero, Claudia; Miranda, J. Abraham; Longhi, Marcela; Faudone, S. N.

    2015-11-01

    The temperature dependence of NQR parameters and proton spin-lattice relaxation times of furosemide in forms 1 and 2 are reported. The NQR line shape shows that form 2 is disordered, even at low temperatures and reorientation of the SO2NH2 group between conformers has been detected above 120 K. Through T1H measurements a transition of form 2 to the high temperature phase of furosemide is observed around 405 K. The high temperature phase is characterized by one NQR line indicating Z‧ = 1 in this phase. Proton transfer and NH2 jumps in form 1 are also observed through T1Q measurements.

  12. QUEST-QUadrupolar Exact SofTware: a fast graphical program for the exact simulation of NMR and NQR spectra for quadrupolar nuclei.

    PubMed

    Perras, Frédéric A; Widdifield, Cory M; Bryce, David L

    2012-01-01

    We present a new program for the exact simulation of solid-state NMR spectra of quadrupolar nuclei in stationary powdered samples which employs diagonalization of the combined Zeeman-quadrupolar Hamiltonian. The program, which we call QUEST (QUadrupolar Exact SofTware), can simulate NMR spectra over the full regime of Larmor and quadrupolar frequency ratios, which encompasses scenarios ranging from high-field NMR to nuclear quadrupole resonance (NQR, where the Larmor frequency is zero) and does not make use of approximations when treating the quadrupolar interaction. With the use of the fast powder averaging scheme of Alderman, Solum, and Grant, exact NMR spectral simulations are only marginally slower than the second-order perturbation theory counterpart. The program, which uses a graphical user interface, also incorporates chemical shift anisotropy and non-coincident chemical shift and quadrupolar tensor frames. The program is validated against newly-acquired experimental data through several examples including: the low-field (79/81)Br NMR spectra of CaBr(2), the (14)N overtone NMR spectrum of glycine, the (187)Re NQR spectra of Re(2)(CO)(10), and lastly the (127)I overtone NQR spectrum of SrI(2), which, to the best of our knowledge, represents the first direct acquisition of an overtone NQR spectrum for a powdered sample. Copyright © 2012 Elsevier Inc. All rights reserved.

  13. Chemical structure and intra-molecular effects on NMR-NQR tensors of harmine and harmaline alkaloids

    NASA Astrophysics Data System (ADS)

    Ahmadinejad, Neda; Tahan, Arezoo; Talebi Tari, Mostafa

    2016-02-01

    Density functional theory (DFT) methods were used to analyze the effects of molecular structure and ring currents on the NMR chemical shielding tensors and NQR frequencies of harmine and harmaline alkaloids in the gas phase. The results demonstrated that NMR tensors and NQR frequencies of 15N nuclei in these compounds depend on chemical environment and resonance interactions. Hence, their values are obviously different in the mentioned structures. The interpretation of natural bond orbital (NBO) data suggests that in harmine structure, the lone pair participation of N9 in π-system electron clouds causes to development of aromaticity nature in pyrrole ring. However, the chemical shielding around N9 atom in harmine structure is higher than in harmaline, while in harmaline structure, lone pair participation of N2 in π-system electron clouds causes to development of aromaticity nature in pyridine ring. Hence, chemical shielding around N2 atom in harmaline structure is higher than in harmine. It can be deduced that by increasing lone pair electrons contribution of nitrogen atoms in ring resonance interactions and aromaticity development, the values of NMR chemical shielding around them increase, while χ and q zz values of these nuclei decrease.

  14. Coexistence of multiple charge-density waves and superconductivity in SrPt2As2 revealed by 75As-NMR /NQR and 195Pt-NMR

    NASA Astrophysics Data System (ADS)

    Kawasaki, Shinji; Tani, Yoshihiko; Mabuchi, Tomosuke; Kudo, Kazutaka; Nishikubo, Yoshihiro; Mitsuoka, Daisuke; Nohara, Minoru; Zheng, Guo-qing

    2015-02-01

    The relationship between charge-density wave (CDW) orders and superconductivity in arsenide superconductor SrPt2As2 with Tc=5.2 K which crystallizes in the CaBe2Ge2 -type structure was studied by 75As nuclear magnetic resonance (NMR) measurements up to 520 K, and 75As nuclear quadrupole resonance (NQR) and 195Pt-NMR measurements down to 1.5 K. At high temperature, 75As-NMR spectrum and nuclear-spin-relaxation rate (1 /T1) have revealed two distinct CDW orders, one realized in the As-Pt-As layer below TCDWAs (1 )=410 K and the other in the Pt-As-Pt layer below TCDWAs (2 )=255 K . The 1 /T1 measured by 75As-NQR shows a clear Hebel-Slichter peak just below Tc and decreases exponentially well below Tc. Concomitantly, 195Pt Knight shift decreases below Tc. Our results indicate that superconductivity in SrPt2As2 is in the spin-singlet state with an s -wave gap and is robust under the two distinct CDW orders in different layers.

  15. Spin and charge dynamics in lightly doped CuO and La{sub 2}CuO{sub 4} from NMR, NQR, and {mu}{sup +}SR

    SciTech Connect

    Borsa, F.; Carretta, P.; Cintolesi, F.

    1995-05-01

    The effects induced by charge defects on the spin dynamics and on the static properties of antiferromagnetic cuprates, as detected through NMR-NQR and {mu}{sup +}SR, are addressed. Information on hole localization and evidence supporting hole segregation are presented.

  16. sup 139 La NMR and NQR study of the temperature dependent structure of La sub 2 CuO sub 4+. delta

    SciTech Connect

    Hammel, P.C.; Ahrens, E.T.; Reyes, A.P.; Heffner, R.H.; Canfield, P.C.; Cheong, S-W; Fisk, Z. ); Schirber, J.E. )

    1991-01-01

    NMR and NQR reveal substantial structural changes in the metallic phase of LA{sub 2}CuO{sub 4+}{delta} which occur below 220 K. The oxygen octahedra in the metallic phase are not tilted at phase separation; upon cooling to 40 K considerable tilt has developed. The low temperature structure is highly disordered. 4 refs., 2 figs.

  17. Phase Transitions in CsSnCl3 and CsPbBr3 An NMR and NQR Study

    NASA Astrophysics Data System (ADS)

    Sharma, Surendra; Weiden, Norbert; Weiss, Alarich

    1991-04-01

    The phase transitions in CsSnCl3 and CsPbBr3 have been studied by X-ray powder diffraction, by 81Br-NQR and by 'H-, 119Sn-, and 113Cs-NMR. At room temperature in air CsSnCl3 forms a hydrate which can be dehydrated to the monoclinic phase II of CsSnCl3. The high temperature phase I has the Perovskite structure, as the X-ray and NMR experiments show. The three phases of CsPbBr3, known from literature, have been corroborated. The results are discussed in the framework of the group ABX3, A = alkalimetal ion, B = IV main group ion, and X = Halogen ion

  18. 75As NQR and NMR Studies on the Superconducting State of Ca10Pt4As8(Fe1-xPtxAs)10

    NASA Astrophysics Data System (ADS)

    Kobayashi, Yoshiaki; Iida, Takefumi; Suzuki, Kazunori; Kawamata, Takayuki; Itoh, Masayuki; Sato, Masatoshi

    2014-01-01

    75As NQR and NMR measurements of Ca10Pt4As8(Fe1-xPtxAs)10 with the superconducting transition temperature Tc = 33.4 K have been carried out. The observed 75As NQR spectra can be divided into those from As sites in (Fe1-xPtx)As and PtAs2 layers. From the NQR spectra of 75As in the (Fe1-xPtxAs) layers, x is found to be ~20%, indicating that the superconductivity is robust against nonmagnetic impurities. This contradicts the existence of the sign reversal of the order parameter in the system. The 75As nuclear spin-lattice relaxation rates 1/T1's from the (Fe1-xPtx)As and PtAs2 layers indicate that the PtAs2 layers are in a nonmetallic state and do not contribute to the occurrence of the superconductivity.

  19. Ferromagnetic Spin Fluctuation and Unconventional Superconductivity in Rb2Cr3As3 Revealed by 75As NMR and NQR

    NASA Astrophysics Data System (ADS)

    Yang, J.; Tang, Z. T.; Cao, G. H.; Zheng, Guo-qing

    2015-10-01

    We report 75As nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) studies on the superconductor Rb2Cr3As3 with a quasi-one-dimensional crystal structure. Below T ˜100 K , the spin-lattice relaxation rate (1 /T1 ) divided by temperature, 1 /T1T , increases upon cooling down to Tc=4.8 K , showing a Curie-Weiss-like temperature dependence. The Knight shift also increases with decreasing temperature. These results suggest ferromagnetic spin fluctuation. In the superconducting state, 1 /T1 decreases rapidly below Tc without a Hebel-Slichter peak, and follows a T5 variation below T ˜3 K , which points to unconventional superconductivity with point nodes in the gap function.

  20. Ferromagnetic Spin Fluctuation and Unconventional Superconductivity in Rb2Cr3As3 Revealed by 75As NMR and NQR.

    PubMed

    Yang, J; Tang, Z T; Cao, G H; Zheng, Guo-Qing

    2015-10-02

    We report (75)As nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) studies on the superconductor Rb(2)Cr(3)As(3) with a quasi-one-dimensional crystal structure. Below T∼100  K, the spin-lattice relaxation rate (1/T(1)) divided by temperature, 1/T(1)T, increases upon cooling down to T(c)=4.8  K, showing a Curie-Weiss-like temperature dependence. The Knight shift also increases with decreasing temperature. These results suggest ferromagnetic spin fluctuation. In the superconducting state, 1/T(1) decreases rapidly below T(c) without a Hebel-Slichter peak, and follows a T(5) variation below T∼3  K, which points to unconventional superconductivity with point nodes in the gap function.

  1. NMR and NQR parameters of the SiC-doped on the (4,4) armchair single-walled BPNT: a computational study.

    PubMed

    Baei, Mohammad T; Sayyad-Alangi, S Zahra; Moradi, Ali Varasteh; Torabi, Parviz

    2012-03-01

    The structural properties, NMR and NQR parameters in the pristine and silicon carbide (SiC) doped boron phosphide nanotubes (BPNTs) were calculated using DFT methods (BLYP, B3LYP/6-31G) in order to evaluate the influence of SiC-doped on the (4,4) armchair BPNTs. Nuclear magnetic resonance (NMR) parameters including isotropic (CS(I)) and anisotropic (CS(A)) chemical shielding parameters for the sites of various (13)C, (29)Si, (11)B, and (31)P atoms and quadrupole coupling constant (C ( Q )), and asymmetry parameter (η ( Q )) at the sites of various (11)B nuclei were calculated in pristine and SiC- doped (4,4) armchair boron phosphide nanotubes models. The calculations indicated that doping of (11)B and (31)P atoms by C and Si atoms had a more significant influence on the calculated NMR and NQR parameters than did doping of the B and P atoms by Si and C atoms. In comparison with the pristine model, the SiC- doping in Si(P)C(B) model of the (4,4) armchair BPNTs reduces the energy gaps of the nanotubes and increases their electrical conductance. The NMR results showed that the B and P atoms which are directly bonded to the C atoms in the SiC-doped BPNTs have significant changes in the NMR parameters with respect to the B and P atoms which are directly bonded to the Si atoms in the SiC-doped BPNTs. The NQR results showed that in BPNTs, the B atoms at the edges of nanotubes play dominant roles in determining the electronic behaviors of BPNTs. Also, the NMR and NQR results detect that the Fig. 1b (Si(P)C(B)) model is a more reactive material than the pristine and the Fig. 1a (Si(B)C(p)) models of the (4,4) armchair BPNTs.

  2. Electronic properties of Y-Ba-Cu-O superconductors as seen by Cu and O NMR/NQR

    NASA Technical Reports Server (NTRS)

    Brinkmann, D.

    1995-01-01

    Nuclear Magnetic Resonance (NMR) and Nuclear Quadrupole Resonance (NQR) allow the investigation of electronic properties at the atomic level. We will report on such studies of typical members of the the Y-Ba-Cu-O family such as YBa2Cu30(6 + x) (1-2-3-(6 + x)), YBa2Cu4O8 (1-2-4) and Y2Ba4Cu7015 (2-4-7) with many examples of recent work performed in our laboratory. In particular, we will deal with Knight shift and relaxation studies of copper and oxygen. We will discuss important issues of current studies such as: (1) Existence of a common electronic spin-susceptibility in the planes (and perhaps in the chains) of 1-2-4; (2) Strong evidence for the existence of a pseudo spin-gap of the antiferromagnetic fluctuations in 1-2-4 and 2-4-7; (3) Evidence for d-wave pairing in 1-2-4; (4) Strong coupling of inequivalent Cu-O planes in 2-4-7 and possible origin for the high Tc value of this compound; and (5) The possibility to describe NMR data in the framework of a charge-excitation picture.

  3. Electronic properties of Y-Ba-Cu-O superconductors as seen by Cu and O NMR/NQR

    SciTech Connect

    Brinkmann, D.

    1995-04-01

    Nuclear Magnetic Resonance (NMR) and Nuclear Quadrupole Resonance (NQR) allow the investigation of electronic properties at the atomic level. The authors will report on such studies of typical members of the the Y-Ba-Cu-O family such as YBa2Cu30(6 + x) (1-2-3-(6 + x)), YBa2Cu4O8 (1-2-4) and Y2Ba4Cu7015 (2-4-7) with many examples of recent work performed in their laboratory. In particular, they will deal with Knight shift and relaxation studies of copper and oxygen. They will discuss important issues of current studies such as: (1) Existence of a common electronic spin-susceptibility in the planes (and perhaps in the chains) of 1-2-4; (2) Strong evidence for the existence of a pseudo spin-gap of the antiferromagnetic fluctuations in 1-2-4 and 2-4-7; (3) Evidence for d-wave pairing in 1-2-4; (4) Strong coupling of inequivalent Cu-O planes in 2-4-7 and possible origin for the high Tc value of this compound; and (5) The possibility to describe NMR data in the framework of a charge-excitation picture.

  4. (121,123)Sb and (75)As NMR and NQR investigation of the tetrahedrite (Cu12Sb4S13)--Tennantite (Cu12As4S13) system and other metal arsenides.

    PubMed

    Bastow, T J; Lehmann-Horn, J A; Miljak, D G

    2015-10-01

    This work is motivated by the recent developments in online minerals analysis in the mining and minerals processing industry via nuclear quadrupole resonance (NQR). Here we describe a nuclear magnetic resonance (NMR) and NQR study of the minerals tennantite (Cu12As4S13) and tetrahedrite (Cu12 Sb4S13). In the first part NQR lines associated with (75)As in tennantite and (121,123)Sb isotopes in tetrahedrite are reported. The spectroscopy has been restricted to an ambient temperature studies in accord with typical industrial conditions. The second part of this contribution reports nuclear quadrupole-perturbed NMR findings on further, only partially characterised, metal arsenides. The findings enhance the detection capabilities of NQR based analysers for online measurement applications and may aid to control arsenic and antimony concentrations in metal processing stages. Crown Copyright © 2015. Published by Elsevier Inc. All rights reserved.

  5. Volovik effect and Fermi-liquid behavior in the s -wave superconductor CaPd2As2: 75As NMR-NQR measurements

    NASA Astrophysics Data System (ADS)

    Ding, Q.-P.; Wiecki, P.; Anand, V. K.; Sangeetha, N. S.; Lee, Y.; Johnston, D. C.; Furukawa, Y.

    2016-04-01

    The electronic and magnetic properties of the collapsed-tetragonal CaPd2As2 superconductor (SC) with a transition temperature of 1.27 K have been investigated by 75As nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements. The temperature (T ) dependence of the nuclear spin lattice relaxation rates (1 /T1) and the Knight shifts indicate the absence of magnetic correlations in the normal state. In the SC state, 1 /T1 measured by 75As NQR shows a clear Hebel-Slichter (HS) peak just below Tc and decreases exponentially at lower T , confirming a conventional s -wave SC. In addition, the Volovik effect, also known as the Doppler shift effect, has been clearly evidenced by the observation of the suppression of the HS peak with applied magnetic field.

  6. Volovik effect and Fermi-liquid behavior in the s-wave superconductor CaPd2As2: As75 NMR-NQR measurements

    DOE PAGES

    Ding, Q. -P.; Wiecki, P.; Anand, V. K.; ...

    2016-04-07

    The electronic and magnetic properties of the collapsed-tetragonal CaPd2As2 superconductor (SC) with a transition temperature of 1.27 K have been investigated by 75As nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements. The temperature (T) dependence of the nuclear spin lattice relaxation rates (1/T1) and the Knight shifts indicate the absence of magnetic correlations in the normal state. In the SC state, 1/T1 measured by 75As NQR shows a clear Hebel-Slichter (HS) peak just below Tc and decreases exponentially at lower T, confirming a conventional s-wave SC. Additionally, the Volovik effect, also known as the Doppler shift effect, hasmore » been clearly evidenced by the observation of the suppression of the HS peak with applied magnetic field.« less

  7. Glass Structure by Scattering Methods and Spectroscopy — C. NUCLEAR QUADRUPOLE RESONANCE (NQR) STUDIES OF GLASS STRUCTURE

    NASA Astrophysics Data System (ADS)

    Bray, Philip J.

    The following sections are included: * Introduction * NMR Spectroscopy with Quadrupolar Effects * Zeeman and quadrupole interactions * First-order quadrupolar effects * Second-order quadrupolar effects * Case of a small asymmetry parameter * Case of a large(r) asymmetry parameter * Use of computer simulation to extract values of Qcc and η * Consequences of overlap of NMR spectra * NQR Spectroscopy * Genesis of spectra * Discovery of NQR * Instrumentation and procedures * NQR of particular nuclei in inorganic solids * 75As NQR * 11B NQR * 10B NQR * 27Al NQR * NQR of polymers * NQR with a Zeeman perturbation * Acknowledgments * References

  8. Polymorphism and disorder in natural active ingredients. Low and high-temperature phases of anhydrous caffeine: Spectroscopic ((1)H-(14)N NMR-NQR/(14)N NQR) and solid-state computational modelling (DFT/QTAIM/RDS) study.

    PubMed

    Seliger, Janez; Žagar, Veselko; Apih, Tomaž; Gregorovič, Alan; Latosińska, Magdalena; Olejniczak, Grzegorz Andrzej; Latosińska, Jolanta Natalia

    2016-03-31

    The polymorphism of anhydrous caffeine (1,3,7-trimethylxanthine; 1,3,7-trimethyl-1H-purine-2,6-(3H,7H)-dione) has been studied by (1)H-(14)N NMR-NQR (Nuclear Magnetic Resonance-Nuclear Quadrupole Resonance) double resonance and pure (14)N NQR (Nuclear Quadrupole Resonance) followed by computational modelling (Density Functional Theory, supplemented Quantum Theory of Atoms in Molecules with Reduced Density Gradient) in solid state. For two stable (phase II, form β) and metastable (phase I, form α) polymorphs the complete NQR spectra consisting of 12 lines were recorded. The assignment of signals detected in experiment to particular nitrogen sites was verified with the help of DFT. The shifts of the NQR frequencies, quadrupole coupling constants and asymmetry parameters at each nitrogen site due to polymorphic transition were evaluated. The strongest shifts were observed at N(3) site, while the smallest at N(9) site. The commercial pharmaceutical sample was found to contain approximately 20-25% of phase I and 75-80% of phase II. The orientational disorder in phase II with a local molecular arrangement mimics that in phase I. Substantial differences in the intermolecular interaction phases I and II of caffeine were analysed using computational (DFT/QTAIM/RDS) approach. The analysis of local environment of each nitrogen nucleus permitted drawing some conclusions on the topology of interactions in both polymorphs. For the most stable orientations in phase I and phase II the maps of the principal component qz of EFG tensor and its asymmetry parameter at each point of the molecular system were calculated and visualized. The relevant maps calculated for both phases I and II indicates small variation in electrostatic potential upon phase change. Small differences between packings in phases slightly disturb the neighbourhood of the N(1) and N(7) nitrogens, thus are meaningless from the biological point of view. The composition of two phases in pharmaceutical material

  9. A study of transition-metal organometallic complexes combining 35Cl solid-state NMR spectroscopy and 35Cl NQR spectroscopy and first-principles DFT calculations.

    PubMed

    Johnston, Karen E; O'Keefe, Christopher A; Gauvin, Régis M; Trébosc, Julien; Delevoye, Laurent; Amoureux, Jean-Paul; Popoff, Nicolas; Taoufik, Mostafa; Oudatchin, Konstantin; Schurko, Robert W

    2013-09-09

    A series of transition-metal organometallic complexes with commonly occurring metal-chlorine bonding motifs were characterized using (35)Cl solid-state NMR (SSNMR) spectroscopy, (35)Cl nuclear quadrupole resonance (NQR) spectroscopy, and first-principles density functional theory (DFT) calculations of NMR interaction tensors. Static (35)Cl ultra-wideline NMR spectra were acquired in a piecewise manner at standard (9.4 T) and high (21.1 T) magnetic field strengths using the WURST-QCPMG pulse sequence. The (35)Cl electric field gradient (EFG) and chemical shielding (CS) tensor parameters were readily extracted from analytical simulations of the spectra; in particular, the quadrupolar parameters are shown to be very sensitive to structural differences, and can easily differentiate between chlorine atoms in bridging and terminal bonding environments. (35)Cl NQR spectra were acquired for many of the complexes, which aided in resolving structurally similar, yet crystallographically distinct and magnetically inequivalent chlorine sites, and with the interpretation and assignment of (35)Cl SSNMR spectra. (35)Cl EFG tensors obtained from first-principles DFT calculations are consistently in good agreement with experiment, highlighting the importance of using a combined approach of theoretical and experimental methods for structural characterization. Finally, a preliminary example of a (35)Cl SSNMR spectrum of a transition-metal species (TiCl4) diluted and supported on non-porous silica is presented. The combination of (35)Cl SSNMR and (35)Cl NQR spectroscopy and DFT calculations is shown to be a promising and simple methodology for the characterization of all manner of chlorine-containing transition-metal complexes, in pure, impure bulk and supported forms. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1991-12-17

    Our previous studies (1,2) on the zerofield NMR spectra of Cu/Co catalysts revealed that the method of preparation sensitively influences the magnetic character of the Catalyst. Catalytic studies of the earlier investigators also (3) show similar influence on the product selectivity and indicate reproducible performance is critically dependent on the control and rigor of the preparation technique. To compliment the NMR results, we have made a thorough investigation of the Hysteresis character of the Cu/Co catalysts with the metal ratio varying from 0.2 to 4.0.

  11. Antiferromagnetic properties of a water-vapor-inserted YBa2 Cu3 O6.5 compound studied byNMR, NQR, and μSR

    NASA Astrophysics Data System (ADS)

    Dooglav, A. V.; Egorov, A. V.; Mukhamedshin, I. R.; Savinkov, A. V.; Alloul, H.; Bobroff, J.; Macfarlane, W. A.; Mendels, P.; Collin, G.; Blanchard, N.; Picard, P. G.; King, P. J. C.; Lord, J.

    2004-08-01

    We present a detailed NQR, nuclear magnetic resonance (NMR), and μSR study of the magnetic phase obtained during a topotactic chemical reaction of YBa2Cu3O6.5 high-temperature superconductor with low-pressure water vapor. Cu65 -enriched samples have been used for NQR/NMR studies which allows to get a good resolution in the Cu(1) NQR and Cu(2) zero field NMR (ZFNMR) spectra. It is shown that the NQR spectrum of the starting material transforms progressively under insertion of water, and almost completely disappears when about one H2O molecule is inserted per unit cell. Similarly, a Cu65 ZFNMR signal characteristic of this water inserted material appears and grows with increasing water content, which indicates that the products of the reaction are nonsuperconducting antiferromagnetic phases in which the copper electronic magnetic moments in the CuO2 bilayers are ordered. The use of Cu65 -enriched samples allowed us to reliably resolve three different copper resonances which correspond to different internal magnetic fields. The antiferromagnetic phases are also felt by proton NMR which reveals two sites with static internal fields of 150 and about 15 Gauss, respectively. μSR studies performed on a series of samples prepared in the same way as the C65u -enriched ones reveal two muon sites with the same local fields as the proton sites, which vanish at T≈400K . This indicates that muons preferentially occupy proton vacancy sites, and that the magnetic phases have similar Néel temperatures as the other bilayer undoped cuprate compounds. An analysis of the internal fields on the different spin probes suggests that they can be all assigned to a single magnetic phase at large water content in which the Cu(1) electron spins order with those of the Cu(2) . The detailed evolution of the spectra with the progressive increase of water content is shown to be compatible with a coexistence of phases during the early stages ot the reaction. It appears that even samples packed

  12. Antiferromagnetic order in the ladder compound SrCu{sub 2}O{sub 3}: Cu-NMR/NQR measurements

    SciTech Connect

    Ohsugi, S.; Kitaoka, Y.; Azuma, M.; Fujishiro, Y.; Takano, M.

    1999-12-01

    The authors carried out the extensive Cu-nuclear magnetic and quadrupole resonance (NMR/NQR) experiments on the Zn(Ni)-doped ladder compound SrCu{sub 2}O{sub 3} (Sr123), Sr(Cu{sub 1{minus}x}M{sub x}){sub 2}O{sub 3} (M = Zn and Ni) with x {le} 0.02 and the La-doped Sr123, Sr{sub 1{minus}x}La{sub x}Cu{sub 2}O{sub 3} with {alpha} {le} 0.03. A spin-correlation length {xi}{sub s}/a (a: the lattice spacing between the Cu sites along the leg) of nonmagnetic impurity-induced staggered polarization (IISP) estimated from a quasi-one-dimensional (Q1D) IISP along the two legs in the 0.1--2% Zn-doped Sr123 was found to be independent of temperature (T) and scaled to an mean impurity distance D{sub AV} with the relation of {xi}{sub s}/a = 2.5 + D{sub AV}. The {xi}{sub s}/a's are much longer in x = 0.001 ({xi}{sub s}/a {approximately} 50) and 0.005 ({xi}{sub s}/a {approximately} 12) than an instantaneous spin-correlation length {xi}{sub 0}/a {approximately} 3--8 in Sr123. The formula of Neel T, T{sub N} (WC-Q1D) = J exp({minus}D{sub AV}/({xi}{sub s}/a)) (J = 2,000 K) based on the weakly interladder-coupled (WC) Q1D model explains the experimental T{sub N} values quantitatively.

  13. Copper Nqr and NMR Study of Metal-Substituted Yttrium BARIUM(2) COPPER(3) OXYGEN(7) and Yttrium BARIUM(2) COPPER(4) OXYGEN(8)

    NASA Astrophysics Data System (ADS)

    Cheng, Show-Jye

    Pulsed nuclear quadrupole resonance (NQR) and nuclear magnetic resonance (NMR) have been used to investigate the effect of metal-substitution for copper in YBa_2Cu_3O_7 (YBCO123) and YBa_2Cu_4O_8 (YBCO124). Among many metal substitutions, Zn has an especially dramatic effect in suppressing the superconducting temperature T_{c}, and hence superconductivity. More interesting is that Zn and Fe have the same T_{c} suppression effect in YBCO124. This study focuses on the Zn substitutions in YBCO123 and Zn, Fe, and Co substitutions in YBCO124. In Zn doped YBCO123, Cu(2), plane site, NQR spectra and the frequency dependence of the spin-lattice relaxation rates have been measured over a temperature range from 77 K to 300 K to study the correlation of the suppression of the relaxation rate with the distance between the probe Cu nuclei and the impurity. It is found that the relaxation rate is insensitive to the variation of the NQR resonance frequency. However, by comparing the results of the Zn doped YBCO124 with those of YBCO123, it can be concluded that the suppression of the relaxation rate for both YBCO compounds in the normal state is caused by destruction of short-range antiferromagnetic correlation with substitution of nonmagnetic ion Zn on the Cu(2) sites. NQR and NMR measurements were carried out on both Cu(2), plane, and Cu(1), chain sites, for various concentrations of Zn, Fe, and Co dopants in YBCO124 over a temperature range from 77 K to 300 K. A strong correlation of the enhancement of Cu(2) spin lattice relaxation rate and suppression of superconductivity by impurities was found. The temperature dependence of the Cu(2) NMR linewidth exhibits a strong RKKY type exchange interaction below 225 K for Zn and Fe doped samples, which indicates the formation of the local magnetic moment. The enhancement of the relaxation rate is caused by the local magnetic moment Fe^ {+3} ion and the moments on Cu(2) neighbors when Zn^{+2} is substituted on Cu(2). This study gives

  14. NMR and NQR study of the electronic and structural properties of Al-Cu-Fe and Al-Cu-Ru quasicrystals

    SciTech Connect

    Shastri, A.; Borsa, F.; Torgeson, D.R.; Shield, J.E.; Goldman, A.I. )

    1994-12-01

    [sup 27]Al and [sup 63,65]Cu NMR is reported for powdered stable Al-Cu-Fe and Al-Cu-Ru icosahedral quasicrystals and crystalline approximants, and for an Al-Pd-Mn single-grain quasicrystal. [sup 27]Al NQR spectra at 4.2 K were observed in Al-Cu-Fe and Al-Cu-Ru samples. From quadrupole-perturbed NMR spectra at different magnetic fields, and from zero-field NQR spectra, a wide distribution of local electric-field gradient (EFG) tensor components and principal-axis-system orientations was found at the Al site. A model EFG calculation based on a 1/1 Al-Cu-Fe approximant successfully explained the observed NQR spectra. The average local gradient is largely determined by the [ital p]-electron wave function at the Al site, while the width of the distribution is due to EFG lattice contribution. Comparison of [sup 63]Cu and [sup 27]Al NMR shows the EFG distribution at the two sites is similar, but the electronic contribution to the EFG is considerably smaller at the Cu site, in agreement with a more [ital s]-type wave function of the conduction electrons. Overall spread of EFG values is well reproduced by calculation based on the approximant. However, the experimental spectra indicate a much larger number of nonequivalent sites when compared with the simulated NQR spectra based on the 1/1 approximant. The short-range, local chemical order is well represented by the approximant, but differences in coordination must be included at intermediate range in the quasicrystal. Measured [sup 27]Al Knight shift, magnetic susceptibility, and nuclear spin-lattice relaxation time as a function of temperature indicate reduced density of states at the Fermi level by a factor of 7 or 8 from the value in Al metal, consistent with the notion of a pseudogap for these quasicrystals. No differences in measured parameters were detected as a function of composition of the quasicrystalline alloys.

  15. NQR and NMR studies of YBa/sub 2/Cu/sub 3/O/sub x/ (6. 0 /le/ x /le/ 6. 91)

    SciTech Connect

    Imai, T.; Shimizu, T.; Yasuoka, H.; Ueda, Y.; Kosuge, K.

    1989-01-01

    Nuclear Quadrupole Resonance (NQR) and Nuclear Magnetic Resonance (NMR) have been utilized to investigate the 90 K class superconductor YBa/sub 2/Cu/sub 3/O/sub 6.91/ and relevant oxides YBa/sub 2/Cu/sub 3/O/sub chi/(6.0/le/chi/le/6.91). Two/sup 63/Cu NQR lines have been observed at about 31 MHz and 22 MHz for chi = 6.91, which were proved to be from the Cu2 and Cu1 sites respectively using the NMR technique for an oriented sample. The spin-lattice relaxation time T/sub 1/ exhibits anomalous temperature dependence with high relaxation rate in the normal state. Power-law like temperature dependence was observed well below T/sub c/ for the Cu2 sites. The former indicates the strong influence of Cu spin fluctuations, while the latter may be understood as the realization of the anisotropic superconductivity. Antiferromagnetic nuclear resonance has been obtained for chi = 6.0 yielding a clear evidence of magnetic ordering in the Cu2-O/sub 2/ planes. This is consistent with neutron scattering and /mu/ SR studies.

  16. Suppression of electron correlations in the collapsed tetragonal phase of CaFe2As2 under ambient pressure demonstrated by As75 NMR/NQR measurements

    NASA Astrophysics Data System (ADS)

    Furukawa, Y.; Roy, B.; Ran, S.; Bud'ko, S. L.; Canfield, P. C.

    2014-03-01

    The static and the dynamic spin correlations in the low-temperature collapsed tetragonal and the high-temperature tetragonal phase in CaFe2As2 have been investigated by As75 nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements. Through the temperature (T) dependence of the nuclear spin lattice relaxation rates (1/T1) and the Knight shifts, although stripe-type antiferromagnetic (AFM) spin correlations are realized in the high-temperature tetragonal phase, no trace of the AFM spin correlations can be found in the nonsuperconducting, low-temperature, collapsed tetragonal (cT) phase. Given that there is no magnetic broadening in As75 NMR spectra, together with the T-independent behavior of magnetic susceptibility χ and the T dependence of 1/T1Tχ, we conclude that Fe spin correlations are completely quenched statically and dynamically in the nonsuperconducting cT phase in CaFe2As2.

  17. Suppression of electron correlations in the collapsed tetragonal phase of CaFe2As2 under ambient pressure demonstrated by As75 NMR/NQR measurements

    SciTech Connect

    Furukawa, Yuji; Roy, Beas; Ran, Sheng; Budko, Sergey L.; Canfield, Paul C.

    2014-03-20

    The static and the dynamic spin correlations in the low-temperature collapsed tetragonal and the high-temperature tetragonal phase in CaFe2As2 have been investigated by As75 nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements. Through the temperature (T) dependence of the nuclear spin lattice relaxation rates (1/T1) and the Knight shifts, although stripe-type antiferromagnetic (AFM) spin correlations are realized in the high-temperature tetragonal phase, no trace of the AFM spin correlations can be found in the nonsuperconducting, low-temperature, collapsed tetragonal (cT) phase. Given that there is no magnetic broadening in As75 NMR spectra, together with the T-independent behavior of magnetic susceptibility χ and the T dependence of 1/T1Tχ, we conclude that Fe spin correlations are completely quenched statically and dynamically in the nonsuperconducting cT phase in CaFe2As2.

  18. Hydrogen bonding and stacking pi-pi interactions in solid 6-thioguanine and 6-mercaptopurine (antileukemia and antineoplastic drugs) studied by NMR-NQR double resonance spectroscopy and density functional theory.

    PubMed

    Latosińska, J N; Seliger, J; Zagar, V; Burchardt, D V

    2009-07-30

    A chemotherapeutic drug 6-thioguanine (2-amino-1,7-dihydro-6H-purine-6-thione, 6-TG) has been studied experimentally in the solid state by NMR-NQR double resonance and theoretically by the density functional theory. Fourteen resonance frequencies on (14)N have been detected and assigned to particular nitrogen sites in the 6-TG molecule. A valid assignment of NQR frequencies for 6-mercaptopurine (6-MP) has been proposed. The effects of molecular aggregations, related to intermolecular hydrogen bonding and stacking pi-pi interactions on the NQR parameters have been analyzed within the DFT and AIM (atoms in molecules) formalism for 6-TG and 6-mercaptopurine (6-MP). The so-called global reactivity descriptors have been calculated to compare the properties of molecules of 6-TG and 6-MP, to check the effect of -NH(2) group as well as to identify the differences in crystal packing.

  19. NMR and NQR study of Si-doped (6,0) zigzag single-walled aluminum nitride nanotube as n or P-semiconductors.

    PubMed

    Baei, Mohammad T; Peyghan, Ali Ahmadi; Tavakoli, Khadijeh; Babaheydari, Ali Kazemi; Moghimi, Masoumeh

    2012-09-01

    Density functional theory (DFT) calculations were performed to investigate the electronic structure properties of pristine and Si-doped aluminum nitride nanotubes as n or P-semiconductors at the B3LYP/6-31G* level of theory in order to evaluate the influence of Si-doped in the (6,0) zigzag AlNNTs. We extended the DFT calculation to predict the electronic structure properties of Si-doped aluminum nitride nanotubes, which are very important for production of solid-state devices and other applications. To this aim, pristine and Si-doped AlNNT structures in two models (Si(N) and Si(Al)) were optimized, and then the electronic properties, the isotropic (CS(I)) and anisotropic (CS(A)) chemical shielding parameters for the sites of various (27)Al and (14)N atoms, NQR parameters for the sites of various of (27)Al and (14)N atoms, and quantum molecular descriptors were calculated in the optimized structures. The optimized structures, the electronic properties, NMR and NQR parameters, and quantum molecular descriptors for the Si(N) and Si(Al) models show that the Si(N) model is a more reactive material than the pristine or Si(Al) model.

  20. {sup 89}Y NMR and Cu NQR of hydrogenated oxygen-deficient YBa{sub 2}Cu{sub 3}O{sub 6.7}

    SciTech Connect

    Goren, S.D.; Korn, C.; Perrin, C.; Hoffmann, W.; Vieth, H.M.; Lueders, K.

    1995-08-01

    The room-temperature {sup 89}Y NMR line shift and line shape as well as the low-temperature Cu NQR lines were obtained as a function of hydrogen concentration for oxygen-depleted hydrogen-doped YBCO (H{sub {ital x}}YBa{sub 2}Cu{sub 3}O{sub 6.7}) in order to investigate the interplay of the effect of hydrogen addition and oxygen removal on the electronic structure and superconducting-antiferromagnetic transition properties. The results seem to indicate that as far as filling the conduction band is concerned, hydrogen contributes twice as many electrons as the chain oxygen contributes holes. In contrast to this, the transition from a superconductor to an antiferromagnet is governed by other considerations which favor a 1:1 ratio. It is also seen that hydrogen enters into either an additional site or a new phase when enough hydrogen is added to oxygen-depleted YBCO.

  1. Detection of {sup 14}N and {sup 35}Cl in cocaine base and hydrochloride using NQR, NMR, and SQUID techniques

    SciTech Connect

    Yesinowski, J.P.; Buess, M.L.; Garroway, A.N.; Ziegeweid, M.; Pines, A. |

    1995-07-01

    Results from {sup 14}N pure NQR of cocaine in the free base form (cocaine base) yield a nuclear quadrupole coupling constant (NQCC) e{sup 2}Qq/h of 5.0229 ({+-}0.0001) MHz and an asymmetry parameter {eta} of 0.0395 ({+-}0.0001) at 295 K, with corresponding values of 5.0460 ({+-}0.0013) MHz and 0.0353 ({+-}0.0008) at 77 K. Both pure NQR (at 295-77 K) and a superconducting quantum interference device (SQUID) detector (at 4.2 K) were used to measure the very low (<1 MHz) {sup 14}N transition frequencies in cocaine hydrochloride; at 295 K the NQCC is 1.1780 ({+-}0.0014) MHz and the asymmetry parameter is 0.2632 ({+-}0.0034). Stepping the carrier frequency enables one to obtain a powder pattern without the severe intensity distortions that otherwise arise from finite pulse power. A powder pattern simulation using an NQCC value of 5.027 MHz and an asymmetry parameter {eta} of 0.2 agrees reasonably well with the experimental stepped-frequency spectrum. The use of pure NQR for providing nondestructive, quantitative, and highly specific detection of crystalline compounds is discussed, as are experimental strategies. 31 refs., 8 figs., 1 tab.

  2. I: Low Frequency NMR and NQR Using a dc SQUID. II: Variable-temperature 13C CP/MAS of Organometallics

    SciTech Connect

    Ziegeweid, Marcia A.

    1995-11-01

    NMR and NQR at low frequencies are difficult prospects due to small nuclear spin polarization. Furthermore, the sensitivity of the inductive pickup circuitry of standard spectrometers is reduced as the frequency is lowered. I have used a cw-SQUID (Superconducting Quantum Interference Device) spectrometer, which has no such frequency dependence, to study the local atomic environment of 14N via the quadrupolar interaction. Because 14N has spin I = 1 and a 0-6 MHz frequency range, it is not possible to obtain well-resolved spectra in high magnetic fields. I have used a technique to observe 14N NQR resonances via their effect on neighboring protons mediated by the heteronuclear dipolar interaction to study peptides and narcotics. The sensitivity of the SQUID is not enough to measure low-frequency surface (or other low spin density) systems. The application of spin-polarized xenon has been previously used to enhance polarization in conventional NMR experiments. Because xenon only polarizes spins with which it is in contact, it is surface selective. While differences in chemical shifts between surface and bulk spins are not large, it is expected that the differences in quadrupole coupling constant should be very large due to the drastic change of the electric field gradient surrounding spins at the surface. With this in mind, I have taken preliminary steps to measure SQUID detected polarization transfer from Xe to another spin species at 4.2 K and in small magnetic fields (<50 G). In this regime, the spin-lattice relaxation of xenon is dependent on the applied magnetic field. The results of our efforts to characterize the relaxation of xenon are presented. The final section describes the solid-state variable-temperature (VT) one- and two-dimensional 13C cross polarization (CP)/magic angle spinning (MAS) NMR of Hf(η5-C5H5)21-C5H5)2, Zr

  3. NMR and NQR study of atomic motion below 500 K in YBa{sub 2}Cu{sub 3}O{sub 7}

    SciTech Connect

    Klein, S.P.; Wang, R.; Sleight, A.W.; Warren, W.W. Jr.

    1997-09-01

    Measurements of the intensity of the {sup 63}Cu NQR and quadrupolar-satellite NMR at elevated temperatures are reported for the planar Cu(2) sites in samples of nominal composition YBa{sub 2}Cu{sub 3}O{sub 7}. It is observed that spin-echo intensities decrease dramatically between room temperature and 500 K and that the onset of intensity loss occurs at lower temperatures in more defective samples. Measurements of the spin-echo decay rates reveal that the intensity loss is associated with loss of phase coherence exceeding that expected from spin-spin and spin-lattice relaxation. By means of a simple, illustrative model, these effects can be attributed to changes in the local atomic environment, presumed to be caused by motion of oxygen atoms in the Cu(1) layer. These motions occur on a time scale on the order of 10 {mu}s at 500 K and their probability is enhanced at lower temperatures by the presence of structural defects. {copyright} {ital 1997} {ital The American Physical Society}

  4. Doping Dependence of Normal-State Properties in Iron-Based Oxypnictide Superconductor LaFeAsO1-y Probed by 57Fe-NMR and 75As-NMR/NQR

    NASA Astrophysics Data System (ADS)

    Mukuda, Hidekazu; Terasaki, Nobuyuki; Tamura, Nobukatsu; Kinouchi, Hiroaki; Yashima, Mitsuharu; Kitaoka, Yoshio; Miyazawa, Kiichi; Shirage, Parasharam M.; Suzuki, Shinnosuke; Miyasaka, Shigeki; Tajima, Setsuko; Kito, Hijiri; Eisaki, Hiroshi; Iyo, Akira

    2009-08-01

    We report systematic 57Fe-NMR and 75As-NMR/NQR studies on an underdoped sample (Tc=20 K), an optimally doped sample (Tc=28 K), and an overdoped sample (Tc=22 K) of oxygen-deficient iron (Fe)-based oxypnictide superconductor LaFeAsO1-y. A microscopic phase separation between superconducting domains and magnetic domains is shown to take place in the underdoped sample, indicating a local inhomogeneity in association with the density distribution of oxygen deficiencies. As a result, 1/T1T in the normal state of the superconducting domain decreases significantly upon cooling at both the Fe and As sites regardless of the electron-doping level in LaFeAsO1-y. On the basis of this result, we claim that 1/T1T is not always enhanced by antiferromagnetic fluctuations close to an antiferromagnetic phase in the underdoped superconducting sample. This contrasts with the behavior in hole-doped Ba0.6K0.4Fe2As2 (Tc=38 K), which exhibits a significant increase in 1/T1T upon cooling. We remark that the crucial difference between the normal-state properties of LaFeAsO1-y and Ba0.6K0.4Fe2As2 originates from the fact that the relevant Fermi surface topologies are differently modified depending on whether electrons or holes are doped into the FeAs layers.

  5. Theoretical study addressing the effects of tautomerism and explicit/implicit water molecules on NQR and NMR parameters of tetrazole-5-thione.

    PubMed

    Tahan, Arezoo

    2017-07-01

    DFT/B3LYP calculations were employed to study the effects of tautomerism and explicit/implicit water molecules on Nuclear Quadrupole Resonance (NQR) and Nuclear Magnetic Resonance (NMR) tensors of nitrogen nuclei in tetrazole-5-thione structure. The obtained results revealed that nuclear quadrupole coupling constant (χ) and isotropic chemical shielding (σiso ) values of nitrogen nuclei in tetrazole ring of five possible tautomeric forms of tetrazole-5-thione, i.e. two thione forms called tautomers A and E and three thiol forms called tautomers B, C, and D, were functions of resonance energy(E2 ) values of nitrogen lone pairs. Furthermore, it was observed that by increasing participation of lone pairs of nitrogen atoms in the ring resonance interactions, the σiso values around them were increased, while their χ and qzz values were decreased. However, the results indicated that with exception of tautomer B, the order of qzz and χ values of nitrogen nuclei in tetrazole ring was exactly opposite of the order of resonance energy values for the same nitrogen nuclei in all tautomers and their mono-hydrated complexes. In addition, a significant decrease was noticed in χ and qzz values when a water molecule was put in different positions near the tetrazole ring in tautomers A-E. The mentioned result can be attributed to hydrogen bond formation between nitrogen nuclei and the oxygen of water. In mono-hydrated complexes, the σiso values around nitrogen atoms acting as hydrogen donors in hydrogen bond formation (N-H….OH2 ) were decreased, while its values were increased for nitrogen atoms acting as hydrogen acceptors in hydrogen bond formation(N….H-OH). Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  6. Static and dynamic structures of crystalline nAlCl 3· mCH 3CN ( n : m = 1 : 1, 2 : 3, and 1 : 2) by means of 35Cl NQR and 27Al NMR

    NASA Astrophysics Data System (ADS)

    Yamada, Koji; Watanabe, Yoshihisa; Okuda, Tsutomu

    1995-02-01

    Static and dynamic structures of crystalline AlCl 3·CH 3CN, 2AlCl 3·3CH 3CN and AlCl 3·2CH 3CN are investigated by means of 35Cl NQR and 27Al NMR spectroscopy. A neutral molecular complex Cl 3AlNCCH 3 having three-fold symmetry is found for the 1 : 1 compound, whereas the 2 : 3 and 1 : 2 crystals consist of complex ion pairs and are expressed as [Al(CH 3CN) 6] 3+·3[AlCl 4] - and [AlCl(CH 3CN) 5] 2+·2[AlCl 4] -·CH 3CN, respectively. The temperature dependences of the 35Cl NQR spectra and the spin-lattice relaxation times reveal tha the reorientation of the tetrahedral AlCl -4 anion or AlCl 3 group takes place far below their melting temperatures. 27Al NMR parameters, chemical shift and quadrupole coupling constant are consistent with these structural models.

  7. Comparative experimental analysis of composite pulses in 14N NQR.

    PubMed

    Mikhaltsevitch, V T; Rudakov, T N; Flexman, J H; Hayes, P A; Chisholm, W P

    2004-01-01

    Experimental results of comparing composite pulses in nitrogen-14 NQR, that are analogous to common 90 degrees RF pulses in powder, are presented. All tested pulses have been taken from publications in journals. Comparative diagrams of the measurement results for induction signals and echo signals are presented. The results of the measurements demonstrate that the best outcomes are achieved when the composite pulse (45)0(95)180(164)0 is used.

  8. 75As-NQR/NMR Studies on Oxygen-Deficient Iron-Based Oxypnictide Superconductors LaFeAsO1-y ( y = 0, 0.25, 0.4) and NdFeAsO0.6

    NASA Astrophysics Data System (ADS)

    Mukuda, Hidekazu; Terasaki, Nobuyuki; Kinouchi, Hiroaki; Yashima, Mitsuharu; Kitaoka, Yoshio; Suzuki, Shinnosuke; Miyasaka, Shigeki; Tajima, Setsuko; Miyazawa, Kiichi; Shirage, Parasharam; Kito, Hijiri; Eisaki, Hiroshi; Iyo, Akira

    2008-09-01

    We report 75As-NQR/NMR studies on the oxygen-deficient iron (Fe)-based oxypnictide superconductors LaFeAsO0.6 (Tc = 28 K) along with the results on LaFeAsO, LaFeAsO0.75 (Tc = 20 K), and NdFeAsO0.6 (Tc = 53 K). Nuclear spin-lattice relaxation rate 1/T1 of 75As-NQR at zero field on LaFeAsO0.6 has revealed a T3 dependence below Tc upon cooling without the coherence peak just below Tc, evidencing the unconventional superconducting state with the line-node gap. We have found an intimate relationship between the nuclear quadrupole frequency νQ of 75As and Tc for four samples used in this study. It implies microscopically that the local configuration of Fe and As atoms is significantly related to the Tc of the Fe-oxypnictide superconductors, namely, the Tc can be enhanced up to 50 K when the local configuration of Fe and As atoms is optimal, in which the band structure may be also optimized through the variation of hybridization between As 4 p orbitals and Fe 3d orbitals.

  9. 14N NQR and proton NMR study of ferroelectric phase transition and proton exchange in organic ferroelectric (H2-TPPZ)(Hca)2.

    PubMed

    Seliger, Janez; Zagar, Veselko; Asaji, Tetsuo; Hasegawa, Yumi

    2010-04-07

    The complete (14)N nuclear quadrupole resonance spectrum has been measured in ferroelectric (H(2)-TPPZ)(Hca)(2) using nuclear quadrupole double resonance. The quadrupole coupling tensors are assigned to various nitrogen positions in the crystal structure. Two types of asymmetric N-H(+)...N hydrogen bonds are observed in the ferroelectric phase. A slow dynamics influencing the (14)N NQR spectrum and relaxation has been observed in the paraelectric phase. The analysis of the (14)N NQR spectra in the paraelectric phase shows that above T(c) each hydrogen bond exchanges between the two types observed in the ferroelectric phase. The change of the type of hydrogen bond is associated with the transfer of protons within the bond.

  10. NMR and NQR study of Ca-substituted superconducting YBa{sub 2}Cu{sub 4}O{sub 8}

    SciTech Connect

    Mali, M.; Roos, J.; Brinkmann, D.

    1996-02-01

    We report a set of nuclear quadrupole resonance (NQR) measurements including a spin-echo double-resonance (SEDOR) experiment which provides convincing evidence that the additional chain Cu NQR line in Ca-substituted YBa{sub 2}Cu{sub 4}O{sub 8} does stem from chain Cu sites disturbed by the {open_quote}{open_quote}impurity{close_quote}{close_quote} Ca ions. From an analysis of signal intensities we conclude that {open_quote}{open_quote}impurity{close_quote}{close_quote} Ca ions, responsible for the additional line, substitute Y{sup 3+}. At high Ca doping, the concentration of the substituted Y sites, {ital x}{sup {prime}}, is appreciably smaller than the nominal Ca concentration, {ital x}. Since it is {ital x}{sup {prime}} which is responsible for a direct increase of the hole charge-carrier concentration, {ital n}, effects connected with the increase of {ital n} such as the planar Cu spin-lattice relaxation rate, the NQR frequency, and the magnetic shift are only weakly dependent on {ital x}. Thus, the substantial increase of {ital T}{sub {ital c}} with {ital x} suggests that, besides the increase of {ital n}, other effects have to play a role in the {ital T}{sub {ital c}} enhancement. One such effect might be the opening of the spin pseudogap. At 150 K, both the main and additional Cu NQR lines in nominal YBa{sub 1.9}Ca{sub 0.1}Cu{sub 4}O{sub 8} show distinctly anomalies not seen in pure YBa{sub 2}Cu{sub 4}O{sub 8} that point out the Ca doping induced structural phase transition recently observed in specific-heat, elastic-neutron-scattering, and x-ray-diffraction measurements. {copyright} {ital 1996 The American Physical Society.}

  11. Persistence of singlet fluctuations in the coupled spin tetrahedra system Cu2Te2O5Br2 revealed by high-field magnetization, 79Br NQR, and 125Te NMR

    NASA Astrophysics Data System (ADS)

    Baek, S.-H.; Choi, K.-Y.; Berger, H.; Büchner, B.; Grafe, H.-J.

    2012-11-01

    We present high-field magnetization and 79Br nuclear quadrupole resonance (NQR) and 125Te nuclear magnetic resonance (NMR) studies in the weakly coupled Cu2+ (S=1/2) tetrahedral system Cu2Te2O5Br2. The field-induced level crossing effects were observed by the magnetization measurements in a long-ranged magnetically ordered state which was confirmed by a strong divergence of the spin-lattice relaxation rate T1-1 at T0=13.5 K. In the paramagnetic state, T1-1 reveals an effective singlet-triplet spin gap much larger than that observed by static bulk measurements. Our results imply that the inter- and the intratetrahedral interactions compete, but at the same time they cooperate strengthening effectively the local intratetrahedral exchange couplings. We discuss that the unusual feature originates from the frustrated intertetrahedral interactions.

  12. (14)N NQR, (1)H NMR and DFT/QTAIM study of hydrogen bonding and polymorphism in selected solid 1,3,4-thiadiazole derivatives.

    PubMed

    Seliger, Janez; Zagar, Veselko; Latosińska, Jolanta N

    2010-10-28

    The 1,3,4-thiadiazole derivatives (2-amino-1,3,4-thiadiazole, acetazolamide, sulfamethizole) have been studied experimentally in the solid state by (1)H-(14)N NQDR spectroscopy and theoretically by Density Functional Theory (DFT). The specific pattern of the intra and intermolecular interactions in 1,3,4-thiadiazole derivatives is described within the QTAIM (Quantum Theory of Atoms in Molecules)/DFT formalism. The results obtained in this work suggest that considerable differences in the NQR parameters permit differentiation even between specific pure association polymorphic forms and indicate that the stronger hydrogen bonds are accompanied by the larger η and smaller ν(-) and e(2)Qq/h values. The degree of π-electron delocalization within the 1,3,4-thiadiazole ring and hydrogen bonds is a result of the interplay between the substituents and can be easily observed as a change in NQR parameters at N atoms. In the absence of X-ray data NQR parameters can clarify the details of crystallographic structure revealing information on intermolecular interactions.

  13. Optimised NQR pulse technique for the effective detection of Heroin Base.

    PubMed

    Rudakov, T N; Hayes, P A; Flexman, J H

    2008-03-01

    The nuclear quadrupole resonance (NQR) method has been applied to Heroin Base (HB) to find an optimised multi-pulse technique for effective detection of HB. Experimental results of applying the proposed spin-locking multi-pulse (SLMP) technique to nitrogen-14 NQR in this sample are presented and convincingly demonstrate as a path towards efficient detection. A detection using a sequence of this character could be achieved over real-world scan volumes for screening of goods. All experiments were carried out at room temperature.

  14. Two-dimensional NQR using ultra-broadband electronics

    NASA Astrophysics Data System (ADS)

    Mandal, S.; Song, Y.-Q.

    2014-03-01

    We have recently developed an ultra-broadband instrument that can effectively excite and detect NMR and NQR signals over a wide frequency range. Our current system operates between 100 kHz and 3.2 MHz using an un-tuned sample coil. The major benefits of this instrument compared to conventional NQR/NMR systems include increased robustness, ease of use (in particular for multi-frequency experiments), and elimination of the need for tuning adjustments in the hardware. Here we describe its use for performing two-dimensional (2D) scans, which allow improved interpretation of complex NQR spectra by detecting the connected resonances. Our method relies on population transfers between the three energy levels of spin-1 nuclei (such as 14N) by using multi-frequency excitation and a single RF coil. Experimental results on pure samples and mixtures are also presented.

  15. Two-dimensional NQR using ultra-broadband electronics.

    PubMed

    Mandal, S; Song, Y-Q

    2014-03-01

    We have recently developed an ultra-broadband instrument that can effectively excite and detect NMR and NQR signals over a wide frequency range. Our current system operates between 100 kHz and 3.2 MHz using an un-tuned sample coil. The major benefits of this instrument compared to conventional NQR/NMR systems include increased robustness, ease of use (in particular for multi-frequency experiments), and elimination of the need for tuning adjustments in the hardware. Here we describe its use for performing two-dimensional (2D) scans, which allow improved interpretation of complex NQR spectra by detecting the connected resonances. Our method relies on population transfers between the three energy levels of spin-1 nuclei (such as (14)N) by using multi-frequency excitation and a single RF coil. Experimental results on pure samples and mixtures are also presented. Copyright © 2014 Elsevier Inc. All rights reserved.

  16. Volovik effect and Fermi-liquid behavior in the s-wave superconductor CaPd2As2: As75 NMR-NQR measurements

    SciTech Connect

    Ding, Q. -P.; Wiecki, P.; Anand, V. K.; Sangeetha, N. S.; Lee, Y.; Johnston, D. C.; Furukawa, Y.

    2016-04-07

    The electronic and magnetic properties of the collapsed-tetragonal CaPd2As2 superconductor (SC) with a transition temperature of 1.27 K have been investigated by 75As nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements. The temperature (T) dependence of the nuclear spin lattice relaxation rates (1/T1) and the Knight shifts indicate the absence of magnetic correlations in the normal state. In the SC state, 1/T1 measured by 75As NQR shows a clear Hebel-Slichter (HS) peak just below Tc and decreases exponentially at lower T, confirming a conventional s-wave SC. Additionally, the Volovik effect, also known as the Doppler shift effect, has been clearly evidenced by the observation of the suppression of the HS peak with applied magnetic field.

  17. Single-spin fluid, spin gap, and [ital d]-wave pairing in YBa[sub 2]Cu[sub 4]O[sub 8]: A NMR and NQR study

    SciTech Connect

    Bankay, M.; Mali, M.; Roos, J.; Brinkmann, D. )

    1994-09-01

    We present results of [sup 17]O and [sup 63,65]Cu nuclear magnetic resonance (NMR) and nuclear quadrupolar resonance (NQR) studies in the normal and superconducting state of the 82-K superconductor YBa[sub 2]Cu[sub 4]O[sub 8]. The various components of the Cu and O Knight-shift tensors show strong but similar temperature dependences over the temperature range from 8.5 to 300 K in both the CuO[sub 2] planes and the chains, supporting the picture that there is only one spin component in the planes and the chains, although with different susceptibilities. The oxygen data obey the Korringa relation. This may be interpreted as Fermi-liquid behavior of the electronic system far away from the antiferromagnetic wave vector. The temperature dependence of both the planar Cu and O shift tensors and the planar Cu spin-lattice relaxation rate suggest the opening of a pseudo-spin-gap well above [ital T][sub [ital c

  18. Superconducting fluctuations and {sup 63}Cu NQR-NMR relaxation in YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}: Effect of magnetic field and a test for the pairing-state symmetry

    SciTech Connect

    Carretta, P.; Livanov, D.V.; Rigamonti, A.; Varlamov, A.A. |

    1996-10-01

    Evidence is presented of superconducting fluctuations in the {sup 63}Cu NQR-NMR relaxation rate in YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}, as obtained from a careful comparison of measurements carried out in the absence and in the presence of a field parallel to the {ital c} axis. It is shown that the field causes a reduction of the relaxation rate {ital W} in a range of about 10 K above {ital T}{sub {ital c}}. This effect is related to the suppression by the magnetic field of the phase-sensitive positive Maki-Thompson contribution while the negative contribution from the DOS fluctuations is almost field independent. Furthermore, it is argued how the fluctuation effects on {ital W} can be used to discuss the pairing state symmetry, at variance with the insensitivity of the transport measurements. It is pointed out that the existence of the Maki-Thompson contribution to {ital W} evidences an {ital s}-wave symmetry component for the pairing in YBa{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}. {copyright} {ital 1996 The American Physical Society.}

  19. An innovative method for the non-destructive identification of photodegradation products in solid state: 1H-14N NMR-NQR and DFT/QTAIM study of photodegradation of nifedipine (anti-hypertensive) to nitrosonifedipine (potential anti-oxidative).

    PubMed

    Latosińska, J N; Latosińska, M; Seliger, J; Zagar, V

    2012-08-30

    Stability of the antihypertensive drug nifedipine (NIF) has been studied experimentally in solid state by (1)H-(14)N NMR-NQR double resonance (NQDR) and theoretically by the Density Functional Theory (DFT). Photodegradation of NIF to its metabolite in vivo nitrosonifedipine, NO-NIF (antioxidative agent) upon long term daylight exposure was detected and the changes in the molecular structure of NIF were analysed. The photoconversion of NIF to NO-NIF in solid was found to be accompanied with the electron density redistribution at nitrogen sites (NH to N and NO(2) to NO) and proved to be successfully detected with identification of photoproducts by (1)H-(14)N NQDR and DFT methods. The increase in the e(2)qQ/h and η describing EFG tendency towards non-spherical symmetry was significantly greater upon the reduction of NO(2) site than upon hydrogen abstraction from NH site. The level of sensitivity of detection of the photodegradation product was about 1% of the original sample. The Quantum Theory of Atoms in Molecules (QTAIM) analysis has been found useful in predicting photoreactive sites in the molecules and finding the explanation of differences in reactivity between parent NIF and its photoproduct NO-NIF. Using NIF as a model, this study demonstrates the suitability of NQDR supported by DFT for non-destructive determination of the photodegradation products in solid state. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Superconducting Characteristics of Filled Skutterudites LaPt4Ge12 and PrPt4Ge12: 73Ge-NQR/NMR Studies

    NASA Astrophysics Data System (ADS)

    Fumiya Kanetake,; Hidekazu Mukuda,; Yoshio Kitaoka,; Ko-ichi Magishi,; Hitoshi Sugawara,; Kohei M. Itoh,; Eugene E. Haller,

    2010-06-01

    We report on the superconducting characteristics of the filled skutterudites LaPt4Ge12 (Tc=8.3 K) and PrPt4Ge12 (Tc=7.9 K) by 73Ge-nuclear quadrupole resonance (NQR) at a zero field. In PrPt4Ge12, the nuclear spin-lattice relaxation rate 73(1/T1) has revealed a coherence peak just below Tc, indicating that the superconductivity of PrPt4Ge12 is accounted for in terms of the conventional BCS regime. The result was consistently reproduced by not only an isotropic s-wave gap model but also an anisotropic s-wave gap model with a point node. In the conventional superconductor LaPt4Ge12, the coherence peak in 73(1/T1) is markedly suppressed owing to some damping effect of quasiparticles. We note that the Tcs of LaPt4Ge12 and PrPt4Ge12 being higher than that of other RPt4Ge12 may be attributed to the larger density of states, not to some local anharmonic phonon modes derived from the possible rattling of R ions.

  1. Uniform mixing of antiferromagnetism and high- Tc superconductivity in multilayer copper oxides Ba2Can-1CunO2nF2 (n=2,3,4) with apical fluorines: C63u-NMR/NQR and F19-NMR studies

    NASA Astrophysics Data System (ADS)

    Shimizu, S.; Sakaguchi, T.; Mukuda, H.; Kitaoka, Y.; Shirage, P. M.; Kodama, Y.; Iyo, A.

    2009-02-01

    We report C63u-NMR/NQR and F19-NMR studies on the multilayered high- Tc copper oxides Ba2Can-1CunO2nF2 with n=2,3,4 , where n is the number of CuO2 planes. It is revealed that bilayered Ba2CaCu2O4F2 is an underdoped superconductor with hole carriers, which are introduced into CuO2 planes by an unexpected deviation from the nominal content of apical fluorines. In a previous paper, we proposed a self-doping mechanism as the origin of carrier doping in n=3 and n=4 ; in the mechanism, electrons are transferred from the inner CuO2 plane (IP) to the outer one (OP). However, since it has been found that the bilayered compound is hole doped, we have re-examined the superconducting and magnetic properties in n=3 and n=4 by C63u-NMR/NQR and F19-NMR . The extensive NMR studies have confirmed that the apical-fluorine compounds are not self-doped but hole doped and that antiferromagnetism (AFM) and superconductivity (SC) coexist in a single CuO2 plane. In n=4 , the AFM ordering occurs at TN=80K well above Tc=55K , where the respective AFM moments are MAFM=0.11μB and 0.18μB at the OP and the IP. In n=3 , on the other hand, the underdoped single IP exhibits a spontaneous moment MAFM=0.12μB at low temperatures and a peak in the nuclear-spin-lattice relaxation rate 1/T1 of F19 at TN=23K much lower than Tc=76K . We note that the increase in the number of IPs from one to two results in the strengthening of the interlayer coupling; TN increases as the interlayer coupling becomes stronger, although the doping levels for both compounds are comparable. Consequently, we conclude that the uniform mixing of AFM and SC is a general property inherent to a single CuO2 plane in an underdoped regime for hole doping. This conclusion incorporates the angle-resolved photoemission spectroscopy results on the n=4 compound [Chen , Phys. Rev. Lett. 97, 236401 (2006)]; it was found that the two Fermi sheets of the IP and OP are observed and that the SC gap opens at the IP and OP below Tc=55K .

  2. Line-narrowing in proton-detected nitrogen-14 NMR

    NASA Astrophysics Data System (ADS)

    Cavadini, Simone; Vitzthum, Veronika; Ulzega, Simone; Abraham, Anuji; Bodenhausen, Geoffrey

    2010-01-01

    In solids spinning at the magic angle, the indirect detection of single-quantum (SQ) and double-quantum (DQ) 14N spectra ( I = 1) via spy nuclei S = 1/2 such as protons can be achieved in the manner of heteronuclear single- or multiple-quantum correlation (HSQC or HMQC) spectroscopy. The HMQC method relies on the excitation of two-spin coherences of the type T11IT11S and T21IT11S at the beginning of the evolution interval t1. The spectra obtained by Fourier transformation from t1 to ω1 may be broadened by the homogenous decay of the transverse terms of the spy nuclei S. This broadening is mostly due to homonuclear dipolar S- S' interactions between the proton spy nuclei. In this work we have investigated the possibility of inserting rotor-synchronized symmetry-based C or R sequences and decoupling schemes such as Phase-Modulated Lee-Goldburg (PMLG) sequences in the evolution period. These schemes reduce the homonuclear proton-proton interactions and lead to an enhancement of the resolution of both SQ and DQ proton-detected 14N HMQC spectra. In addition, we have investigated the combination of HSQC with symmetry-based sequences and PMLG and shown that the highest resolution in the 14N dimension is achieved by using HSQC in combination with symmetry-based sequences of the R-type. We show improvements in resolution in samples of L-alanine and the tripeptide ala-ala-gly (AAG). In particular, for L-alanine the width of the 14N SQ peak is reduced from 2 to 1.2 kHz, in agreement with simulations. We report accurate measurements of quadrupolar coupling constants and asymmetry parameters for amide 14N in AAG peptide bonds.

  3. Line-narrowing in proton-detected nitrogen-14 NMR.

    PubMed

    Cavadini, Simone; Vitzthum, Veronika; Ulzega, Simone; Abraham, Anuji; Bodenhausen, Geoffrey

    2010-01-01

    In solids spinning at the magic angle, the indirect detection of single-quantum (SQ) and double-quantum (DQ) (14)N spectra (I=1) via spy nuclei S=1/2 such as protons can be achieved in the manner of heteronuclear single- or multiple-quantum correlation (HSQC or HMQC) spectroscopy. The HMQC method relies on the excitation of two-spin coherences of the type T(11)(I)T(11)(S) and T(21)(I)T(11)(S) at the beginning of the evolution interval t(1). The spectra obtained by Fourier transformation from t(1) to omega(1) may be broadened by the homogenous decay of the transverse terms of the spy nuclei S. This broadening is mostly due to homonuclear dipolar S-S' interactions between the proton spy nuclei. In this work we have investigated the possibility of inserting rotor-synchronized symmetry-based C or R sequences and decoupling schemes such as Phase-Modulated Lee-Goldburg (PMLG) sequences in the evolution period. These schemes reduce the homonuclear proton-proton interactions and lead to an enhancement of the resolution of both SQ and DQ proton-detected (14)N HMQC spectra. In addition, we have investigated the combination of HSQC with symmetry-based sequences and PMLG and shown that the highest resolution in the (14)N dimension is achieved by using HSQC in combination with symmetry-based sequences of the R-type. We show improvements in resolution in samples of l-alanine and the tripeptide ala-ala-gly (AAG). In particular, for l-alanine the width of the (14)N SQ peak is reduced from 2 to 1.2 kHz, in agreement with simulations. We report accurate measurements of quadrupolar coupling constants and asymmetry parameters for amide (14)N in AAG peptide bonds.

  4. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, June 15--September 15, 1991

    SciTech Connect

    Not Available

    1991-12-17

    Our previous studies (1,2) on the zerofield NMR spectra of Cu/Co catalysts revealed that the method of preparation sensitively influences the magnetic character of the Catalyst. Catalytic studies of the earlier investigators also (3) show similar influence on the product selectivity and indicate reproducible performance is critically dependent on the control and rigor of the preparation technique. To compliment the NMR results, we have made a thorough investigation of the Hysteresis character of the Cu/Co catalysts with the metal ratio varying from 0.2 to 4.0.

  5. Using nitrogen-14 nuclear quadrupole resonance and electric field gradient information for the study of radiation effects

    SciTech Connect

    Iselin, L.H.

    1995-12-01

    Nitrogen-14 nuclear quadrupole resonance (NQR) was used in an attempt to detect the effects of ionizing radiation on organic material. Previously reported resonances for urea were detected at 2,913.32 {+-} 0.01 kHz and 2,347.88 {+-} 0.08 kHz with associated T{sub 2}* values 780 {+-} 20 {micro}s and 523 {+-} 24 {micro}s, respectively. The previously unreported {nu}{sub {minus}} line for urea-d{sup 4} was detected at 2,381 {+-} 0.04 Khz and used to determine accurately for the first time the values for the nuclear quadrupole coupling constant {chi} (3,548.74 {+-} 0.03 kHz) and the asymmetry parameter {eta} (0.31571 {+-} 0.00007) for urea-d{sup 4}. The inverse linewidth parameter T{sub 2}* for {nu}{sub +} was measured at 928 {+-} 23 {micro}s and for {nu}{sub {minus}} at 721 {+-} 12 {micro}s. Townes and Dailey analysis was performed and urea-d{sup 4} exhibits a 0.004 increase in lone pair electronic density and a slight decrease in N-H bond electronic density, as compared to urea, probably due to the mass difference. A relationship is proposed, referred to as NQR linewidth analysis, between the dynamic spin relaxation times T{sub 2} and T{sub 2}* and the widths of the distributions of the NQR parameters. Linewidth analysis is presented as a tool for possible use in future NQR work in all area, not just radiation effects. This relationship is tested using sodium nitrite T{sub 2} and T{sub 2}* values for {nu}{sub {minus}} and {nu}{sub {minus}} as a function of temperature.

  6. Novel superconducting characteristics and unusual normal-state properties in iron-based pnictide superconductors: 57FeNMR and 75AsNQR/NMR studies in REFeAsO 1- y (RE = La, Pr, Nd) and Ba 0.6K 0.4Fe 2As 2

    NASA Astrophysics Data System (ADS)

    Mukuda, H.; Terasaki, N.; Yashima, M.; Nishimura, H.; Kitaoka, Y.; Iyo, A.

    2009-05-01

    We discuss the novel superconducting characteristics and unusual normal-state properties of iron (Fe)-based pnictide superconductors REFeAsO 1- y (RE = La, Pr, Nd) and Ba 0.6K 0.4Fe 2As 2 ( Tc = 38 K) by means of 57FeNMR and 75AsNQR/NMR. In the superconducting state of LaFeAsO 0.7 ( Tc = 28 K), the spin component of the 57Fe-Knight shift decreases to almost zero at low temperatures, which provide firm evidence of the superconducting state formed by spin-singlet Cooper pairing. The nuclear spin-lattice relaxation rates (1/ T1) in LaFeAsO 0.7 and Ba 0.6K 0.4Fe 2As 2 exhibit a T3-like dependence without a coherence peak just below Tc, indicating that an unconventional superconducting state is commonly realized in these Fe-based pnictide compounds. All these events below Tc are consistently argued in terms of an extended s ±-wave pairing with a sign reversal of the order parameter among Fermi surfaces. In the normal state, 1/ T1T decreases remarkably upon cooling for both the Fe and As sites of LaFeAsO 0.7. In contrast, it gradually increases upon cooling in Ba 0.6K 0.4Fe 2As 2. Despite the similarity between the superconducting properties of these compounds, a crucial difference was observed in their normal-state properties depending on whether electrons or holes are doped into the FeAs layers. These results may provide some hint to address a possible mechanism of Fe-based pnictide superconductors.

  7. Scientific Support for NQR Explosive Detection Development

    DTIC Science & Technology

    2006-07-01

    Final 3. DATES COVERED (From - To) 8 March 2004 - 7 March 2006 4. TITLE AND SUBTITLE Scientific Support for NQR Explosive Detection Development...Laboratory (NRL) to improve explosive detection using nuclear quadrupole resonance ( NQR ) is summarized. The work includes studies of the effects...superconducting coils for explosive detection. Additional studies involving slowly rotating NQR measurements were also pursued. 15. SUBJECT TERMS Nuclear

  8. Increasing 14N NQR signal by 1H-14N level crossing with small magnetic fields.

    PubMed

    Thurber, Kent R; Sauer, Karen L; Buess, Michael L; Klug, Christopher A; Miller, Joel B

    2005-11-01

    NQR detection of materials, such as TNT, is hindered by the low signal-to-noise ratio at low NQR frequencies. Sweeping small (0-26 mT) magnetic fields to shift the (1)H NMR frequency relative to the (14)N NQR frequencies can provide a significant increase of the (14)N NQR signal-to-noise ratio. Three effects of (1)H-(14)N level crossing are demonstrated in diglycine hydrochloride and TNT. These effects are (1) transferring (1)H polarization to one or more of the (14)N transitions, including the use of an adiabatic flip of the (1)H polarization during the field sweep, (2) shortening the effective (14)N T(1) by the interaction of (1)H with the (14)N transitions, (3) "level transfer" effect where the third (14)N (spin 1) energy level or other (14)N sites with different NQR frequency are used as a reservoir of polarization which is transferred to the measured (14)N transition by the (1)H. The (14)N NQR signal-to-noise ratio can be increased by a factor of 2.5 for one (14)N site in diglycine hydrochloride (and 2.2 in TNT), even though the maximum (1)H frequency used in this work, 111 6 kHz, is only 30% larger than the measured (14)N frequencies (834 kHz for diglycine hydrochloride and 843 kHz for TNT).

  9. NQR spin-echo methods at very low temperatures

    SciTech Connect

    Goudemond, I.P.; Keartland, J.M.; Hoch, M.J.R. )

    1991-03-01

    Pulsed methods may be successfully used in very-low-temperature NMR or NQR experiments provided good thermal anchoring of the sample is achieved. In order to reduce heating effects, it is advantageous to use rf pulses that are shorter than the standard magnetization tipping pulses used at higher temperatures. The study describes the use of short nonstandard rf pulses in NQR spin-echo experiments on powdered samples. Theoretical density-matrix calculations were carried out, and the resulting expression for the echo amplitude confirmed by experiment. Measurements were made on a powder sample of high-purity semimetallic arsenic using a sample probe designed for use in a dilution refrigerator. Preliminary spin-lattice relaxation-time measurements show that the Korringa relation holds in arsenic down to 150 mK.

  10. Calculations of multipulse sequence in NQR of spins 32.

    PubMed

    Odin, C

    1999-12-01

    The general formalism of the interaction representation with respect to an operator which is its own inverse is developed and applied to pure NQR of spins I = 32. Under the assumption of no relaxation and no dipolar coupling, it is shown that the calculation of the response to pure NQR multipulse sequences can be performed with the same concepts used in high field NMR, such as coherence pathways. All the tools and mathematical expressions to predict the time evolution of the signal created by a pure NQR multipulse sequence are presented explicitly. It takes into account the off-resonance irradiation as well as the angular dependence of the excitation and detection for every value of the electric field gradient asymmetry parameter. Particular attention is devoted to the powder average, which is performed via a probability function derived analytically for the first time, leading to a drastic reduction of simulation times. The theory is illustrated by the study of the optimization and excitation bandwidths of one- to three-pulse sequences and compared to experimental results on Chloranil. We show that the three-pulse "stimulated echo" sequence gives a more uniform excitation profile than the traditional two-pulse echo sequence for powder samples. Thus, the "stimulated echo" sequence could be useful to cover a large spectrum when the experiment duration, or the signal to noise ratio, are not critical parameters. Analytical expressions for the nutation spectra obtained by one or two-pulse sequences are also derived for the first time.

  11. Explosives detection by nuclear quadrupole resonance (NQR)

    NASA Astrophysics Data System (ADS)

    Garroway, Allen N.; Buess, Michael L.; Yesinowski, James P.; Miller, Joel B.; Krauss, Ronald A.

    1994-10-01

    Pure nuclear quadrupole resonance (NQR) of 14N nuclei is quite promising as a method for detecting explosives such as RDX and contraband narcotics such as cocaine and heroin in quantities of interest. Pure NQR is conducted without an external applied magnetic field, so potential concerns about damage to magnetically encoded data or exposure of personnel to large magnetic fields are not relevant. Because NQR frequencies of different compounds are quite distinct, we do not encounter false alarms from the NQR signals of other benign materials. We have constructed a laboratory prototype NQR explosives detector which interrogates a volume of 300 liters (10 ft3). This paper presents abbreviated results from a demonstration of the laboratory prototype NQR explosives detector conducted at the Federal Aviation Administration Technical Center in May 1994 on RDX-based explosives.

  12. NMR-NQR study of the crossover from the spin-glass to the superconducting phase in La{sub 2{minus}x}Sr{sub x}CuO{sub 4}

    SciTech Connect

    Julien, M.H.; Carretta, P.; Borsa, F.; Rigamonti, A.

    1999-04-20

    {sup 139}La and {sup 63}Cu NQR relaxation rates are used to obtain insights on the effects of itinerant holes on the magnetic in-plane correlation length, for x {le} 0.04 in La{sub 2{minus}x}Sr{sub x}CuO{sub 4}. For these concentrations, corresponding to spin-glass behavior at low temperature, evidence for the microsegregation of holes along stripes is presented. Preliminary relaxation results for an amount of Sr doping leading to superconductivity are also presented and discussed in terms of the crossover from the spin-glass to the underdoped superconducting regime: for x = 0.06 a slowing down of spin fluctuations is evidenced and superconductivity is found to coexist with spin-freezing.

  13. 63Cu-NMR/NQR studies on apical-F bi-layered cuprates Ba2CaCu2O4F2 and Ba2CaCu2O4(F1.6O0.4)

    NASA Astrophysics Data System (ADS)

    Shimizu, S.; Sakaguchi, T.; Mukuda, H.; Kitaoka, Y.; Iyo, A.; Shirage, P. M.; Kito, H.; Kodama, Y.

    2009-10-01

    We report 63Cu-NMR/NQR on the bi-layered high- Tc copper oxide Ba2CaCu2O4F2, which is expected to be a Mott insulator in an ideal case of a nominal content of fluorine, and less fluorinated Ba2CaCu2O4(F1.6O0.4) to clear the doping mechanism in apical-fluorine multilayered system Ba2CaCunO2nF2, where n is the number of the layers in a unit cell. In the case of n=3 and, especially, n=4, the origin of carrier doping has been attributed to a self-doping mechanism based on the nominal stoichiometry; electrons are transferred between the inner CuO2 plane (IP) and the outer one (OP), keeping Cu+2 on average. It is revealed that Ba2CaCu2O4F2 is an underdoped superconductor with hole carriers, doped by an inevitable deviation from the nominal content of apical fluorines. This result suggests that hole carriers are doped in the same manner for the case of n=3 and 4, and that we should reconsider the self-doping mechanism as the carrier source in the apical-fluorine system.

  14. Analysis of 27Al- and 93Nb-NMR spectra of PrNb2Al20 single crystal

    NASA Astrophysics Data System (ADS)

    Kubo, Tetsuro; Kotegawa, Hisashi; Tou, Hideki; Higashinaka, Ryuji; Nakama, Akihiro; Aoki, Yuji; Sato, Hideyuki

    2016-02-01

    We report the results of 27Al- and 93Nb- nuclear magnetic resonance (NMR) and nuclear quadrupole resonance (NQR) measurements in PrNb2Al20 single crystals. The field angle dependence of the observed 93Nb-NMR lines for the single crystal at around 5 T and at 50 K is reproduced by a simulation using previously reported NQR parameters νQ,Nb ≈ 1.82 MHz and ηNb ≈ 0, while 27Al-NMR lines were not reproduce by the previously reported NQR parameters νQ,Al(3) ≈ 1.53 MHz and ηAl(3) ≈ 0.17. By reexamining and reconsidering the NMR and NQR lines for powder samples, we obtained a correct NQR parameters for Al(3) site to be νQ,Al(3),new ≈ 1 MHz and ηAl(3),new ≈ 0.4.

  15. FPGA based pulsed NQR spectrometer

    NASA Astrophysics Data System (ADS)

    Hemnani, Preeti; Rajarajan, A. K.; Joshi, Gopal; Motiwala, Paresh D.; Ravindranath, S. V. G.

    2014-04-01

    An NQR spectrometer for the frequency range of 1 MHz to 5 MHZ has been designed constructed and tested using an FPGA module. Consisting of four modules viz. Transmitter, Probe, Receiver and computer controlled (FPGA & Software) module containing frequency synthesizer, pulse programmer, mixer, detection and display, the instrument is capable of exciting nuclei with a power of 200W and can detect signal of a few microvolts in strength. 14N signal from NaNO2 has been observed with the expected signal strength.

  16. Optical detection of low frequency NQR signals: a step forward from conventional NQR

    NASA Astrophysics Data System (ADS)

    Begus, S.; Pirnat, J.; Jazbinsek, V.; Trontelj, Z.

    2017-03-01

    In searching for the more sensitive 14N nuclear quadrupole resonance (NQR) detecting system for illicit substances, a promising combination of a classic RF pulse NQR spectrometer and a K optically pumped magnetometer was tested. The initial results are encouraging. The principles of such a combination are described, and the detection limits in the low frequency RF region, where the 14N pulse NQR frequencies are usually positioned, are presented. Several illicit substances which are difficult to detect with a classic pulse NQR spectrometer were detected with both types of spectrometers. We noticed that with the proposed combination of classic RF excitation of 14N nuclei, using a pulse NQR spectrometer and subsequent optical detection of the sample’s response, a gain in S/N of up to a factor of 10 was possible.

  17. NMR/NQR study on magnetism of spin ladder Sr{sub 14{minus}x}A{sub x}Cu{sub 24}O{sub 41} (A = Ca and La)

    SciTech Connect

    Tsuji, Sigenori; Maki, Katsuhiko; Kumagai, Kenichi

    1999-12-01

    Hole-doping effects are investigated by Cu-NMR for single crystal of Sr{sub 14{minus}x}Ca{sub x}Cu{sub 24}O{sub 41}. The charge order of Cu{sup 2+} and Cu{sup 3+} and spin dimer ground state in the chain of Sr{sub 14}Cu{sub 24}O{sub 41} are proved by NMR study. The magnetic order of Cu spins in the chain and also the field-induced staggered moments at the ladder Cu site are confirmed for 3 {le} x {le} 6 of Sr{sub 14{minus}x}La{sub x}Cu{sub 24}O{sub 41}.

  18. NQR application to the study of hydrogen dynamics in hydrogen-bonded molecular dimers

    NASA Astrophysics Data System (ADS)

    Asaji, Tetsuo

    2016-12-01

    The temperature dependences of 1H NMR as well as 35Cl NQR spin-lattice relaxation times T 1 were investigated in order to study the hydrogen transfer dynamics in carboxylic acid dimers in 3,5-dichloro- and 2,6-dichlorobenzoic acids. The asymmetry energy A/ k B and the activation energy V/ k B for the hydrogen transfer were estimated to be 240 K and 900 K, and 840 K and 2500 K, respectively, for these compounds. In spite of a large asymmetric potential the quantum nature of hydrogen transfer is recognized in the slope of the temperature dependence of T 1 on the low-temperature side of the T 1 minimum. The NQR T 1 measurements was revealed to be a good probe for the hydrogen transfer dynamics.

  19. Fragmentation of nitrogen-14 nuclei at 2.1 Gev per nucleon.

    NASA Technical Reports Server (NTRS)

    Heckman, H. H.; Greiner, D. E.; Lindstrom, P. J.; Bieser, F. S.

    1971-01-01

    An experiment has been carried out at the bevatron on the nuclear fragmentation of nitrogen-14 ions at an energy of 2.1 billion electron volts (Gev) per nucleon. Because of the near equality of the velocities of the nitrogen-14 beam and the fragmentation products at an angle of 0 deg, we find it possible to identify the nuclear fragments isotopically.

  20. NQR investigation and characterization of cocrystals and crystal polymorphs

    NASA Astrophysics Data System (ADS)

    Seliger, Janez; Žagar, Veselko; Asaji, Tetsuo

    2013-05-01

    The application of 14N NQR to the study of cocrystals and crystal polymorphs is reviewed. In ferroelectric and antiferroelectric organic cocrystals 14N NQR is used to determine proton position in an N-H...O hydrogen bond and proton displacement below TC. In cocrystal isonicitinamide - oxalic acid (2:1) 14N NQR is used to distinguish between two polymorphs and to determine the type of the hydrogen bond (N-...H-O). The difference in the 14N NQR spectra of cocrystal formers and cocrystal is investigated in case of carbamazepine, saccharin and carbamazepine - saccharin (1:1). The experimental resolution allows an unambiguous distinction between the 14N NQR spectrum of the cocrystal and the 14N NQR spectra of the cocrystal formers. The possibility of application of NQR and double resonance for the determination of the inhomogeneity of the sample and for the study of the life time of an unstable polymorph is discussed.

  1. A miniaturized NQR spectrometer for a multi-channel NQR-based detection device.

    PubMed

    Beguš, Samo; Jazbinšek, Vojko; Pirnat, Janez; Trontelj, Zvonko

    2014-10-01

    A low frequency (0.5-5 MHz) battery operated sensitive pulsed NQR spectrometer with a transmitter power up to 5 W and a total mass of about 3 kg aimed at detecting (14)N NQR signals, predominantly of illicit materials, was designed and assembled. This spectrometer uses a standard software defined radio (SDR) platform for the data acquisition unit. Signal processing is done with the LabView Virtual instrument on a personal computer. We successfully tested the spectrometer by measuring (14)N NQR signals from aminotetrazole monohydrate (ATMH), potassium nitrate (PN), paracetamol (PCM) and trinitrotoluene (TNT). Such a spectrometer is a feasible component of a portable single or multichannel (14)N NQR based detection device.

  2. A miniaturized NQR spectrometer for a multi-channel NQR-based detection device

    NASA Astrophysics Data System (ADS)

    Beguš, Samo; Jazbinšek, Vojko; Pirnat, Janez; Trontelj, Zvonko

    2014-10-01

    A low frequency (0.5-5 MHz) battery operated sensitive pulsed NQR spectrometer with a transmitter power up to 5 W and a total mass of about 3 kg aimed at detecting 14N NQR signals, predominantly of illicit materials, was designed and assembled. This spectrometer uses a standard software defined radio (SDR) platform for the data acquisition unit. Signal processing is done with the LabView Virtual instrument on a personal computer. We successfully tested the spectrometer by measuring 14N NQR signals from aminotetrazole monohydrate (ATMH), potassium nitrate (PN), paracetamol (PCM) and trinitrotoluene (TNT). Such a spectrometer is a feasible component of a portable single or multichannel 14N NQR based detection device.

  3. 14 N NQR spectrum of sildenafil citrate

    NASA Astrophysics Data System (ADS)

    Stephenson, David; Singh, Nadia

    2015-04-01

    The 14N nuclear quadrupole resonance (NQR) spectrum of sildenafil citrate tablets has been recorded allowing the quadrupole coupling constants and asymmetry parameters of all six unique nitrogen atoms in its structure to be determined. A density function calculation gives results that are largely in agreement with the experimental values.

  4. The Na+-translocating NADH:quinone oxidoreductase (Na+-NQR) from Vibrio cholerae enhances insertion of FeS in overproduced NqrF subunit.

    PubMed

    Tao, Minli; Fritz, Günter; Steuber, Julia

    2008-01-01

    The Na+-translocating NADH:quinone oxidoreductase (Na+-NQR) from Vibrio cholerae is a membrane-bound, respiratory Na+ pump. Its NqrF subunit contains one FAD and a [2Fe-2S] cluster and catalyzes the initial oxidation of NADH. A soluble variant of NqrF lacking its hydrophobic, N-terminal helix (NqrF') was produced in V. cholerae wild type and nqr deletion strain. Under identical conditions of growth and induction, the yield of NqrF' increased by 30% in the presence of the Na+-NQR. FAD-containing NqrF' species with or without the FeS cluster were observed, indicating that assembly of the FeS center, but not insertion of the flavin cofactor, was limited during overproduction in V. cholerae. A comparison of these distinct NqrF' species with regard to specific NADH dehydrogenase activity, pH dependence of activity and thermal inactivation showed that NqrF' lacking the [2Fe-2S] cluster was less stable, partially unfolded, and therefore prone to proteolytic degradation in V. cholerae. We conclude that the overall yield of NqrF' critically depends on the amount of fully assembled, FeS-containing NqrF' in the V. cholerae host cells. The Na+-NQR is proposed to increase the stability of NqrF' by stimulating the maturation of FeS centers.

  5. NQR detection of explosive simulants using RF atomic magnetometers

    NASA Astrophysics Data System (ADS)

    Monti, Mark C.; Alexson, Dimitri A.; Okamitsu, Jeffrey K.

    2016-05-01

    Nuclear Quadrupole Resonance (NQR) is a highly selective spectroscopic method that can be used to detect and identify a number of chemicals of interest to the defense, national security, and law enforcement community. In the past, there have been several documented attempts to utilize NQR to detect nitrogen bearing explosives using induction sensors to detect the NQR RF signatures. We present here our work on the NQR detection of explosive simulants using optically pumped RF atomic magnetometers. RF atomic magnetometers can provide an order of magnitude (or more) improvement in sensitivity versus induction sensors and can enable mitigation of RF interference, which has classically has been a problem for conventional NQR using induction sensors. We present the theory of operation of optically pumped RF atomic magnetometers along with the result of laboratory work on the detection of explosive simulant material. An outline of ongoing work will also be presented along with a path for a fieldable detection system.

  6. Broadband quantitative NQR for authentication of vitamins and dietary supplements.

    PubMed

    Chen, Cheng; Zhang, Fengchao; Bhunia, Swarup; Mandal, Soumyajit

    2017-05-01

    We describe hardware, pulse sequences, and algorithms for nuclear quadrupole resonance (NQR) spectroscopy of medicines and dietary supplements. Medicine and food safety is a pressing problem that has drawn more and more attention. NQR is an ideal technique for authenticating these substances because it is a non-invasive method for chemical identification. We have recently developed a broadband NQR front-end that can excite and detect (14)N NQR signals over a wide frequency range; its operating frequency can be rapidly set by software, while sensitivity is comparable to conventional narrowband front-ends over the entire range. This front-end improves the accuracy of authentication by enabling multiple-frequency experiments. We have also developed calibration and signal processing techniques to convert measured NQR signal amplitudes into nuclear spin densities, thus enabling its use as a quantitative technique. Experimental results from several samples are used to illustrate the proposed methods. Copyright © 2017 Elsevier Inc. All rights reserved.

  7. Broadband quantitative NQR for authentication of vitamins and dietary supplements

    NASA Astrophysics Data System (ADS)

    Chen, Cheng; Zhang, Fengchao; Bhunia, Swarup; Mandal, Soumyajit

    2017-05-01

    We describe hardware, pulse sequences, and algorithms for nuclear quadrupole resonance (NQR) spectroscopy of medicines and dietary supplements. Medicine and food safety is a pressing problem that has drawn more and more attention. NQR is an ideal technique for authenticating these substances because it is a non-invasive method for chemical identification. We have recently developed a broadband NQR front-end that can excite and detect 14N NQR signals over a wide frequency range; its operating frequency can be rapidly set by software, while sensitivity is comparable to conventional narrowband front-ends over the entire range. This front-end improves the accuracy of authentication by enabling multiple-frequency experiments. We have also developed calibration and signal processing techniques to convert measured NQR signal amplitudes into nuclear spin densities, thus enabling its use as a quantitative technique. Experimental results from several samples are used to illustrate the proposed methods.

  8. Crystallization and preliminary analysis of the NqrA and NqrC subunits of the Na+-translocating NADH:ubiquinone oxidoreductase from Vibrio cholerae

    PubMed Central

    Vohl, Georg; Nedielkov, Ruslan; Claussen, Björn; Casutt, Marco S.; Vorburger, Thomas; Diederichs, Kay; Möller, Heiko M.; Steuber, Julia; Fritz, Günter

    2014-01-01

    The Na+-translocating NADH:ubiquinone oxidoreductase (Na+-NQR) from Vibrio cholerae is a membrane protein complex consisting of six different subunits NqrA–NqrF. The major domains of the NqrA and NqrC subunits were heterologously expressed in Escherichia coli and crystallized. The structure of NqrA1–377 was solved in space groups C2221 and P21 by SAD phasing and molecular replacement at 1.9 and 2.1 Å resolution, respectively. NqrC devoid of the transmembrane helix was co-expressed with ApbE to insert the flavin mononucleotide group covalently attached to Thr225. The structure was determined by molecular replacement using apo-NqrC of Parabacteroides distasonis as search model at 1.8 Å resolution. PMID:25005105

  9. NQR in Alanine and Lysine Iodates

    NASA Astrophysics Data System (ADS)

    Petrosyan, A. M.; Burbelo, V. M.; Tamazyan, R. A.; Karapetyan, H. A.; Sukiasyan, R. P.

    2000-02-01

    The structure o f iodates of α- and β-alanine ( Ala) (2(β-Ala • HIO3) • H2O , β-Ala-2HIO3 , D L-Ala• HIO3 • 2H2O, L-Ala • HIO3) and L-lysine (L-Lys) (L-Lys • HIO3, L-Lys • 2HIO3,L-Lys • 3HIO3, L-Lys • 6HIO3) have been investigated by means of iodine-127 NQR, IR spectroscopy and X-ray diffraction

  10. 14N NQR study of nicotinamide and related compounds.

    PubMed

    Seliger, J; Zagar, V

    2008-01-01

    14N nuclear quadrupole resonance (NQR) frequencies have been measured in picolinamide, nicotinamide, isonicotinamide, 2,6-pyridine dicarboxamide, and acetamide by double resonance. The 14N NQR spectra in picolinamide, nicotinamide, isonicotinamide, and 2,6-pyridine dicarboxamide show the presence of two distinct nitrogen positions: the ring position with the quadrupole coupling constant about 4,5 MHz and the amide position with the quadrupole coupling constant about 2.6 MHz. The NQR data are related to the structure of the investigated compounds and to the N--H...O hydrogen bonds. Copyright (c) 2007 John Wiley & Sons, Ltd.

  11. An electronically tuned wideband probehead for NQR spectroscopy in the VHF range

    NASA Astrophysics Data System (ADS)

    Scharfetter, Hermann

    2016-10-01

    Nuclear quadrupole resonance spectroscopy is an analytical method which allows to characterize materials which contain quadrupolar nuclei, i.e. nuclei with spin ⩾1. The measurement technology is similar to that of NMR except that no static magnetic field is necessary. In contrast to NMR, however, it is frequently necessary to scan spectra with a very large bandwidth with a span of several tens of % of the central frequency so as to localize unknown peaks. Standard NMR probeheads which are typically constructed as resonators must be tuned and matched to comparatively narrow bands and must thus be re-tuned and re-matched very frequently when scanning over a whole NQR spectrum. At low frequencies up to few MHz dedicated circuits without the need for tuning and matching have been developed, but many quadrupole nuclei have transitions in the VHF range between several tens of MHz up to several hundreds of MHz. Currently available commercial NQR probeheads employ stepper motors for setting mechanically tuneable capacitors in standard NMR resonators. These yield high quality factors (Q) and thus high SNR but are relatively large and clumsy and do not allow for fast frequency sweeps. This article presents a new concept for a NQR probehead which combines a previously published no-tune no-match wideband concept for the transmit (TX) pulse with an electronically tuneable receive (RX) part employing varactor diodes. The prototype coil provides a TX frequency range of 57 MHz with a center frequency of 97.5 MHz with a return loss of ⩽-15 dB. During RX the resonator is tuned and matched automatically to the right frequency via control voltages which are read out from a previously generated lookup table, thus providing high SNR. The control voltages which bias the varactors settle very fast and allow for hopping to the next frequency point in the spectrum within less than 100 μs. Experiments with a test sample of ZnBr2 proved the feasibility of the method.

  12. An electronically tuned wideband probehead for NQR spectroscopy in the VHF range.

    PubMed

    Scharfetter, Hermann

    2016-10-01

    Nuclear quadrupole resonance spectroscopy is an analytical method which allows to characterize materials which contain quadrupolar nuclei, i.e. nuclei with spin ⩾1. The measurement technology is similar to that of NMR except that no static magnetic field is necessary. In contrast to NMR, however, it is frequently necessary to scan spectra with a very large bandwidth with a span of several tens of % of the central frequency so as to localize unknown peaks. Standard NMR probeheads which are typically constructed as resonators must be tuned and matched to comparatively narrow bands and must thus be re-tuned and re-matched very frequently when scanning over a whole NQR spectrum. At low frequencies up to few MHz dedicated circuits without the need for tuning and matching have been developed, but many quadrupole nuclei have transitions in the VHF range between several tens of MHz up to several hundreds of MHz. Currently available commercial NQR probeheads employ stepper motors for setting mechanically tuneable capacitors in standard NMR resonators. These yield high quality factors (Q) and thus high SNR but are relatively large and clumsy and do not allow for fast frequency sweeps. This article presents a new concept for a NQR probehead which combines a previously published no-tune no-match wideband concept for the transmit (TX) pulse with an electronically tuneable receive (RX) part employing varactor diodes. The prototype coil provides a TX frequency range of 57MHz with a center frequency of 97.5MHz with a return loss of ⩽-15dB. During RX the resonator is tuned and matched automatically to the right frequency via control voltages which are read out from a previously generated lookup table, thus providing high SNR. The control voltages which bias the varactors settle very fast and allow for hopping to the next frequency point in the spectrum within less than 100μs. Experiments with a test sample of ZnBr2 proved the feasibility of the method. Copyright © 2016

  13. NMR Reveals Double Occupancy of Quinone-type Ligands in the Catalytic Quinone Binding Site of the Na+-translocating NADH:Quinone Oxidoreductase from Vibrio cholerae*

    PubMed Central

    Nedielkov, Ruslan; Steffen, Wojtek; Steuber, Julia; Möller, Heiko M.

    2013-01-01

    The sodium ion-translocating NADH:quinone oxidoreductase (Na+-NQR) from the pathogen Vibrio cholerae exploits the free energy liberated during oxidation of NADH with ubiquinone to pump sodium ions across the cytoplasmic membrane. The Na+-NQR consists of four membrane-bound subunits NqrBCDE and the peripheral NqrF and NqrA subunits. NqrA binds ubiquinone-8 as well as quinones with shorter prenyl chains (ubiquinone-1 and ubiquinone-2). Here we show that the quinone derivative 2,5-dibromo-3-methyl-6-isopropyl-p-benzoquinone (DBMIB), a known inhibitor of the bc1 and b6f complexes found in mitochondria and chloroplasts, also inhibits quinone reduction by the Na+-NQR in a mixed inhibition mode. Tryptophan fluorescence quenching and saturation transfer difference NMR experiments in the presence of Na+-NQR inhibitor (DBMIB or 2-n-heptyl-4-hydroxyquinoline N-oxide) indicate that two quinone analog ligands are bound simultaneously by the NqrA subunit with very similar interaction constants as observed with the holoenzyme complex. We conclude that the catalytic site of quinone reduction is located on NqrA. The two ligands bind to an extended binding pocket in direct vicinity to each other as demonstrated by interligand Overhauser effects between ubiquinone-1 and DBMIB or 2-n-heptyl-4-hydroxyquinoline N-oxide, respectively. We propose that a similar spatially close arrangement of the native quinone substrates is also operational in vivo, enhancing the catalytic efficiency during the final electron transfer steps in the Na+-NQR. PMID:24003222

  14. NQR Studies of Halogen Treated 1-2-3 System

    NASA Astrophysics Data System (ADS)

    Ossipyan, Ya. A.; Sidorov, N. S.; Kulakov, V. I.; Matukhin, V. L.; Pogoreltsev, A. I.; Anashkin, V. N.; Safin, I. A.; Matukhin, L. E.

    1998-07-01

    NQR spectra of copper in polycrystalline samples of iodine treated RBa2Cu3Oy (R = Y, Gd) were studied. The results of all the experiments show evidence for the modifications occurring in the oxygen sublattice in treated compounds.

  15. PEANUT experiment in NQR spectroscopy for I=3/2.

    PubMed

    Sinyavsky, Nikolay; Dolinenkov, Philip; Maćkowiak, Mariusz

    2012-01-01

    The experiment with phase inversion and phase-inverted echo-amplitude detected nutation (PEANUT) was introduced in the nuclear quadrupole resonance (NQR). Formulas were obtained describing the NQR (I=3/2) experiment. Exemplary experiments are provided confirming the predicted particularities of the PEANUT spectra in NQR Cl-35. It is proposed to apply the method for the purpose of determination the asymmetry parameter of the electric field gradient (EFG) tensor in powders with the help of the analysis of PEANUT interferograms. Application of two-dimensional PEANUT experiments, in which the nutation frequencies correlate with the resonance NQR frequencies, can substantially simplify the interpretation of complex spectra. Copyright © 2012 Elsevier Inc. All rights reserved.

  16. NQR Characteristics of an RDX Plastic Explosives Simulant.

    PubMed

    Turecek, J; Schwitter, B; Miljak, D; Stancl, M

    2012-12-01

    For reliable detection of explosives, a combination of methods integrated within a single measurement platform may increase detection performance. However, the efficient field testing of such measurement platforms requires the use of inexplosive simulants that are detectable by a wide range of methods. Physical parameters such as simulant density, elemental composition and crystalline structure must closely match those of the target explosive. The highly discriminating bulk detection characteristics of nuclear quadrupole resonance (NQR) especially constrain simulant design. This paper describes the development of an inexplosive RDX simulant suited to a wide range of measurement methods, including NQR. Measurements are presented that confirm an RDX NQR response from the simulant. The potential use of the simulant for field testing a prototype handheld NQR-based RDX detector is analyzed. Only modest changes in prototype operation during field testing would be required to account for the use of simulant rather than real explosive.

  17. Measurement of in-situ stress in salt and rock using NQR techniques

    SciTech Connect

    Schempp, E.; Hirschfeld, T.; Klainer, S.

    1980-12-01

    A discussion of how stress and strain affect the quantities which can be measured in an NQR experiment shows that, for stresses of the magnitude to be expected at depths up to about 10,000 feet, quadrupole coupling constants will fall in the range of 1 to 10 kHz for both the sodium and chloride ions in NaCl. The most promising system involves pulsed nuclear double resonance detection; and alterative is to observe the quadrupolar splitting of the NMR signal. Choices to be made in the measurement and mapping techniques are discussed. The well-known perturbation of the homogenous stress field in the neighborhood of a borehole is shown to be advantageous from the point of view of obtaining directional information on the stress. Construction and operation of a borehole stress sensor are considered. The NQR technique seems feasible for measuring the magnitude and direction of underground stress with a resolution of about 25 psi, or 2.5% at 1000 psi. Downhole instrumentation suitable for in-situ determinations of stress appears within the state of the art. Additional tasks required on the project are identified.

  18. Frequency selective detection of nuclear quadrupole resonance (NQR) spin echoes

    NASA Astrophysics Data System (ADS)

    Somasundaram, Samuel D.; Jakobsson, Andreas; Smith, John A. S.; Althoefer, Kaspar A.

    2006-05-01

    Nuclear Quadrupole Resonance (NQR) is a radio frequency (RF) technique that can be used to detect the presence of quadrupolar nuclei, such as the 14N nucleus prevalent in many explosives and narcotics. The technique has been hampered by low signal-to-noise ratios and is further aggravated by the presence of RF interference (RFI). To ensure accurate detection, proposed detectors should exploit the rich form of the NQR signal. Furthermore, the detectors should also be robust to any remaining residual interference, left after suitable RFI mitigation has been employed. In this paper, we propose a new NQR data model, particularly for the realistic case where multiple pulse sequences are used to generate trains of spin echoes. Furthermore, we refine two recently proposed approximative maximum likelihood (AML) detectors, enabling the algorithm to optimally exploit the data model of the entire echo train and also incorporate knowledge of the temperature dependent spin-echo decay time. The AML-based detectors ensure accurate detection and robustness against residual RFI, even when the temperature of the sample is not precisely known, by exploiting the dependencies of the NQR resonant lines on temperature. Further robustness against residual interference is gained as the proposed detector is frequency selective; exploiting only those regions of the spectrum where the NQR signal is expected. Extensive numerical evaluations based on both simulated and measured NQR data indicate that the proposed Frequency selective Echo Train AML (FETAML) detector offers a significant improvement as compared to other existing detectors.

  19. Asymmetric Induction by a Nitrogen 14N/15N Isotopomer in Conjunction with Asymmetric Autocatalysis

    PubMed Central

    Ozaki, Hanae; Harada, Shunya; Tada, Kyohei; Ayugase, Tomohiro; Ozawa, Hitomi; Kawasaki, Tsuneomi

    2016-01-01

    Abstract Chirality arising from isotope substitution, especially with atoms heavier than the hydrogen isotopes, is usually not considered a source of chirality in a chemical reaction. An N 2 ,N 2 ,N 3 ,N 3‐tetramethyl‐2,3‐butanediamine containing nitrogen (14N/15N) isotope chirality was synthesized and it was revealed that this isotopically chiral diamine compound acts as a chiral initiator for asymmetric autocatalysis. PMID:27754589

  20. Asymmetric Induction by a Nitrogen (14) N/(15) N Isotopomer in Conjunction with Asymmetric Autocatalysis.

    PubMed

    Matsumoto, Arimasa; Ozaki, Hanae; Harada, Shunya; Tada, Kyohei; Ayugase, Tomohiro; Ozawa, Hitomi; Kawasaki, Tsuneomi; Soai, Kenso

    2016-12-05

    Chirality arising from isotope substitution, especially with atoms heavier than the hydrogen isotopes, is usually not considered a source of chirality in a chemical reaction. An N(2) ,N(2) ,N(3) ,N(3) -tetramethyl-2,3-butanediamine containing nitrogen ((14) N/(15) N) isotope chirality was synthesized and it was revealed that this isotopically chiral diamine compound acts as a chiral initiator for asymmetric autocatalysis.

  1. New perspectives in the PAW/GIPAW approach: J(P-O-Si) coupling constants, antisymmetric parts of shift tensors and NQR predictions.

    PubMed

    Bonhomme, Christian; Gervais, Christel; Coelho, Cristina; Pourpoint, Frédérique; Azaïs, Thierry; Bonhomme-Coury, Laure; Babonneau, Florence; Jacob, Guy; Ferrari, Maude; Canet, Daniel; Yates, Jonathan R; Pickard, Chris J; Joyce, Siân A; Mauri, Francesco; Massiot, Dominique

    2010-12-01

    In 2001, Pickard and Mauri implemented the gauge including projected augmented wave (GIPAW) protocol for first-principles calculations of NMR parameters using periodic boundary conditions (chemical shift anisotropy and electric field gradient tensors). In this paper, three potentially interesting perspectives in connection with PAW/GIPAW in solid-state NMR and pure nuclear quadrupole resonance (NQR) are presented: (i) the calculation of J coupling tensors in inorganic solids; (ii) the calculation of the antisymmetric part of chemical shift tensors and (iii) the prediction of (14)N and (35)Cl pure NQR resonances including dynamics. We believe that these topics should open new insights in the combination of GIPAW, NMR/NQR crystallography, temperature effects and dynamics. Points (i), (ii) and (iii) will be illustrated by selected examples: (i) chemical shift tensors and heteronuclear (2)J(P-O-Si) coupling constants in the case of silicophosphates and calcium phosphates [Si(5)O(PO(4))(6), SiP(2)O(7) polymorphs and α-Ca(PO(3))(2)]; (ii) antisymmetric chemical shift tensors in cyclopropene derivatives, C(3)X(4) (X = H, Cl, F) and (iii) (14)N and (35)Cl NQR predictions in the case of RDX (C(3)H(6)N(6)O(6)), β-HMX (C(4)H(8)N(8)O(8)), α-NTO (C(2)H(2)N(4)O(3)) and AlOPCl(6). RDX, β-HMX and α-NTO are explosive compounds. Copyright © 2010 John Wiley & Sons, Ltd.

  2. On the Nature of the "Bleaching out" Process of the 35Cl NQR Signals in 1,2,3-Trichlorobenzene

    NASA Astrophysics Data System (ADS)

    Wigand, Silvia; Weiden, Norbert; Weiss, Alarich

    1990-04-01

    The 35Cl NQR frequencies, linewidths, and spin-lattice relaxation times T1(35Cl) of 1,2,3-trichlorotrideuterobenzene were measured at various temperatures. The deuterated compound shows the same bleaching out phenomenon as 1,2,3-trichlorobenzene. Single crystal 2H NMR measurements were carried out at 295 and 193 K. The nuclear quadrupole coupling constants at room temperature are in the range of 175.8 ≦ e2qQh-1 (2H)/kHz ≦ 179.5, and the asymmetry parameters η in the range of 0.060 ≦ η (2H) ≦ 0.073. As for the principal axes of the electric field gradient tensor, it was found that Φzz(2H) is parallel to the C - D bond, Φyy (2H) is perpendicular to the benzene ring plane and Φxx(2H) lies in the ring plane. The linewidths of the 2H NMR satellites are idependent of temperature. For the undeuterated compound, the temperature dependence of T1(1H) was also measured. The mechanism leading to the bleaching out of the 35Cl NQR signals is discussed.

  3. Nuclear Quadrupole Resonance (NQR) Method and Probe for Generating RF Magnetic Fields in Different Directions to Distinguish NQR from Acoustic Ringing Induced in a Sample

    DTIC Science & Technology

    1997-08-01

    77,719 TITLE OF THE INVENTION NUCLEAR QUADRUPOLE RESONANCE ( NQR ) METHOD AND PROBE FOR GENERATING RF MAGNETIC FIELDS IN DIFFERENT DIRECTIONS TO...DISTINGUISH NQR FROM ACOUSTIC RINGING INDUCED IN A SAMPLE BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a...nuclear quadrupole 15 resonance ( NQR ) method and probe for generating RF magnetic fields in different directions towards a sample. More specifically

  4. Relaxation of Lattice Inperfections as Studied by Chlorine NQR

    NASA Astrophysics Data System (ADS)

    Hashimoto, Masao; Adachi, Masahiro; Mano, Koichi

    1986-02-01

    The intensities, linewidths, and frequencies of 35Cl NQR signals in 6-nitro-2,4-bis(trichlorom ethyl)-benzo[1,3]dioxine were found to vary remarkably depending on the crystallization methods and annealing. This finding was correlated to the degree of crystal disorder. For a sample obtained by slow crystallization from an ethanolic solution of the compound, the growth of the height of the NQR absorption signal due to annealing was measured as a function of the isothermal annealing time. A kinetic analysis of the growth process gave an activation energy of approx. 110 kJ/mole for the relaxation process of the imperfection dominating the NQR signals. The dimorphism of the compound and the magnitude of the activation energy suggest the presence of misoriented molecules accompanied by vacancies in the crystal lattice of the stable phase.

  5. NQR study of chalcogenide glasses Ge-As-Se.

    PubMed

    Glotova, Olga; Korneva, Irina; Sinyavsky, Nikolay; Ostafin, Michal; Nogaj, Boleslaw

    2011-07-01

    A three-component Ge-As-Se system is studied by the nuclear quadrupole resonance (NQR) method on (75)As nuclei and by the nutation NQR spectroscopy. The NQR (75)As spectra of the glasses Ge(0.021) As(0.375) Se(0.604), Ge(0.043) As(0.348) Se(0.609) and Ge(0.068) As(0.318) Se(0.614) reveal broad lines with two peaks assigned to the main structural unit of As(2)Se(3). With increasing average coordination number ( ̅r), the spectrum signals are shifted towards higher frequencies. At ̅r > 2.54, the spectrum becomes complex, which is a consequence of formation of more complex molecular structures in the glasses of high content of germanium. At fixed frequencies the asymmetry parameter η of the samples studied is determined. Copyright © 2011 John Wiley & Sons, Ltd.

  6. Neutron damage studies of organic materials with NQR spectroscopy

    SciTech Connect

    Hintenlang, D.E.; Jamil, K. )

    1992-01-01

    Noninvasive techniques for the evaluation of radiation damage to materials exposed to neutrons provide valuable methods for monitoring neutron-induced radiation damage. Radiation damage to many organic materials is difficult to monitor without destructive testing. The authors present a new technique for the evaluation of neutron-induced radiation damage based on nuclear quadrupole resonance (NQR) techniques. This demonstrates the NQR response to neutron damage in two organic materials and provides quantitative estimates of microdosimetry and damage sites associated with neutron-induced damage in these materials. They have used {sup 14}N as a probe nucleus to detect molecular bonding changes induced by neutron irradiation. For these studies, two simple, nitrogen containing, organic materials known to provide strong NQR signals were chosen: urea (CO(NH{sub 2}){sub 2}) and thiourea (CS(NH{sub 2}){sub 2}).

  7. Rapid detection of arsenic minerals using portable broadband NQR

    NASA Astrophysics Data System (ADS)

    Lehmann-Horn, J. A.; Miljak, D. G.; O'Dell, L. A.; Yong, R.; Bastow, T. J.

    2014-10-01

    The remote real-time detection of specific arsenic species would significantly benefit in minerals processing to mitigate the release of arsenic into aquatic environments and aid in selective mining. At present, there are no technologies available to detect arsenic minerals in bulk volumes outside of laboratories. Here we report on the first room-temperature broadband 75As nuclear quadrupole resonance (NQR) detection of common and abundant arsenic ores in the Earth crust using a large sample (0.78 L) volume prototype sensor. Broadband excitation aids in detection of natural minerals with low crystallinity. We briefly discuss how the proposed NQR detector could be employed in mining operations.

  8. Recording 2-D Nutation NQR Spectra by Random Sampling Method

    PubMed Central

    Sinyavsky, Nikolaj; Jadzyn, Maciej; Ostafin, Michal; Nogaj, Boleslaw

    2010-01-01

    The method of random sampling was introduced for the first time in the nutation nuclear quadrupole resonance (NQR) spectroscopy where the nutation spectra show characteristic singularities in the form of shoulders. The analytic formulae for complex two-dimensional (2-D) nutation NQR spectra (I = 3/2) were obtained and the condition for resolving the spectral singularities for small values of an asymmetry parameter η was determined. Our results show that the method of random sampling of a nutation interferogram allows significant reduction of time required to perform a 2-D nutation experiment and does not worsen the spectral resolution. PMID:20949121

  9. Recording 2-D Nutation NQR Spectra by Random Sampling Method.

    PubMed

    Glotova, Olga; Sinyavsky, Nikolaj; Jadzyn, Maciej; Ostafin, Michal; Nogaj, Boleslaw

    2010-10-01

    The method of random sampling was introduced for the first time in the nutation nuclear quadrupole resonance (NQR) spectroscopy where the nutation spectra show characteristic singularities in the form of shoulders. The analytic formulae for complex two-dimensional (2-D) nutation NQR spectra (I = 3/2) were obtained and the condition for resolving the spectral singularities for small values of an asymmetry parameter η was determined. Our results show that the method of random sampling of a nutation interferogram allows significant reduction of time required to perform a 2-D nutation experiment and does not worsen the spectral resolution.

  10. (75)As NQR studies on FeAs2.

    PubMed

    Lehmann-Horn, J A; Yong, R; Miljak, D G; Bastow, T J

    2015-10-01

    (75)As NQR spectra and relaxation times of synthetic and natural FeAs2 samples have been studied at variable static magnetic field and temperature. FeAs2 is a well understood diamagnetic semiconductor and occurs as the natural mineral lollingite in selected ore deposits. We observed a spin-spin relaxation time enhancement of up to five in synthetic powders in the presence of a weak external static magnetic field. The effect is of interest with regard to signal-to-noise ratio improvement for materials characterization applications where broad NQR absorption lines are excited with wideband pulse sequences. Copyright © 2015 Elsevier Inc. All rights reserved.

  11. Comparison of various NMR methods for the indirect detection of nitrogen-14 nuclei via protons in solids

    NASA Astrophysics Data System (ADS)

    Shen, Ming; Trébosc, Julien; O'Dell, Luke A.; Lafon, Olivier; Pourpoint, Frédérique; Hu, Bingwen; Chen, Qun; Amoureux, Jean-Paul

    2015-09-01

    We present an experimental comparison of several through-space Hetero-nuclear Multiple-Quantum Correlation experiments, which allow the indirect observation of homo-nuclear single- (SQ) or double-quantum (DQ) 14N coherences via spy 1H nuclei. These 1H-{14N} D-HMQC sequences differ not only by the order of 14N coherences evolving during the indirect evolution, t1, but also by the radio-frequency (rf) scheme used to excite and reconvert these coherences under Magic-Angle Spinning (MAS). Here, the SQ coherences are created by the application of center-band frequency-selective pulses, i.e. long and low-power rectangular pulses at the 14N Larmor frequency, ν0(14N), whereas the DQ coherences are excited and reconverted using rf irradiation either at ν0(14N) or at the 14N overtone frequency, 2ν0(14N). The overtone excitation is achieved either by constant frequency rectangular pulses or by frequency-swept pulses, specifically Wide-band, Uniform-Rate, and Smooth-Truncation (WURST) pulse shapes. The present article compares the performances of four different 1H-{14N} D-HMQC sequences, including those with 14N rectangular pulses at ν0(14N) for the indirect detection of homo-nuclear (i) 14N SQ or (ii) DQ coherences, as well as their overtone variants using (iii) rectangular or (iv) WURST pulses. The compared properties include: (i) the sensitivity, (ii) the spectral resolution in the 14N dimension, (iii) the rf requirements (power and pulse length), as well as the robustness to (iv) rf offset and (v) MAS frequency instabilities. Such experimental comparisons are carried out for γ-glycine and L-histidine.HCl monohydrate, which contain 14N sites subject to moderate quadrupole interactions. We demonstrate that the optimum choice of the 1H-{14N} D-HMQC method depends on the experimental goal. When the sensitivity and/or the robustness to offset are the major concerns, the D-HMQC sequence allowing the indirect detection of 14N SQ coherences should be employed. Conversely, when the highest resolution and/or adjusted indirect spectral width are needed, overtone experiments are the method of choice. The overtone scheme using WURST pulses results in broader excitation bandwidths than that using rectangular pulses, at the expense of reduced sensitivity. Numerically exact simulations also show that the sensitivity of the overtone 1H-{14N} D-HMQC experiment increases for larger quadrupole interactions.

  12. NqrM (DUF539) Protein Is Required for Maturation of Bacterial Na+-Translocating NADH:Quinone Oxidoreductase

    PubMed Central

    Kostyrko, Vitaly A.; Bertsova, Yulia V.; Serebryakova, Marina V.; Baykov, Alexander A.

    2015-01-01

    ABSTRACT Na+-translocating NADH:quinone oxidoreductase (Na+-NQR) catalyzes electron transfer from NADH to ubiquinone in the bacterial respiratory chain, coupled with Na+ translocation across the membrane. Na+-NQR maturation involves covalent attachment of flavin mononucleotide (FMN) residues, catalyzed by flavin transferase encoded by the nqr-associated apbE gene. Analysis of complete bacterial genomes has revealed another putative gene (duf539, here renamed nqrM) that usually follows the apbE gene and is present only in Na+-NQR-containing bacteria. Expression of the Vibrio harveyi nqr operon alone or with the associated apbE gene in Escherichia coli, which lacks its own Na+-NQR, resulted in an enzyme incapable of Na+-dependent NADH or reduced nicotinamide hypoxanthine dinucleotide (dNADH) oxidation. However, fully functional Na+-NQR was restored when these genes were coexpressed with the V. harveyi nqrM gene. Furthermore, nqrM lesions in Klebsiella pneumoniae and V. harveyi prevented production of functional Na+-NQR, which could be recovered by an nqrM-containing plasmid. The Na+-NQR complex isolated from the nqrM-deficient strain of V. harveyi lacks several subunits, indicating that nqrM is necessary for Na+-NQR assembly. The protein product of the nqrM gene, NqrM, contains a single putative transmembrane α-helix and four conserved Cys residues. Mutating one of these residues (Cys33 in V. harveyi NqrM) to Ser completely prevented Na+-NQR maturation, whereas mutating any other Cys residue only decreased the yield of the mature protein. These findings identify NqrM as the second specific maturation factor of Na+-NQR in proteobacteria, which is presumably involved in the delivery of Fe to form the (Cys)4[Fe] center between subunits NqrD and NqrE. IMPORTANCE Na+-translocating NADH:quinone oxidoreductase complex (Na+-NQR) is a unique primary Na+ pump believed to enhance the vitality of many bacteria, including important pathogens such as Vibrio cholerae, Vibrio

  13. NqrM (DUF539) Protein Is Required for Maturation of Bacterial Na+-Translocating NADH:Quinone Oxidoreductase.

    PubMed

    Kostyrko, Vitaly A; Bertsova, Yulia V; Serebryakova, Marina V; Baykov, Alexander A; Bogachev, Alexander V

    2015-12-07

    Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR) catalyzes electron transfer from NADH to ubiquinone in the bacterial respiratory chain, coupled with Na(+) translocation across the membrane. Na(+)-NQR maturation involves covalent attachment of flavin mononucleotide (FMN) residues, catalyzed by flavin transferase encoded by the nqr-associated apbE gene. Analysis of complete bacterial genomes has revealed another putative gene (duf539, here renamed nqrM) that usually follows the apbE gene and is present only in Na(+)-NQR-containing bacteria. Expression of the Vibrio harveyi nqr operon alone or with the associated apbE gene in Escherichia coli, which lacks its own Na(+)-NQR, resulted in an enzyme incapable of Na(+)-dependent NADH or reduced nicotinamide hypoxanthine dinucleotide (dNADH) oxidation. However, fully functional Na(+)-NQR was restored when these genes were coexpressed with the V. harveyi nqrM gene. Furthermore, nqrM lesions in Klebsiella pneumoniae and V. harveyi prevented production of functional Na(+)-NQR, which could be recovered by an nqrM-containing plasmid. The Na(+)-NQR complex isolated from the nqrM-deficient strain of V. harveyi lacks several subunits, indicating that nqrM is necessary for Na(+)-NQR assembly. The protein product of the nqrM gene, NqrM, contains a single putative transmembrane α-helix and four conserved Cys residues. Mutating one of these residues (Cys33 in V. harveyi NqrM) to Ser completely prevented Na(+)-NQR maturation, whereas mutating any other Cys residue only decreased the yield of the mature protein. These findings identify NqrM as the second specific maturation factor of Na(+)-NQR in proteobacteria, which is presumably involved in the delivery of Fe to form the (Cys)4[Fe] center between subunits NqrD and NqrE. Na(+)-translocating NADH:quinone oxidoreductase complex (Na(+)-NQR) is a unique primary Na(+) pump believed to enhance the vitality of many bacteria, including important pathogens such as Vibrio cholerae

  14. Applications of Nanoscale NMR Using Ensembles of NV Centers in Diamond

    NASA Astrophysics Data System (ADS)

    Bucher, Dominik; Glenn, David; Walsworth, Ronald

    2016-05-01

    Ensembles of nitrogen vacancy (NV) centers in diamond are now the frontier modality for nuclear magnetic resonance (NMR) signals at length-scales of microns to Angstroms. Promising applications including NMR and nuclear quadrupole resonance (NQR) spectroscopy in sub-nanoliter volumes, studies of diffusion and transport in small samples of biological tissue, and magnetic resonance imaging (MRI) of individual biological cells and molecules. Here, we describe recent progress toward such applications.

  15. 35Cl NQR study of geometric isotope effect in hydrogen bonded chlorooctanes

    NASA Astrophysics Data System (ADS)

    Zdanowska-Fraçzek, M.

    1994-05-01

    35Cl NQR spectroscopy was applied to study the geometric isotope effect in a wide range of 2 : 1 salts of chloroacetic, trichloroacetic and difluorochloroacetic acids. The NQR results were correlated with IR spectroscopic studies, which provided information on the potential shape for proton motion. The NQR results were discussed on the basis of a variational correlated ground state wave function theory of a single hydrogen bond.

  16. The single NqrB and NqrC subunits in the Na(+)-translocating NADH: quinone oxidoreductase (Na(+)-NQR) from Vibrio cholerae each carry one covalently attached FMN.

    PubMed

    Casutt, Marco S; Schlosser, Andreas; Buckel, Wolfgang; Steuber, Julia

    2012-10-01

    The Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR) is the prototype of a novel class of flavoproteins carrying a riboflavin phosphate bound to serine or threonine by a phosphodiester bond to the ribityl side chain. This membrane-bound, respiratory complex also contains one non-covalently bound FAD, one non-covalently bound riboflavin, ubiquinone-8 and a [2Fe-2S] cluster. Here, we report the quantitative analysis of the full set of flavin cofactors in the Na(+)-NQR and characterize the mode of linkage of the riboflavin phosphate to the membrane-bound NqrB and NqrC subunits. Release of the flavin by β-elimination and analysis of the cofactor demonstrates that the phosphate group is attached at the 5'-position of the ribityl as in authentic FMN and that the Na(+)-NQR contains approximately 1.7mol covalently bound FMN per mol non-covalently bound FAD. Therefore, each of the single NqrB and NqrC subunits in the Na(+)-NQR carries a single FMN. Elimination of the phosphodiester bond yields a dehydro-2-aminobutyrate residue, which is modified with β-mercaptoethanol by Michael addition. Proteolytic digestion followed by mass determination of peptide fragments reveals exclusive modification of threonine residues, which carry FMN in the native enzyme. The described reactions allow quantification and localization of the covalently attached FMNs in the Na(+)-NQR and in related proteins belonging to the Rhodobacter nitrogen fixation (RNF) family of enzymes. This article is part of a Special Issue entitled: 17th European Bioenergetics Conference (EBEC 2012).

  17. 14N NQR and relaxation in ammonium nitrate

    NASA Astrophysics Data System (ADS)

    Stephenson, David

    2015-04-01

    The complete 14N nuclear quadrupole resonance (NQR) spectrum of ammonium nitrate is presented recorded using two double resonance techniques - double contact cross relaxation and zero field NQR. The spectra gave the quadrupole coupling constant (Qcc) and asymmetry parameter ( η) values for the nitro of 611 kHz, 0.229 and that for the ammonium nitrogen of 242 kHz, 0.835. The three relaxation transition probabilities have been determined for both the nitro and ammonium nitrogen atoms. The bi-exponential relaxation times (T 1) were measured at 295 K. The values for nitro are 16.9 s and 10.5 s and that of the ammonium are 23.0 s and 16.4 s.

  18. Investigating a Quadrant Surface Coil Array for NQR Remote Sensing

    DTIC Science & Technology

    2014-10-23

    resonant at the same frequency. Coils will be in a “quadrant surface layout” in which all coils are in a four square arrangement to measure mutual ...Coil Array, probe, Nuclear Magnetic Resonance, tuning, decoupling, RLC, mutual coupling, RLC I. INTRODUCTION N Nuclear quadrupole resonance (NQR...same tuning to the 28.578MHz resonant frequency. III. QUADRANT MUTUAL COUPLING Now that the probes are tuned individually, the focus is now on

  19. Downregulation of Na(+)-NQR complex is essential for Vibrio alginolyticus in resistance to balofloxacin.

    PubMed

    Li, Peipei; Liu, Xianjie; Li, Hui; Peng, Xuan-Xian

    2012-05-17

    Increasingly isolated frequency of antibiotic-resistant V. alginolyticus strains in clinic and aquaculture has been reported, but the mechanisms of V. alginolyticus antibiotic resistance are largely absent. In the present study, native/SDS-PAGE based proteomics, which may provide information on protein-protein interaction, was utilized to investigate differential proteins of V. alginolyticus in resistance to balofloxacin. Ten proteins were altered, in which V12G01_04671, V12G01_00457, V12G01_15927, V12G01_15240, NqrA (spot 26), and NqrF (spot 30) were downregulated, while V12G01_22043, TolC, V12G01_15130, V12G01_19297 were upregulated. Importantly, the two components of Na(+)-NQR complex, NqrA and NqrF, were vertically lined and was further investigated. Western blotting assay indicated that downregulation of the two proteins contrasted sharply with upregulation of a control protein TolC, which was consistent with the result obtained from 2-DE gel analysis. Furthermore, overexpression of NqrA, NqrF and TolC resulted in decrease and elevation of bacterial survival ability in medium with balofloxacin, respectively. These results indicate that downregulation of Na(+)-NQR complex is essential for V. alginolyticus resistance to balofloxacin. This is the first report on the role of Na(+)-NQR complex in antibiotic resistance. This finding highlights the way to an understanding of antibiotic-resistant mechanisms in content of metabolic regulation. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. An NQR study of the polymorphism of triphenylchloromethane.

    PubMed

    Brunetti, A H

    2004-01-01

    This work is a study of the polymorphic transformations of triphenylchloromethane (TPCM) as well as the structure and dynamics of this molecular solid. Crystalline TPCM has been studied by a variety of techniques and many of its physical properties have been characterized. Previous crystallographic studies have reported the existence of two crystalline phases. Phase II, stable above 372 K, is trigonal with space group P3; and Z = 6. The compound associates pairwise (halogen-to-halogen and triphenylmethyl-to-triphenylmethyl) and linearly with all carbon-halogen bonds aligned with C3 and S6 axes of the lattice. Below 372 K, a triclinic modification (phase III) is found (P1;, Z = 10) where the molecules are also aligned pairwise with close Cl cdots, three dots, centered Cl interactions. However, the C-Cl bonds were no longer parallel. On the other hand, DTA studies have also reported a phase transition at 381 K (to phase I) that can been obtained from slow evaporation of pentane or ether solutions. Crystallographic information about these phases has not been obtained in the literature. Five NQR lines have been observed from liquid nitrogen temperature to 372 K in good agreement with phase III that has Z = 10. Above 372 K, three lines are observed which are related to phase II. Any effort to observe phase I through NQR failed; phase II remains until the sample is melted. Instead, if phase II is cooled down, a second-order phase transition to a new phase at 259 K is observed through NQR studies. The temperature dependence of experimental data in the phase transition region is well explained assuming the transitions occur when molecules in the crystal lattice change their direction uniformly with a change in temperature and the liberational modes, coupled in an anharmonic way with the uniform mode, change their frequencies in such a way that entropy compensates the unfavorable potential energy increase due to the uniform angular tilt.

  1. Variable-Pitch Rectangular Cross-section Radiofrequency Coils for the Nitrogen-14 Nuclear Quadrupole Resonance Investigation of Sealed Medicines Packets

    PubMed Central

    2012-01-01

    The performance of rectangular radio frequency (RF) coils capable of being used to detect nuclear quadrupole resonance (NQR) signals from blister packs of medicines has been compared. The performance of a fixed-pitch RF coil was compared with that from two variable-pitch coils, one based on a design in the literature and the other optimized to obtain the most homogeneous RF field over the whole volume of the coil. It has been shown from 14N NQR measurements with two medicines, the antibiotic ampicillin (as trihydrate) and the analgesic medicine Paracetamol, that the latter design gives NQR signal intensities almost independent of the distribution of the capsules or pills within the RF coil and is therefore more suitable for quantitative analysis. PMID:23057555

  2. Investigation of YBa sub 2 Cu sub 3 O sub 7 by NMR and construction of an ultralow-temperature cryostat

    SciTech Connect

    Lovellette, M.N.

    1989-01-01

    The author reports investigation by {sup 63}Cu NMR and NQR on the high-temperature superconductor YBa{sub 2}Cu{sub 3}O{sub 7}. The decay of the magnetization observed following an inversion of the Cu spin system is found to be nonexponential. The spin-lattice relaxation rate observed by NMR is not affected by the onset of superconductivity, and throughout the temperature range of 5 to 150 K is only weakly temperature-dependent. However, the NQR spin-lattice relaxation rate drops dramatically with decreasing temperature in the superconducting state. This suggests that different relaxation mechanism are functioning in zero field as observed by NQR and high field as observed by NMR. The NMR spin-lattice relaxation can be explained by the presence of a dilute fluctuating spin system which orders at a temperature of approximately 1 K. The concentration of spins found by NMR techniques, 0.67 {plus minus} 0.25 {times} 10{sup 21} spins/cm{sup 3} is in good agreement with the concentration determined by dc susceptibility measurements. The design and construction of a cryostat to conduct high-resolution NMR measurements on {sup 3}He-B is described.

  3. (14)N NQR, relaxation and molecular dynamics of the explosive TNT.

    PubMed

    Smith, John A S; Rowe, Michael D; Althoefer, Kaspar; Peirson, Neil F; Barras, Jamie

    2015-10-01

    Multiple pulse sequences are widely used for signal enhancement in NQR detection applications. Since the various (14)N NQR relaxation times, signal decay times and frequency of each NQR line have a major influence on detection sequence performance, it is important to characterise these parameters and their temperature variation, as fully as possible. In this paper we discuss such measurements for a number of the ν+ and ν- NQR lines of monoclinic and orthorhombic TNT and relate the temperature variation results to molecular dynamics. The temperature variation of the (14)N spin-lattice relaxation times T1 is interpreted as due to hindered rotation of the NO2 group about the C-NO2 bond with an activation energy of 89 kJ mol(-1) for the ortho and para groups of monoclinic TNT and 70 kJ mol(-1) for the para group of orthorhombic TNT. Copyright © 2015 Elsevier Inc. All rights reserved.

  4. /sup 127/I NQR spectra of carborane-containing compounds of polycoordinated iodine

    SciTech Connect

    Semin, G.K.; Grushin, V.V.; Gushchin, S.I.; Lisichkina, I.N.; Petokhov, S.A.; Tolstaya, T.P.

    1985-05-20

    The NQR spectra of polycoordinated iodine compounds is studied. A table presents the I 127 NQR spectra of electroneutral PhIC1/sub 2/ derivatives with intermolecular coordination in the solid state and ionic compounds including compounds with interionic coordination. A considerable increase in the quadrupole coupling constants and significant decrease in the asymmetry parameter is found in carborane-containing CBIC1/sub 2/ and PhCBIX compounds in comparison with the corresponding phenyl and diphenyl derivatives.

  5. Study of Caking of Powders Using NQR Relaxometry with Inversion of the Laplace Transform

    NASA Astrophysics Data System (ADS)

    Sinyavsky, N. Ya.

    2017-04-01

    For the first time, it has been proposed to study the processes of caking nonmetallic powders containing quadrupole nuclei using the distribution of the spin-lattice and spin-spin relaxation times in NQR. The results of experimental studies of the effect of caking samples on the distributions of relaxation times of T1 and T2 for the 14N NQR in powders of NaNO2 and C6H12N4 are presented.

  6. Na+-NQR (Na+-translocating NADH:ubiquinone oxidoreductase) as a novel target for antibiotics.

    PubMed

    Dibrov, Pavel; Dibrov, Elena; Pierce, Grant N

    2017-09-01

    The recent breakthrough in structural studies on Na+-translocating NADH:ubiquinone oxidoreductase (Na+-NQR) from the human pathogen Vibrio cholerae creates a perspective for the systematic design of inhibitors for this unique enzyme, which is the major Na+ pump in aerobic pathogens. Widespread distribution of Na+-NQR among pathogenic species, its key role in energy metabolism, its relation to virulence in different species as well as its absence in eukaryotic cells makes this enzyme especially attractive as a target for prospective antibiotics. In this review, the major biochemical, physiological and, especially, the pharmacological aspects of Na+-NQR are discussed to assess its 'target potential' for drug development. A comparison to other primary bacterial Na+ pumps supports the contention that NQR is a first rate prospective target for a new generation of antimicrobials. A new, narrowly targeted furanone inhibitor of NQR designed in our group is presented as a molecular platform for the development of anti-NQR remedies. © FEMS 2017. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  7. Broadband excitation and indirect detection of nitrogen-14 in rotating solids using Delays Alternating with Nutation (DANTE)

    NASA Astrophysics Data System (ADS)

    Vitzthum, Veronika; Caporini, Marc A.; Ulzega, Simone; Bodenhausen, Geoffrey

    2011-09-01

    A train of short rotor-synchronized pulses in the manner of Delays Alternating with Nutations for Tailored Excitation (DANTE) applied to nitrogen-14 nuclei ( I = 1) in samples spinning at the magic angle at high frequencies (typically νrot = 62.5 kHz so that τrot = 16 μs) allows one to achieve uniform excitation of a great number of spinning sidebands that arise from large first-order quadrupole interactions, as occur for aromatic nitrogen-14 nuclei in histidine. With routine rf amplitudes ω1( 14N)/(2 π) = 60 kHz and very short pulses of a typical duration 0.5 < τp < 2 μs, efficient excitation can be achieved with 13 rotor-synchronized pulses in 13 τrot = 208 μs. Alternatively, with 'overtone' DANTE sequences using 2, 4, or 8 pulses per rotor period one can achieve efficient broadband excitation in fewer rotor periods, typically 2-4 τrot. These principles can be combined with the indirect detection of 14N nuclei via spy nuclei with S = ½ such as 1H or 13C in the manner of Dipolar Heteronuclear Multiple-Quantum Correlation (D-HMQC).

  8. Broadband excitation and indirect detection of nitrogen-14 in rotating solids using Delays Alternating with Nutation (DANTE).

    PubMed

    Vitzthum, Veronika; Caporini, Marc A; Ulzega, Simone; Bodenhausen, Geoffrey

    2011-09-01

    A train of short rotor-synchronized pulses in the manner of Delays Alternating with Nutations for Tailored Excitation (DANTE) applied to nitrogen-14 nuclei (I=1) in samples spinning at the magic angle at high frequencies (typically νrot=62.5 kHz so that τrot=16 μs) allows one to achieve uniform excitation of a great number of spinning sidebands that arise from large first-order quadrupole interactions, as occur for aromatic nitrogen-14 nuclei in histidine. With routine rf amplitudes ω1(14N)/(2π)=60 kHz and very short pulses of a typical duration 0.5<τp<2 μs, efficient excitation can be achieved with 13 rotor-synchronized pulses in 13 τrot=208 μs. Alternatively, with 'overtone' DANTE sequences using 2, 4, or 8 pulses per rotor period one can achieve efficient broadband excitation in fewer rotor periods, typically 2-4 τrot. These principles can be combined with the indirect detection of 14N nuclei via spy nuclei with S=½ such as 1H or 13C in the manner of Dipolar Heteronuclear Multiple-Quantum Correlation (D-HMQC). Copyright © 2011 Elsevier Inc. All rights reserved.

  9. Solid-state nitrogen-14 nuclear magnetic resonance enhanced by dynamic nuclear polarization using a gyrotron.

    PubMed

    Vitzthum, Veronika; Caporini, Marc A; Bodenhausen, Geoffrey

    2010-07-01

    By combining indirect detection of 14N with dynamic nuclear polarization (DNP) using a gyrotron, the signal-to-noise ratio can be dramatically improved and the recovery delay between subsequent experiments can be shortened. Spectra of glassy samples of the amino acid proline doped with the stable bi-radical TOTAPOL rotating at 15.625 kHz at 110K were obtained in a 400 MHz solid-state NMR spectrometer equipped with a gyrotron for microwave irradiation at 263 GHz. DNP enhancement factors on the order of epsilon approximately 40 were achieved. The recovery delays can be reduced from 60 s without radicals at 300 K to 6 s with radicals at 110 K. In the absence of radicals at room temperature, the proton relaxation in proline is inefficient due to the absence of rotating methyl groups and other heat sinks, thus making long recovery delays mandatory. DNP allows one to reduce the acquisition times of 13C-detected 14N spectra from several days to a few hours. Copyright (c) 2010 Elsevier Inc. All rights reserved.

  10. Site-selective NMR measurements in single crystal PrNb2Al20

    NASA Astrophysics Data System (ADS)

    Kubo, Tetsuro; Kotegawa, Hisashi; Tou, Hideki; Harima, Hisatomo; Higashinaka, Ryuji; Nakama, Akihiro; Aoki, Yuji; Sato, Hideyuki

    2017-04-01

    We report the result and analysis of the nuclear magnetic resonance (NMR) measurements at the magnetic field of 8.57 T and temperature of 80 K using a single crystal PrNb2Al20. Combining the field angle dependence of NMR spectra, numerical simulation, and band calculation, we deconvoluted the NMR signals from the Nb, Al 48 f, and Al 96g sites. Unfortunately, the overlapping of NMR lines prevents us to extract the NMR signals from the Al 16c site. However, the obtained nuclear quadrupole resonance (NQR) parameters for the Nb and Al 48f sites are consistent with the previous reports [T. Kubo et al., 2014 JPS Conf. Proc. 3 012031; 2015 J. Phys.: Conf. Ser. 592 012093; 2016 J. Phys. Conf.: Ser. 683 012015] and for the Al 96g site are refined to be vQ = 0.98 MHz and η = 0.46.

  11. A general numerical analysis of time-domain NQR experiments.

    PubMed

    Harel, Elad; Cho, Herman

    2006-12-01

    We introduce a general numerical approach for solving the Liouville equation of an isolated quadrupolar nuclide that can be used to analyze the unitary dynamics of time-domain NQR experiments. A numerical treatment is necessitated by the dimensionality of the Liouville space, which precludes analytical, closed form solutions for I > 3/2. Accurate simulations of experimental nutation curves, forbidden transition intensities, powder and single crystal spectra, and off-resonance irradiation dynamics can be computed with this method. We also examine the validity of perturbative approximations where the signal intensity of a transition is proportional to the transition moment between the eigenstates of the system, thus providing a simple basis for determining selection rules. Our method allows us to calculate spectra for all values of the asymmetry parameter, eta, and sample orientations relative to the coil axis. We conclude by demonstrating the methodology for calculating the response of the quadrupole system to amplitude- and frequency-modulated pulses.

  12. Gapless superconductivity in overdoped Hg system: Cu-NQR study

    SciTech Connect

    Ohsugi, Shigeki; Tsuchiya, Tetsuo; Koyama, Tadashi; Fueki, Kazuo

    1996-11-01

    The nuclear quadrupole resonance (NQR) investigation of Cu in the overdoped compounds HgBa{sub 2}CuO{sub y} (Hg1201) with Y=4.06 (T{sub c}=92K) and 4.11 (64K) and HgBa{sub 2}CaCu{sub 2}O{sub y} (Hg1212) with y=6.13 (T{sub c}=125K) and 6.21 (117K) was carried out in zero field. From the temperature (T) dependence of the nuclear spin-lattice relaxation time, T{sub 1}, of {sup 63}Cu, the authors discuss a cause of the T{sub c} suppression with decreasing the number of CuO{sub 2} layers.

  13. A General Numerical Analysis of Time-Domain NQR Experiments

    SciTech Connect

    Harel, Elad; Cho, Herman M.

    2006-12-01

    We introduce a general numerical approach for solving the Liouville equation of a quadrupolar nuclide that we show can be used to analyze time-domain NQR experiments. A computer-based treatment is necessitated by the dimensionality of the Liouville space, which precludes analytical, closed form solutions for I > 3/2. Accurate simulations of experimental nutation curves, forbidden transition intensities, powder and single crystal spectra, and off-resonance irradiation dynamics can be computed with this method. We also examine the validity of perturbative approximations where the signal intensity of a transition is proportional to the transition moment between the eigenstates of the system, thus providing a simple basis for determining selection rules. Our method allows us to calculate spectra for all values of the asymmetry parameter, ?, and sample orientations relative to the coil axis. We conclude by demonstrating the methodology for calculating the response of the quadrupole system to amplitude- and frequency-modulated pulses.

  14. Localization and Function of the Membrane-bound Riboflavin in the Na+-translocating NADH:Quinone Oxidoreductase (Na+-NQR) from Vibrio cholerae*

    PubMed Central

    Casutt, Marco S.; Huber, Tamara; Brunisholz, René; Tao, Minli; Fritz, Günter; Steuber, Julia

    2010-01-01

    The sodium ion-translocating NADH:quinone oxidoreductase (Na+-NQR) from the human pathogen Vibrio cholerae is a respiratory membrane protein complex that couples the oxidation of NADH to the transport of Na+ across the bacterial membrane. The Na+-NQR comprises the six subunits NqrABCDEF, but the stoichiometry and arrangement of these subunits are unknown. Redox-active cofactors are FAD and a 2Fe-2S cluster on NqrF, covalently attached FMNs on NqrB and NqrC, and riboflavin and ubiquinone-8 with unknown localization in the complex. By analyzing the cofactor content and NADH oxidation activity of subcomplexes of the Na+-NQR lacking individual subunits, the riboflavin cofactor was unequivocally assigned to the membrane-bound NqrB subunit. Quantitative analysis of the N-terminal amino acids of the holo-complex revealed that NqrB is present in a single copy in the holo-complex. It is concluded that the hydrophobic NqrB harbors one riboflavin in addition to its covalently attached FMN. The catalytic role of two flavins in subunit NqrB during the reduction of ubiquinone to ubiquinol by the Na+-NQR is discussed. PMID:20558724

  15. Localization and function of the membrane-bound riboflavin in the Na+-translocating NADH:quinone oxidoreductase (Na+-NQR) from Vibrio cholerae.

    PubMed

    Casutt, Marco S; Huber, Tamara; Brunisholz, René; Tao, Minli; Fritz, Günter; Steuber, Julia

    2010-08-27

    The sodium ion-translocating NADH:quinone oxidoreductase (Na(+)-NQR) from the human pathogen Vibrio cholerae is a respiratory membrane protein complex that couples the oxidation of NADH to the transport of Na(+) across the bacterial membrane. The Na(+)-NQR comprises the six subunits NqrABCDEF, but the stoichiometry and arrangement of these subunits are unknown. Redox-active cofactors are FAD and a 2Fe-2S cluster on NqrF, covalently attached FMNs on NqrB and NqrC, and riboflavin and ubiquinone-8 with unknown localization in the complex. By analyzing the cofactor content and NADH oxidation activity of subcomplexes of the Na(+)-NQR lacking individual subunits, the riboflavin cofactor was unequivocally assigned to the membrane-bound NqrB subunit. Quantitative analysis of the N-terminal amino acids of the holo-complex revealed that NqrB is present in a single copy in the holo-complex. It is concluded that the hydrophobic NqrB harbors one riboflavin in addition to its covalently attached FMN. The catalytic role of two flavins in subunit NqrB during the reduction of ubiquinone to ubiquinol by the Na(+)-NQR is discussed.

  16. Magnetic and structural properties of an octanuclear Cu(II) S=1/2 mesoscopic ring: Susceptibility and NMR measurements

    SciTech Connect

    Lascialfari, A.; Jang, Z. H.; Borsa, F.; Gatteschi, D.; Cornia, A.; Rovai, D.; Caneschi, A.; Carretta, P.

    2000-03-01

    Magnetic susceptibility, {sup 1}H NMR and {sup 63}Cu NMR-NQR experiments on two slightly different species of the molecular S=1/2 antiferromagnetic (AF) ring Cu8, [Cu{sub 8}(dmpz){sub 8}(OH){sub 8}]{center_dot}2C{sub 5}H{sub 5}N (Cu8P) and [Cu{sub 8}(dmpz){sub 8}(OH){sub 8}]{center_dot}2C{sub 5}H{sub 5}NO{sub 2} (Cu8N), are presented. The magnetic energy levels are calculated exactly for an isotropic Heisenberg model Hamiltonian in zero magnetic field. From the magnetic susceptibility measurements we estimate the AF exchange coupling constant J{approx}1000 K and the resulting gap {delta}{approx}500 K between the S{sub T}=0 ground state and the S{sub T}=1 first excited state. The {sup 63,65}Cu NQR spectra indicate the presence of four crystallographically inequivalent copper nuclei in each ring. From the combination of the {sup 63}Cu NQR spectra and of the {sup 63}Cu NMR spectra at high magnetic field, we estimate the quadrupole coupling constant v{sub Q} of each site and the average asymmetry parameter {eta} of the electric-field gradient tensor. The nuclear spin-lattice relaxation rate (NSLR) decreases exponentially on decreasing temperature for all nuclei investigated. The gap parameter extracted from {sup 63}Cu NQR-NSLR is the same as for the susceptibility while a smaller value is obtained from the {sup 63}Cu NMR-NSLR in an external magnetic field of 8.2 T. (c) 2000 The American Physical Society.

  17. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1991-01-14

    Copper and cobalt are the key elements in syngas conversion catalyst systems used for higher alcohol synthesis. Their proximity and synergy sensitively control the selectivity and efficiency of the process. It is believed that their outer electronic charge distribution which is responsible for their electrical and magnetic properties might be governing their catalytic properties also. To examine the correlation between catalytic and magnetic properties, a series of copper cobalt catalysts (Co/Cu ratio 5:1 to 5:5) with and without a support were prepared. The nuclear quadrupole resonance spectrum of copper and (zero-field) nuclear magnetic resonance spectrum of cobalt and magnetization and hysteresis character of the catalyst were analyzed. Similar to the catalytic results, the magnetic results also were found to be very sensitive to the preparation technique. The results indicate possible electron exchange between copper and cobalt, and cobalt and the support Titania.

  18. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1991-07-15

    The primary objective of the project is to examine the relations between the catalytic and magnetic properties of the copper-cobalt higher alcohol synthesis catalysts. We have undertaken to investigate the magnetic character by studying the Nuclear Quadrupole resonance of copper and (Zerofield) Nuclear Magnetic Resonance of cobalt in copper cobalt catalysts.

  19. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1990-09-14

    The primary objective of the project is to investigate the magnetic nature of the higher alcohol synthesis catalyst-Cu/Co supported on specific supports: chromia and titania with and without an alkali metal promoter, and examine the relations between catalytic and magnetic properties.

  20. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1991-12-17

    The primary objective of the project is to examine the relations between the catalytic and magnetic properties of the copper-cobalt higher alcohol synthesis catalysts. We have undertaken to investigate the magnetic character by studying the Nuclear Quadrupole resonance of copper and (Zerofield) Nuclear Magnetic Resonance of cobalt in copper cobalt catalysts.

  1. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts

    SciTech Connect

    Not Available

    1992-01-14

    Our studies were essentially concerned with analyzing the magnetic character of the Cu-Co catalysts for Cu/Co ratio ranging from 0.2 to 4 (1,2). The results clearly indicate that; (a) as the copper content increases beyond 50% significant intermetallic interactions occur between copper and cobalt; (b) the magnetic character of the bimetallic clusters formed is sensitively dependant on the method of preparation.

  2. Application of 14N NQR to the study of piroxicam polymorphism.

    PubMed

    Lavrič, Zoran; Pirnat, Janez; Lužnik, Janko; Seliger, Janez; Zagar, Veselko; Trontelj, Zvonko; Srčič, Stane

    2010-12-01

    A study was conducted to test the capability of the (14)N nuclear quadrupole resonance (NQR) method to discriminate qualitatively and quantitatively among different forms of piroxicam. Samples of commercial piroxicam form I and its monohydrate were obtained on the local market. Additionally, samples of form I and II were prepared by recrystallization in 1,2-dichloroethane and ethanol, respectively. DSC and FT-IR were employed as reference methods. A (14)N NQR spectrometer was used to measure samples of different forms and mixtures of piroxicam at 2587 and 3439  kHz. DSC and FT-IR clearly confirmed differences between the different piroxicam forms. Measurements of (14)N NQR signals of different forms of piroxicam at 2587  kHz detected only spectral peaks of form I. The dependence of (14)N NQR signal intensity on the concentration of form I in mixtures with the monohydrate showed a clear linear relationship at both measured frequencies, though the scattering of data was greater at 3439  kHz due to the lower S/N ratio. The (14)N NQR method has the potential to become an additional and important spectroscopic tool in the study of solid-state forms, not only of pure active pharmaceutical ingredients or excipients, but also of their mixtures. This ability lends the method to a possible successful utilization at different levels of pharmaceutical manufacturing and product quality control. © 2010 Wiley-Liss, Inc. and the American Pharmacists Association

  3. A computational NQR study on the hydrogen-bonded lattice of cytosine-5-acetic acid.

    PubMed

    Mirzaei, Mahmoud; Hadipour, Nasser L

    2008-04-15

    A computational study at the level of density functional theory (DFT) employing 6-311++G** standard basis set was carried out to evaluate nuclear quadrupole resonance (NQR) spectroscopy parameters in cytosine-5-acetic acid (C5AA). Since the electric field gradient (EFG) tensors are very sensitive to the electrostatic environment at the sites of quadruple nuclei, the most possible interacting molecules with the target one were considered in a five-molecule model system of C5AA using X-ray coordinates transforming. The hydrogen atoms positions were optimized and two model systems of original and H-optimized C5AA were considered in NQR calculations. The calculated EFG tensors at the sites of (17)O, (14)N, and (2)H nuclei were converted to their experimentally measurable parameters, quadrupole coupling constants and asymmetry parameters. The evaluated NQR parameters reveal that the nuclei in original and H-optimized systems contribute to different hydrogen bonding (HB) interaction. The comparison of calculated parameters between optimized isolated gas-phase and crystalline monomer also shows the relationship between the structural deformation and NQR parameters in C5AA. The basis set superposition error (BSSE) calculations yielded no significant errors for employed basis set in the evaluation of NQR parameters. All the calculations were performed by Gaussian 98 package of program. (c) 2007 Wiley Periodicals, Inc.

  4. Oxidant-induced formation of a neutral flavosemiquinone in the Na+-translocating NADH:Quinone oxidoreductase (Na+-NQR) from Vibrio cholerae.

    PubMed

    Tao, Minli; Casutt, Marco S; Fritz, Günter; Steuber, Julia

    2008-01-01

    The Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR) from the human pathogen Vibrio cholerae is a respiratory flavo-FeS complex composed of the six subunits NqrA-F. The Na(+)-NQR was produced as His(6)-tagged protein by homologous expression in V. cholerae. The isolated complex contained near-stoichiometric amounts of non-covalently bound FAD (0.78 mol/mol Na(+)-NQR) and riboflavin (0.70 mol/mol Na(+)-NQR), catalyzed NADH-driven Na(+) transport (40 nmol Na(+)min(-1) mg(-1)), and was inhibited by 2-n-heptyl-4-hydroxyquinoline-N-oxide. EPR spectroscopy showed that Na(+)-NQR as isolated contained very low amounts of a neutral flavosemiquinone (10(-3) mol/mol Na(+)-NQR). Reduction with NADH resulted in the formation of an anionic flavosemiquinone (0.10 mol/mol Na(+)-NQR). Subsequent oxidation of the Na(+)-NQR with ubiquinone-1 or O(2) led to the formation of a neutral flavosemiquinone (0.24 mol/mol Na(+)-NQR). We propose that the Na(+)-NQR is fully oxidized in its resting state, and discuss putative schemes of NADH-triggered redox transitions.

  5. Pressure Dependence of the Chlorine NQR in Three Solid Chloro Anisoles

    NASA Astrophysics Data System (ADS)

    Suresh, K. S.; Ramesh, K. P.; Rao, C. Raghavendra; Ramakrishna, J.

    2001-11-01

    The 35C1 Nuclear Quadrupole Resonance (NQR) frequency (VQ) and spin lattice relaxation time (T1) in the three anisoles 2,3,4-trichloroanisole, 2,3,6-trichloroanisole and 3,5-dichloroanisole have been measured as a function of pressure upto 5.1 kbar at 300 K, and the data have been analysed to estimate the temperature coefficients of the NQR frequency at constant volume. All the three com­ pounds show a non linear variation of the NQR frequency with pressure, the rate of which is positive and decreases with increasing pressure. In case of 3,5-dichloroanisole the value becomes negative in the higher range of pressure studied. The spin lattice relaxation time T1 in all the three compounds shows a weak dependence on pressure, indicating that the relaxation is mainly due to the torsional motions.

  6. A correlation study of quinoline derivatives and their pharmaceutical behavior by ab initio calculated NQR parameters.

    PubMed

    Rafiee, Marjan A; Hadipour, Nasser L; Naderi-manesh, Hossein

    2004-03-01

    In this paper, ab initio calculated NQR parameters for some quinoline-containing derivatives are presented. The calculations are carried out in a search for the relationships between the charge distribution of these compounds and their ability to interact with haematin. On the basis of NQR parameters, pi-electron density on the nitrogen atom of the quinoline ring plays a dominant role in determining the ability of quinolines to interact with haematin. This point was confirmed with investigation of Fe+3 cation-pi quinoline ring interactions in 2- and 4-aminoquinoline. However, our results do not show any preference for those carbon atoms of the quinoline ring which previous reports have noted. In order to calculate the NQR parameters, the electric field gradient (EFG) should be evaluated at the site of a quadrupolar nucleus in each compound. EFGs are calculated by the Gaussian 98 program using the B3LYP/6-31 G* level of theory.

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

    PubMed

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

    2013-05-01

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

  8. Conventional s-Wave Superconductivity in Noncentrosymmetric Ir2Ga9: 71Ga-NQR Evidence

    NASA Astrophysics Data System (ADS)

    Harada, Atsushi; Tamura, Nobukatsu; Mukuda, Hidekazu; Kitaoka, Yoshio; Wakui, Kouhei; Akutagawa, Satoshi; Akimitsu, Jun

    2009-02-01

    We report a $^{71}$Ga nuclear-quadrupole-resonance (NQR) study on the characteristics of superconductivity in noncentrosymmetric Ir$_2$Ga$_9$ at zero field (H=0). The $^{71}$Ga-NQR measurements have revealed that $1/T_1$ has the clear coherence peak just below $T_{\\rm c}$, and decreases exponentially upon further cooling in Ir$_2$Ga$_9$. From these results, Ir$_2$Ga$_9$ is concluded to be the conventional s-wave superconductor. Despite the lack of spatial centrosymmetry, there are no evidence for unconventional superconducting state ascribed to ASOC in Ir$_2$Ga$_9$.

  9. 73Ge-NQR study of heavy-fermion compound CeNi2Ge2

    NASA Astrophysics Data System (ADS)

    Kawasaki, S.; Sada, T.; Miyoshi, T.; Kotegawa, H.; Mukuda, H.; Kitaoka, Y.; Kobayashi, T. C.; Fukuhara, T.; Maezawa, K.; Itoh, K. M.; Haller, E. E.

    2007-03-01

    We report 73Ge-nuclear-quadrupole resonance (NQR) study of heavy-fermion compound CeNi2Ge2. The temperature dependence of the 73Ge nuclear-spin-lattice-relaxation rate 1/T1 indicates the development of magnetic correlations and the formation of a Fermi-liquid state at temperatures lower than TFL=0.4 K, where 1/T1T is constant. The 1/T1T decrease below TcNQR=0.1 K, whereas resistance decreases below Tconset=0.2 K and does not become zero. These results indicate CeNi2Ge2 closely locates to a superconducting quantum critical point.

  10. Effect of substituents on the /sup 35/Cl NQR frequencies of atoms in conditions of hyperconjugation

    SciTech Connect

    Arbuzov, B.A.; Andreeva, A.I.; Bredikhin, A.A.; Safin, I.A.; Vereshchagin, A.N.

    1985-12-10

    The authors studied the mechanisms of the change in the NOR spectra in a series of alpha-chloro-substituted dialkyl ethers, organonitrogen compounds, and benzyl and benzylidene chlorides. The NQR spectra were made on a pulsed IS-3 spectrometer at a temperature of 77 degrees K. There are n-o and ..pi..-o interactions which decrease the Cl 35 and Br 79 NQR frequencies in the series of alpha-chloro ethers, alpha-chloroalkylamides, and benzyl halides. The introduction of a geminal halogen atom (dichloromethyl ethers, benzylidene halides) decreases the effect of hyperconjugation.

  11. Electronic effects in alkyl 4-chlorophenyl sulfone and sulfoxide molecules according to Cl 35 NQR data

    SciTech Connect

    Feshin, V.P.; Voronkov, M.G.; Dolgushin, G.V.; Romanenko, L.S.; Aliev, I.A.; Mirzoeva, M.A.

    1986-11-20

    Compounds of the 4-ClC/sub 6/H/sub 4/S(O)CH/sub n/ x (CH/sub 3/)/sub 3-n/ and 4-ClC/sub 6/H/sub 4/SO/sub 2/R series (R = (CH/sub 2/)/sub n/H and CH/sub n/(CH/sub 3/)/sub 3-n/) were synthesized and studied by the /sup 35/Cl NQR method. It was found that their NQR frequencies change regularly with increase in the number n.

  12. Repetitive experiments of one or two-pulse sequences in NQR of spins I=3/2: Liouville space, steady-state, Ernst angle and optimum signal.

    PubMed

    Odin, Christophe

    2017-09-01

    In NMR, the repetition of pulse sequences with a recycle time that does not allow the spin system to completely relax back to equilibrium is a well known and often used method to increase the signal to noise ratio at given total measuring time. For isolated spins I=1/2, the steady-state of a train of strictly identical pulse sequences separated by free evolution periods of same duration is described by the well known Ernst-Anderson model, and the optimum pulse angle is given by the Ernst angle. We showed recently that equivalent formula, but with super-operators in the Liouville space, can be obtained for general spins I. In this article, this formalism is generalized to pure NQR of spins I=3/2, and applied to calculate the signal resulting from single and solid-echo sequences, in the limit when the recycle time T>5T2q, where T2q is the transverse (coherence) quadrupolar relaxation time. In particular, we show that powder samples have a behaviour that is very close to NMR of spins I=1/2. For instance, the generalized Ernst angle βM that maximizes the signal amplitude for a single pulse train is well described by the simple formula cos(1.52βM)≈exp(-T/T1q), whatever the quadrupolar asymmetry parameter η, T1q being the longitudinal (population) quadrupolar relaxation time. Moreover, a simplified NMR-like formula that describes the overall behaviour of nutation curves is proposed, and it is shown that the signal to noise ratio (SNR) at given experimental time is exactly the same as in NMR of spins I=1/2 as a function of recycle time, when properly normalized. Some theoretical predictions for the single pulse and solid-echo sequence were compared to experiments, and validated, by performing (35)Cl pure NQR experiment on chloranil (C6Cl4O2 tetrachloro-1,4-benzoquinone) powder. Copyright © 2017 Elsevier Inc. All rights reserved.

  13. NQR Study of the Heavy-Fermion Pu-115 Superconductors

    NASA Astrophysics Data System (ADS)

    Koutroulakis, G.; Yasuoka, H.; Tobash, P. H.; Mitchell, J. N.; Bauer, E. D.; Thompson, J. D.

    2014-03-01

    We present 115In nuclear quadrupolar resonance (NQR) measurements on the heavy-fermion superconductors Pu MIn5 (M=Co, Rh; Tc=2.5K, 1.6K, respectively), in the temperature range 0 . 29 K <= T <= 100 K . From the identified spectral lines, we deduce the quadrupolar parameters for the two inequivalent In sites, which are found to be qualitatively similar to those for other Ce- and Pu-115s. The quadrupolar frequency νQ varies with temperature in the normal state as per the empirical formula for conventional metals. As superconductivity develops, however, νQ exhibits a sharp, albeit small shift, which is a key prediction of the theory of composite superconducting (SC) pairing. The temperature variation of the nuclear spin-lattice relaxation rate T1- 1 delineates distinctive regimes of dynamic behavior. An excess of strong in-plane antiferromagnetic spin fluctuations is observed in the vicinity of Tc, which are believed to be playing a central role in the formation of the SC condensate. Analysis of the T1- 1 data in the SC state suggests that these compounds are strong-coupling d-wave superconductors.

  14. Spin 3/2 Zeeman perturbed NQR in the presence of slow sample rotation.

    PubMed

    Panguluri, R P; Suits, B H

    2006-09-01

    Theoretical and experimental results are presented for the case of Zeeman perturbed nuclear quadrupole resonance (NQR) using spin-3/2 nuclei with a small Zeeman interaction, gammaB0, while the sample is very slowly rotated. It is found that the decay envelope for a simple two-pulse echo measurement can be strongly affected even though the sample may rotate only a few degrees or less during the course of the measurement. To lowest order the decay envelope can be described using a one dimensional function of the product of gammaB0, the rotation rate, and the square of the pulse spacing. Aside from an indirect and weak dependence on the quadrupole asymmetry parameter, eta, the result is independent of the NQR frequency. Identical results are expected for a stationary sample in a small rotating magnetic field. The effect seen here may be used to advantage to measure rotational motion, for example of particles in fluids, or may be an additional complication for some Zeeman perturbed NQR measurements, including some NQR detection and imaging methods.

  15. 35Cl NQR and Crystal Structure Studies of Salts of Chlorodifluoro- and Dichloroacetic Acid

    NASA Astrophysics Data System (ADS)

    Basaran, Reha; Dou, Shi-qi; Weiss, Alarich

    1992-02-01

    The 35Cl NQR spectra of several chlorodifluoroacetates were studied as a function of temperature, including the acid ClF2CCOOH. The cations were: Ammonium, guanidinium, paramethylanilinium. Also some acid salts M⊕ClF2CCOO⊖ • n - ClF2CCOOH ( n > l ) were studied by 35Cl NQR. The bleaching temperatures of the NQR signals were determined. In the para-methylanilinium salt and in the guanidinium salt a phase transition has been observed. The crystal structure of guanidinium chlorodifluoroacetate has been determined at room temperature (a = 1089 pm, 6 = 845 pm, c = 832 pm, space group Pnma, Z = 4). For comparison, guanidinium dichloroacetate was studied by 35Cl NQR and by X-ray diffraction, too: P21/c, Z = 4 , a = 804pm, b = 1202 pm, c = 1080 pm, ß = 131.58°. For guanidinium chlorodifluoroacetate and chlorodifluoroacetic acid, the 35Cl spin lattice relaxation time T1 and the line width have been followed up as a function of temperature. Therefrom, the activation energies of the reorientation motion of the group -CF2C1 have been determined to be 14 kJ • mol-1 (from T1) and 12.5 kJ • mol- 1 (from Δv) for the pure acid and 9.2 kJ • mol-1 and 8.8 kJ • mol-1 , respectively, for the guanidinium salt.

  16. /sup 35/Cl NQR spectra of osmium and iridium chlorochalcogen complexes

    SciTech Connect

    Fokin, Z.A.; Bryukhova, E.V.; Pekhn'o, V.I.; Kuznetsov, S.I.

    1986-12-20

    A study was carried out on the NQR spectra of the chlorine atoms in Os(IV) and Ir(III) complexes with sulfur, selenium, and tellurium chlorides as ligands. The ECl/sub 3/ group coordinates as the ligand in the osmium compounds studied.

  17. Energy efficiency increase of NQR spectrometer transmitter at pulse resonance excitation with noise signals.

    PubMed

    Samila, A; Khandozhko, V; Politansky, L

    2017-06-08

    The specific feature of NQR is expansion of spectral lines which is caused not only by dipole-dipole interaction of nuclei, but also by local field nonuniformity caused by the defects and deformation in crystal matrix. Considerable line expansion, which is typical of crystals, requires in pulsed NQR method the optimization of pulse shape and the reserve of transmitter power output. Parametric computer identification was used to study a dependence of parameters of the energy spectra of the output signal of pulsed NQR spectrometer transmitter on the duration of excitation pulses with sine and noise occupation. The energy efficiency of a linear amplifier was calculated and experimental investigations of its temperature conditions were carried out. The energy-efficient broadband transmitter was proposed that can be used in portable setups for the pursuance of research in the field of pulsed NQR spectroscopy, for instance when studying isotopes with quadrupole moments (14)N, (35)Cl, (63)Cu, (69)Ga, (71)Ga, (113)In, (115)In and others. Copyright © 2017 Elsevier Inc. All rights reserved.

  18. Measurement of the spin-lattice relaxation time in the NQR of light nuclei

    SciTech Connect

    Anferov, V.P.; Anferova, S.V.; Grechishkin, V.S.; Sinyavskii, N.Ya.

    1988-01-01

    This work proposed a method for increasing the signal/noise ratio in NQR by preliminary magnetization of the sample in a constant magnetic field B/sub 0/ and it subsequent adiabatic demagnetization. The proposed method for the measurement of spin-lattice relaxation times is verified experimentally with a number of compounds. The results agree well with published data.

  19. 35Cl NQR spectra of certain chlorine-containing chromium compounds

    NASA Astrophysics Data System (ADS)

    Kuznetsov, S. I.; Bryukhova, E. V.; Semin, G. K.

    2015-03-01

    The coordination of chlorobenzene to Cr(CO)3 and ClC6H5Cr+ fragments is shown to result in a considerable rise in the NQR frequency of chlorine atoms. The field constant in (chlorobenzene)chromium tricarbonyl was found to grow markedly, relative to pure chlorobenzene.

  20. Cu-NQR study for stripe ordering in La-based cuprate

    NASA Astrophysics Data System (ADS)

    Matsumura, M.; Sawa, T.; Tamura, T.; Yamamoto, N.; Sera, M.; Yamagata, H.

    2003-05-01

    Cu-NQR spectra were measured in La 2- x- yM ySr xCuO 4, (M=Nd, Gd, Eu, Pr and Y), and La 2- xBa xCuO 4 with x= {1}/{8}. The low temperature tetragonal (LTT) structure is stabilized below Td2 in all the samples other than M=Pr. The usual NQR spectra observed in T> Td2 in all the samples change to abnormally broad ones after a complete wipeout of NQR signal below Td2 except for the cases of M=Nd, Gd and Pr. In the cases of M=Nd and Gd, the complete wipeout continues to 1.5 K probably due to the extrinsic nuclear relaxation path through the paramagnetic fluctuation of Nd and Gd moment. In the case of M=Pr with no LTT phase, usual NQR spectrum continues to 1.5 K. These results support a pinning model for the static stripe ordering in the LTT phase.

  1. Chlorine Substituted Acetic Acids and Salts. Effect of Salification on Chlorine-35 NQR

    NASA Astrophysics Data System (ADS)

    David, Serge; Gourdji, Michel; Guibé, Lucien; Péneau, Alain

    1996-06-01

    The NQR of a quadrupolar probe nucleus is often used to investigate the effect of substituent in molecules. The inductive effect, based on a partial charge migration along the molecular skeleton is the only one present in saturated aliphatics, the conjugative effect appearing in conjugated molecules, especially aromatics. As the stepwise charge migration mechanism, formerly used to explain the inductive effect, is now believed obsolete, we have wanted to reexamined the case of chlorine substituted acetic acids and salts. The data in literature was extended by observing reso-nances and determining NQR frequencies in several acids and salts. The present analysis of the salification of mono-, di-and tri-chloroacetic acids, which is equivalent to a deprotonation or the substitution of the acid hydrogen by a negative unit charge, shows that a model based on the polarization of the chlorine atom(s) by the carboxyle group is consistent with experimental results: the polarization energy appears to be proportional to the NQR frequency shifts; experimental data show a correlation between the NQR frequency shifts accompanying salification and the variations of the intrinsic acidity measured in the gas phase; this, in turn shows that there is a proportionality between the polarization energy and the variations in the acid free enthalpy of dissociation. From the comparison between fluorine, chlorine, bromine and iodine, it also appears that an alternative mechanism, the polarization of the carboxyl group by the halogen, would be important only in the case of the fluoroacetic acid.

  2. Zeeman shift--a tool for assignment of 14N NQR lines of nonequivalent 14N atoms in powder samples.

    PubMed

    Luznik, J; Jazbinsek, V; Pirnat, J; Seliger, J; Trontelj, Z

    2011-09-01

    The use of Zeeman perturbed 14N nuclear quadrupole resonance (NQR) to determine the ν+ and ν-14N lines in polycrystalline samples with several nonequivalent nitrogen atoms was investigated. The 14N NQR line shift due to a weak external Zeeman magnetic field was calculated, assuming isotropic distribution of EFG tensor directions. We calculated the broad line distribution of the ν+ and ν- line shifts and experimentally confirmed the calculated Zeeman field dependence of singularities (NQR peaks) in cyclotrimethylenetrinitramine (RDX) and aminotetrazole monohydrate (ATMH). The calculated and measured frequency shifts agreed well. The proposed measurement method enabled determination of which 14N NQR lines in ATMH belong to ν+ and which to ν- transitions. Copyright © 2011 Elsevier Inc. All rights reserved.

  3. 14N NQR study of polymorphism and hydrogen bonding in molecular complex isonicotinamide-oxalic acid (2:1).

    PubMed

    Seliger, J; Žagar, V

    2010-11-18

    The complete (14)N nuclear quadrupole resonance (NQR) spectra have been measured in the two polymorphic crystalline phases of the molecular complex isonicotinamide-oxalic acid (2:1) by nuclear quadrupole double resonance. The observed NQR frequencies, quadrupole coupling constants, and asymmetry parameters (η) have been assigned to the two nitrogen positions (ring and amide) in a molecule on the basis of the intensity and multiplicity of the double resonance signals. The NQR data for the ring nitrogen in both polymorphic phases deviate from the correlation relations observed in substituted pyridines. This deviation is analyzed in a model, where it is assumed that an additional electric charge on the nitrogen atom changes the NQR parameters. The model suggests that this additional electric charge is negative so that the N···H-O hydrogen bond seem to be partially ionic, of the type N(-)···H-O.

  4. The Conformational Changes Induced by Ubiquinone Binding in the Na+-pumping NADH:Ubiquinone Oxidoreductase (Na+-NQR) Are Kinetically Controlled by Conserved Glycines 140 and 141 of the NqrB Subunit*

    PubMed Central

    Strickland, Madeleine; Juárez, Oscar; Neehaul, Yashvin; Cook, Darcie A.; Barquera, Blanca; Hellwig, Petra

    2014-01-01

    Na+-pumping NADH:ubiquinone oxidoreductase (Na+-NQR) is responsible for maintaining a sodium gradient across the inner bacterial membrane. This respiratory enzyme, which couples sodium pumping to the electron transfer between NADH and ubiquinone, is not present in eukaryotes and as such could be a target for antibiotics. In this paper it is shown that the site of ubiquinone reduction is conformationally coupled to the NqrB subunit, which also hosts the final cofactor in the electron transport chain, riboflavin. Previous work showed that mutations in conserved NqrB glycine residues 140 and 141 affect ubiquinone reduction and the proper functioning of the sodium pump. Surprisingly, these mutants did not affect the dissociation constant of ubiquinone or its analog HQNO (2-n-heptyl-4-hydroxyquinoline N-oxide) from Na+-NQR, which indicates that these residues do not participate directly in the ubiquinone binding site but probably control its accessibility. Indeed, redox-induced difference spectroscopy showed that these mutations prevented the conformational change involved in ubiquinone binding but did not modify the signals corresponding to bound ubiquinone. Moreover, data are presented that demonstrate the NqrA subunit is able to bind ubiquinone but with a low non-catalytically relevant affinity. It is also suggested that Na+-NQR contains a single catalytic ubiquinone binding site and a second site that can bind ubiquinone but is not active. PMID:25006248

  5. The conformational changes induced by ubiquinone binding in the Na+-pumping NADH:ubiquinone oxidoreductase (Na+-NQR) are kinetically controlled by conserved glycines 140 and 141 of the NqrB subunit.

    PubMed

    Strickland, Madeleine; Juárez, Oscar; Neehaul, Yashvin; Cook, Darcie A; Barquera, Blanca; Hellwig, Petra

    2014-08-22

    Na(+)-pumping NADH:ubiquinone oxidoreductase (Na(+)-NQR) is responsible for maintaining a sodium gradient across the inner bacterial membrane. This respiratory enzyme, which couples sodium pumping to the electron transfer between NADH and ubiquinone, is not present in eukaryotes and as such could be a target for antibiotics. In this paper it is shown that the site of ubiquinone reduction is conformationally coupled to the NqrB subunit, which also hosts the final cofactor in the electron transport chain, riboflavin. Previous work showed that mutations in conserved NqrB glycine residues 140 and 141 affect ubiquinone reduction and the proper functioning of the sodium pump. Surprisingly, these mutants did not affect the dissociation constant of ubiquinone or its analog HQNO (2-n-heptyl-4-hydroxyquinoline N-oxide) from Na(+)-NQR, which indicates that these residues do not participate directly in the ubiquinone binding site but probably control its accessibility. Indeed, redox-induced difference spectroscopy showed that these mutations prevented the conformational change involved in ubiquinone binding but did not modify the signals corresponding to bound ubiquinone. Moreover, data are presented that demonstrate the NqrA subunit is able to bind ubiquinone but with a low non-catalytically relevant affinity. It is also suggested that Na(+)-NQR contains a single catalytic ubiquinone binding site and a second site that can bind ubiquinone but is not active. © 2014 by The American Society for Biochemistry and Molecular Biology, Inc.

  6. Riboflavin is an active redox cofactor in the Na+-pumping NADH: quinone oxidoreductase (Na+-NQR) from Vibrio cholerae.

    PubMed

    Juárez, Oscar; Nilges, Mark J; Gillespie, Portia; Cotton, Jennifer; Barquera, Blanca

    2008-11-28

    Here we present new evidence that riboflavin is present as one of four flavins in Na+-NQR. In particular, we present conclusive evidence that the source of the neutral radical is not one of the FMNs and that riboflavin is the center that gives rise to the neutral flavosemiquinone. The riboflavin is a bona fide redox cofactor and is likely to be the last redox carrier of the enzyme, from which electrons are donated to quinone. We have constructed a double mutant that lacks both covalently bound FMN cofactors (NqrB-T236Y/NqrC-T225Y) and have studied this mutant together with the two single mutants (NqrB-T236Y and NqrC-T225Y) and a mutant that lacks the noncovalently bound FAD in NqrF (NqrF-S246A). The double mutant contains riboflavin and FAD in a 0.6:1 ratio, as the only flavins in the enzyme; noncovalently bound flavins were detected. In the oxidized form, the double mutant exhibits an EPR signal consistent with a neutral flavosemiquinone radical, which is abolished on reduction of the enzyme. The same radical can be observed in the FAD deletion mutant. Furthermore, when the oxidized enzyme reacts with ubiquinol (the reduced form of the usual electron acceptor) in a process that reverses the physiological direction of the electron flow, a single kinetic phase is observed. The kinetic difference spectrum of this process is consistent with one-electron reduction of a neutral flavosemiquinone. The presence of riboflavin in the role of a redox cofactor is thus far unique to Na+-NQR.

  7. Growth and NMR evaluation of a single crystal CePd2Ga

    NASA Astrophysics Data System (ADS)

    Kishimoto, Yasuki; Kotegawa, Hisashi; Matsuoka, Eiichi; Sugawara, Hitoshi; Tou, Hideki

    2017-04-01

    We have measured the electrical resistivity and the powder x-ray diffraction (XRD) for ascast, 700 °C, and 800 °C annealed samples of the Ce-based antiferromagnetic compound CePd2Ga. From the XRD measurement, the unit-cell volume of 700 °C and 800 °C annealed sample is smaller by 0.52% and 0.87% than ascast sample. In order to check microscopically, we are carried out Ga-Nuclear Magnetic Resonance (NMR) and Nuclear Quadrupole Resonance (NQR).

  8. N-14 NQR using a high-Tc rf SQUID with a normal metal transformer

    NASA Astrophysics Data System (ADS)

    He, D. F.; Tachiki, M.; Itozaki, H.

    2008-01-01

    We have improved our high-Tc SQUID-based N-14 nuclear quadrupole resonance (NQR) detection system. By using a reed relay SIL5-1A72-71L (MEDER electronic) in the normal metal transformer, the isolation to the excitation field was much improved. The high-Tc rf SQUID could operate stably when the rf excitation field was over 20 mT. By optimizing the input coil of the transformer, better sensitivity of 0.5 fT Hz-1/2 was obtained at the resonant frequency of the tuned normal metal transformer. A spin-locking spin-echo (SLSE) multi-pulse sequence was also used in the system to detect the weak NQR signals produced by samples with longer spin-spin relaxation time T2, such as trinitrotoluene (TNT).

  9. Measurement of temperature and temperature gradient in millimeter samples by chlorine NQR

    NASA Astrophysics Data System (ADS)

    Lužnik, Janko; Pirnat, Janez; Trontelj, Zvonko

    2009-09-01

    A mini-thermometer based on the 35Cl nuclear quadrupole resonance (NQR) frequency temperature dependence in the chlorates KClO3 and NaClO3 was built and successfully tested by measuring temperature and temperature gradient at 77 K and higher in about 100 mm3 active volume of a mini Joule-Thomson refrigerator. In the design of the tank-circuit coil, an array of small coils connected in series enabled us (a) to achieve a suitable ratio of inductance to capacity in the NQR spectrometer input tank circuit, (b) to use a single crystal of KClO3 or NaClO3 (of 1-2 mm3 size) in one coil as a mini-thermometer with a resolution of 0.03 K and (c) to construct a system for measuring temperature gradients when the spatial coordinates of each chlorate single crystal within an individual coil are known.

  10. Pressure and temperature dependence of the chlorine NQR in caesium and sodium chlorates.

    PubMed

    Ramesh, K P; Suresh, K S; Raghavendra Rao, C; Ramakrishna, J

    2008-06-01

    The (35)Cl nuclear quadrupole resonance (NQR) frequencies (nu(Q)) in caesium and sodium chlorates were measured as a function of temperature, from 77 to 300 K at different pressures up to 5.1 kbar, and the data were analysed to estimate the volume dependence of the electric field gradient (EFG), torsional frequency and also the contributions to the NQR frequency from static and dynamic effects. The variation of spin-lattice relaxation time with pressure at different temperatures was studied in the case of sodium chlorate and at room temperature in case of caesium chlorate. The pressure dependence of the spin-lattice relaxation time (T(1)) suggests that the relaxation is mainly due to the torsional motions.

  11. /sup 127/I NQR spectra of some iodine derivatives of dialkyl ethers

    SciTech Connect

    Feshin, V.P.; Voronkov, M.G.; Romanenko, L.S.; Nikitin, P.A.; Dubinskaya, E.I.; Komarov, V.G.

    1987-12-10

    The authors studied the mutual influence of oxygen and iodine atoms in molecules of iodine-substituted dialkyl ethers in its dependence on the number of carbon atoms separating these atoms. For this the authors determined the /sup 127/I NQR spectra (1/2-3/2 transition) of compounds of this type at 77 K. They /sup 127/I NQR spectra (1/2-3/2 transition) of compounds containing the I-C-OR grouping show that in these molecules the OR group is an electron donor. The electron-donor power of the methoxy group is appreciably higher in ICH/sub 2/OCH/sub 3/ than in ClCH/sub 2/OCH/sub 3/.

  12. 75As-NQR study of the hybridization gap semiconductor CeOs4As12

    NASA Astrophysics Data System (ADS)

    Yogi, M.; Higa, N.; Niki, H.; Kawata, T.; Sekine, C.

    2016-02-01

    We performed an 75As nuclear quadrupole resonance (NQR) measurement on CeOs4As12. The 75As-NQR spectrum shape demonstrates that the Ce-site filling fraction of our high-pressure synthesized sample is close to unity. A presence of the c — f hybridization gap is confirmed from the temperature dependence of the nuclear spin-lattice relaxation rate 1/T1. An increase of 1/T1 below ∼3 K indicates a development of the spin fluctuations. The 1/T1 for CeOs4As12 shows similar behavior as that for CeOs4Sb12 with different magnitude of the c — f hybridization gap. An absence of phase transition in CeOs4As12 may be caused by the increase of the c — f hybridization, which increases the gap magnitude and reduces the residual density of state inside the gap.

  13. Cross-polarisation method for improvement of 14N NQR signal detectability.

    PubMed

    Rudakov, T N; Hayes, P A

    2006-11-01

    This is a study of the cross-polarization effects in the case of 14N quadrupolar spin-system with a long spin-lattice relaxation time. Two important benefits of the cross-polarization technique were demonstrated for PETN: (i) a polarization transfer resulting in increased NQR single shot signal response and (ii) a dynamic reduction in recovery time of the NQR system allowing scan repetition on a much shorter timescale. It was proved that this technique can reduce the optimal waiting time between pulse sequences up to 60 times through a significant reduction of the relaxation time of the quadrupolar spin-system. All experiments were carried out at room temperature using spin-locking multi-pulse sequences and small external magnetic field.

  14. Mapping molecular orientation in solids by rotating-frame NQR techniques

    PubMed

    Casanova; Robert; Pusiol

    1998-07-01

    A multi-dimensional NQR technique to image both the spatial distribution of quadrupolar nuclei and the local orientation of the electric field gradient tensor at the quadrupole sites in solids is reported. The encoding procedure is based on the irradiation of the sample by a pulse sequence composed of spatially homogeneous and inhomogeneous radiofrequency fields. A method that encodes the spatial and orientation information in the amplitudes of the free-induction decay signals and a proper three-dimensional reconstruction procedure that yields the space-orientation-dependent NQR spectra are described. A two-dimensional variant allows rapid measurement of the spatially dependent orientation distribution of molecules, disregarding the spectroscopic information. Copyright 1998 Academic Press.

  15. Singularties of the shape of the nonresonance nutation spectra of NQR powders

    SciTech Connect

    Sinyavskii, N.Ya.; Shelukhina, S.F.

    1995-12-01

    The singularities of nutation NQR spectra for nuclei with spin J = 1, 3/2 in the absence of resonance are considered for powders. It is shown that when determining the asymmetry parameter {eta} from the frequency characteristics of the nutation spectrum one must take into account the frequency shift of the spectrometer relative to exact resonance. Structural studies of single crystals by mutation spectroscopy are demonstrated to be feasible.

  16. Mutual effect of ligands in nitrido and nitroso complexes of osmium and ruthenium from NQR data

    SciTech Connect

    Kravchenko. E.A.; Burtsev, M.Yu.; Sinitsyn, M.N.; Svetlov, A.A.; Kokunov, Ya.V.; Buslaev, A.

    1987-11-01

    The purpose of this investigation was to study by NQR the spectral results of the mutual ligand effect in complex compounds having various types of short bonds. The authors obtained the /sup 35/Cl, /sup 81/Br, and /sup 127/I NQR spectra of a large number of halogen complexes of osmium and ruthenium having short Os=N and M in equilibrium NO bonds of the following types: R(OsNHal/sub 4/) (R = (Ph/sub 4/P)/sup +/, (Bu/sub 4/N)/sup +/; Hal = Cl/sup -/, Br/sup -/, I/sup -/), K/sub 2/(OsNCl/sub 5/), Rb/sub 2/(OsNBr/sub 5/), (NH/sub 4/)/sub 2/(OsNBr/sub 5/), K(OsNHal/sub 4/L) (Hal = Cl/sup -/, Br/sup -/; L = H/sub 2/O, CH/sub 3/CN), K/sub 2/(MNOHal/sub 5/) (M = Os, Ru; Hal = Cl/sup -/, Br/sup -/, I/sup -/). The experimental NQR values measured are connected by the Townes and Dailey theory with the chemical bond characteristics i, sigma, ..pi.., the degree of the ionic, the sigma-covalent, and the ..pi..-covalent natures respectively ( i + sigma + ..pi.. = 1).

  17. Strong pH dependence of coupling efficiency of the Na+ - translocating NADH:quinone oxidoreductase (Na+-NQR) of Vibrio cholerae.

    PubMed

    Toulouse, Charlotte; Claussen, Björn; Muras, Valentin; Fritz, Günter; Steuber, Julia

    2017-02-01

    The Na+-translocating NADH:quinone oxidoreductase (NQR) is the entry site for electrons into the respiratory chain of Vibrio cholerae, the causative agent of cholera disease. NQR couples the electron transfer from NADH to ubiquinone to the translocation of sodium ions across the membrane. We investigated the pH dependence of electron transfer and generation of a transmembrane voltage (ΔΨ) by NQR reconstituted in liposomes with Na+ or Li+ as coupling cation. ΔΨ formation was followed with the voltage-sensitive dye oxonol. With Na+, ΔΨ was barely influenced by pH (6.5-8.5), while Q reduction activity exhibited a maximum at pH 7.5-8.0. With Li+, ΔΨ was generally lower, and the pH profile of electron transfer activity did not reveal a pronounced maximum. We conclude that the coupling efficiency of NQR is influenced by the nature of the transported cation, and by the concentration of protons. The 3D structure of NQR reveals a transmembrane channel in subunit NqrB. It is proposed that partial uncoupling of the NQR observed with the smaller Li+, or with Na+ at pH 7.5-8.0, is caused by the backflow of the coupling cation through the channel in NqrB.

  18. Acid residues in the transmembrane helices of the Na+-pumping NADH:quinone oxidoreductase (Na+-NQR) from Vibrio cholerae involved in sodium translocation†

    PubMed Central

    Juárez, Oscar; Athearn, Kathleen; Gillespie, Portia; Barquera, Blanca

    2009-01-01

    Vibrio cholerae and many other marine and pathogenic bacteria posses a unique respiratory complex, the Na+-pumping NADH: quinone oxidoreductase (Na+-NQR)1, which pumps Na+ across the cell membrane using the energy released by the redox reaction between NADH and ubiquinone. In order to function as a selective sodium pump, Na+-NQR must contain structures that: 1) allow the sodium ion to pass through the hydrophobic core of the membrane, and 2) provide cation specificity to the translocation system. In other sodium transporting proteins, the structures that carry out these roles frequently include aspartate and glutamate residues. The negative charge of these residues facilitates binding and translocation of sodium. In this study we have analyzed mutants of acid residues located in the transmembrane helices of subunits B, D and E of Na+-NQR. The results are consistent with the participation of seven of these residues in the translocation process of sodium. Mutations at NqrB-D397, NqrD-D133 and NqrE-E95 produced a decrease of approximately ten times or more in the apparent affinity of the enzyme for sodium (Kmapp), which suggests that these residues may form part of a sodium-binding site. Mutation at other residues, including NqrB-E28, NqrB-E144, NqrB-E346 and NqrD-D88, had a large effect on the quinone reductase activity of the enzyme and its sodium sensitivity, but less effect on the apparent sodium affinity, consistent with a possible role in sodium conductance pathways. PMID:19694431

  19. Effect of the oxygen protonation on the electronic structure of urea in the solid state: A 14N NQR study

    NASA Astrophysics Data System (ADS)

    Murgich, Juan; Santana R., Magaly

    1981-04-01

    The 14N NQR frequencies of urea complexes with H2O2 (1:1), NH4Cl (1:1), oxalic (2:1), phosphoric (1:1), and nitric acid (1:1) at 77 °K are reported. The analysis of the NQR data indicates that the population of the N nonbonding orbital decreases and that the population of the s N-H and N-C bonds increases as the degree of protonation of the O atom of urea increases. These changes are consistent with a larger weight of structures like C = N+H2 as the protonation increases. The NQR results are in agreement with those obtained from a CNDO/2 calculation for the uronioum ion [Yu. A. Panteleev and A. A. Lipovskii, Zhu. Struk. Khim. 17, 2 (1976)].

  20. Possibility of Valence-Fluctuatsion-Mediated Superconductivity in Cd-Doped CeIrIn5 Probed by In NQR

    NASA Astrophysics Data System (ADS)

    Yashima, M.; Tagami, N.; Taniguchi, S.; Unemori, T.; Uematsu, K.; Mukuda, H.; Kitaoka, Y.; Ōta, Y.; Honda, F.; Settai, R.; Ōnuki, Y.

    2012-09-01

    We report on a pressure-induced evolution of exotic superconductivity and spin correlations in CeIr(In1-xCdx)5 by means of in-nuclear-quadrupole-resonance (NQR) studies. Measurements of an NQR spectrum and nuclear-spin-lattice-relaxation rate 1/T1 have revealed that antiferromagnetism induced by Cd doping emerges locally around Cd dopants, but superconductivity is suddenly induced at Tc=0.7 and 0.9 K at 2.34 and 2.75 GPa, respectively. The unique superconducting characteristics with a large fraction of the residual density of state at the Fermi level which increases with Tc differ from those for anisotropic superconductivity mediated by antiferromagnetic correlations. By incorporating the pressure dependence of the NQR frequency pointing to the valence change of Ce, we suggest that unconventional superconductivity in the CeIr(In1-xCdx)5 system may be mediated by valence fluctuations.

  1. The sodium pumping NADH:quinone oxidoreductase (Na⁺-NQR), a unique redox-driven ion pump.

    PubMed

    Barquera, Blanca

    2014-08-01

    The Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR) is a unique Na(+) pumping respiratory complex found only in prokaryotes, that plays a key role in the metabolism of marine and pathogenic bacteria, including Vibrio cholerae and other human pathogens. Na(+)-NQR is the main entrance for reducing equivalents into the respiratory chain of these bacteria, catalyzing the oxidation of NADH and the reduction of quinone, the free energy of this redox reaction drives the selective translocation of Na(+) across the cell membrane, which energizes key cellular processes. In this review we summarize the unique properties of Na(+)-NQR in terms of its redox cofactor composition, electron transfer reactions and a possible mechanism of coupling and pumping.

  2. Weakly coordinating anions: crystallographic and NQR studies of halogen-metal bonding in silver, thallium, sodium, and potassium halomethanesulfonates.

    PubMed

    Wulfsberg, Gary; Parks, Katherine D; Rutherford, Richard; Jackson, Debra Jones; Jones, Frank E; Derrick, Dana; Ilsley, William; Strauss, Steven H; Miller, Susie M; Anderson, Oren P; Babushkina, T A; Gushchin, S I; Kravchenko, E A; Morgunov, V G

    2002-04-22

    35Cl, (79,81)Br, and (127)I NQR (nuclear quadrupole resonance) spectroscopy in conjunction with X-ray crystallography is potentially one of the best ways of characterizing secondary bonding of metal cations such as Ag(+) to halogen donor atoms on the surfaces of very weakly coordinating anions. We have determined the X-ray crystal structure of Ag(O(3)SCH(2)Cl) (a = 13.241(3) A; b = 7.544(2) A; c = 4.925(2) A; orthorhombic; space group Pnma; Z = 4) and compared it with the known structure of Ag(O(3)SCH(2)Br) (Charbonnier, F.; Faure, R.; Loiseleur, H. Acta Crystallogr., Sect. B 1978, 34, 3598-3601). The halogen atom in each is apical (three-coordinate), being weakly coordinated to two silver ions. (127)I NQR studies on Ag(O(3)SCH(2)I) show the expected NQR consequences of three-coordination of iodine: substantially reduced NQR frequencies nu(1) and nu(2) and a fairly small NQR asymmetry parameter eta. The reduction of the halogen NQR frequency of the coordinating halogen atom in Ag(O(3)SCH(2)X) becomes more substantial in the series X = Cl < Br < I, indicating that the coordination to Ag(+) strengthens in this series, as expected from hard-soft acid-base principles. The numbers of electrons donated by the organic iodine atom to Ag(+) have been estimated; these indicate that the bonding to the cation is weak but not insignificant. We have not found any evidence for the bonding of these organohalogen atoms to another soft-acid metal ion, thallium. A scheme for recycling of thallium halide wastes is included.

  3. The weakly coordinating trichloromethanesulfonate anion: NQR comparison of its coordinating abilities via oxygen with those of the chloroacetate ions.

    PubMed

    Wulfsberg, Gary; Cochran, Michael; Wilcox, Jamie; Koritsanszky, Tibor; Jackson, Debra Jones; Howard, James C

    2004-03-22

    Ionic and covalent derivatives of the chlorine analogue of the nonbasic, weakly coordinating triflate ion, Cl3CSO3(-) or "trichlate" ion, have been prepared and compared with the corresponding more strongly coordinated chloroacetates, Cl(x)CH(3-x)CO(2)M (x = 1-3), using 35Cl NQR (nuclear quadrupole resonance) spectroscopy. The (35)Cl NQR frequencies of all types of derivatives are sensitive to the nature of the metal ion or Lewis acid and are most sensitive in the case of monochloroacetates. In covalent (including zirconocene) derivatives, the average NQR frequencies fall as the Pauling electronegativity of M falls. The results for ionic derivatives contrast with previous results for ionic hexachlorometalates: the average (35)Cl NQR frequencies drop sharply as the ionic radius of the group 1 cation increases. Ab initio Gaussian 98 computations at the B3LYP/6-311++G(3df,3pd) level on isolated XCH2CO2M (M = Li, Na, K; X = F, Cl) molecules duplicate this trend, showing increasing polarization of the C-Cl bond and smaller electric field gradients for larger group 1 ions; the relevance of this to the solid state polymerization of chloroacetates (Herzberg, O.; Epple, M. Eur. J. Inorg. Chem. 2001, 1395-1406) is discussed. We have prepared the dihydrate and monohydrate of trichlic acid, Cl3CSO3H. Although trichlates have the highest average NQR frequencies of any of these salts, the NQR frequencies of trichlic acid dihydrate are anomalously lower than those of trichloroacetic acid, which suggests that it is a strong acid, ionized in the solid state to H5O2+ and Cl3CSO3(-) ions.

  4. Pressure-induced antiferromagnetic superconductivity in CeNiGe3: A Ge73-NQR study under pressure

    NASA Astrophysics Data System (ADS)

    Harada, A.; Kawasaki, S.; Mukuda, H.; Kitaoka, Y.; Thamizhavel, A.; Okuda, Y.; Settai, R.; Ōnuki, Y.; Itoh, K. M.; Haller, E. E.; Harima, H.

    2007-03-01

    We report on antiferromagnetic (AF) properties of pressure-induced superconductivity in CeNiGe3 via the Ge73 nuclear-quadrupole-resonance (NQR) measurements under pressure ( P). The NQR-spectrum measurements have revealed that the incommensurate antiferromagnetic ordering is robust against increasing P with the increase of ordered moment and ordering temperature. Nevertheless the measurements of nuclear spin-lattice relaxation rate (1/T1) have pointed to the onset of superconductivity as a consequence of Ce-4f electrons delocalized by applying P. The emergence of superconductivity under the development of AF order suggests that a novel type of superconducting mechanism works in this compound.

  5. Adequacy of the description of /sup 35/Cl NQR spectroscopic parameters by semiempirical quantum-chemical methods

    SciTech Connect

    Romanenko, E.A.; Nesterenko, A.M.

    1986-09-01

    Correlation relations between experimental /sup 35/Cl NQR spectroscopic parameters, viz., the frequencies and the asymmetry parameters ..nu.. of the tensor of the electric-field gradient and the values calculated by semiempirical quantum-chemical methods, have been considered. The best correlations were obtained for both ..gamma.. and /eta/ when they are calculated by the INDOspd method. The MINDO/3 method is promising for the description of the absolute values of NQR frequencies. The parameters ..cap alpha.. and b of the MINDO/3 method have been evaluated for nitrogenphosphorus and nitrogen-chlorine bonds.

  6. Inhibition of the sodium-translocating NADH-ubiquinone oxidoreductase [Na+-NQR] decreases cholera toxin production in Vibrio cholerae O1 at the late exponential growth phase

    PubMed Central

    Minato, Yusuke; Fassio, Sara R.; Reddekopp, Rylan L.; Häse, Claudia C.

    2014-01-01

    Two virulence factors produced by Vibrio cholerae, cholera toxin (CT) and toxin-corregulated pilus (TCP), are indispensable for cholera infection. ToxT is the central regulatory protein involved in activation of CT and TCP expression. We previously reported that lack of a respiration-linked sodium-translocating NADH–ubiquinone oxidoreductase (Na+-NQR) significantly increases toxT transcription. In this study, we further characterized this link and found that Na+-NQR affects toxT expression only at the early-log growth phase, whereas lack of Na+-NQR decreases CT production after the mid-log growth phase. Such decreased CT production was independent of toxT and ctxB transcription. Supplementing a respiratory substrate, L-lactate, into the growth media restored CT production in the nqrA-F mutant, suggesting that decreased CT production in the Na+-NQR mutant is dependent on electron transport chain (ETC) activity. This notion was supported by the observations that two chemical inhibitors, a Na+-NQR specific inhibitor 2-n-Heptyl-4-hydroxyquinoline N-oxide (HQNO) and a succinate dehydrogenase (SDH) inhibitor, thenoyltrifluoroacetone (TTFA), strongly inhibited CT production in both classical and El Tor biotype strains of V. cholerae. Accordingly, we propose the main respiratory enzyme of V. cholerae, as a potential drug target to treat cholera because human mitochondria do not contain Na+-NQR orthologs. PMID:24361395

  7. 35Cl NQR frequency and spin lattice relaxation time in 3,4-dichlorophenol as a function of pressure and temperature.

    PubMed

    Ramu, L; Ramesh, K P; Chandramani, R

    2013-01-01

    The pressure dependences of (35)Cl nuclear quadrupole resonance (NQR) frequency, temperature and pressure variation of spin lattice relaxation time (T(1)) were investigated in 3,4-dichlorophenol. T(1) was measured in the temperature range 77-300 K. Furthermore, the NQR frequency and T(1) for these compounds were measured as a function of pressure up to 5 kbar at 300 K. The temperature dependence of the average torsional lifetimes of the molecules and the transition probabilities W(1) and W(2) for the Δm = ±1 and Δm = ±2 transitions were also obtained. A nonlinear variation of NQR frequency with pressure has been observed and the pressure coefficients were observed to be positive. A thermodynamic analysis of the data was carried out to determine the constant volume temperature coefficients of the NQR frequency. An attempt is made to compare the torsional frequencies evaluated from NQR data with those obtained by IR spectra. On selecting the appropriate mode from IR spectra, a good agreement with torsional frequency obtained from NQR data is observed. The previously mentioned approach is a good illustration of the supplementary nature of the data from IR studies, in relation to NQR studies of compounds in solid state. Copyright © 2012 John Wiley & Sons, Ltd.

  8. Inhibition of the sodium-translocating NADH-ubiquinone oxidoreductase [Na+-NQR] decreases cholera toxin production in Vibrio cholerae O1 at the late exponential growth phase.

    PubMed

    Minato, Yusuke; Fassio, Sara R; Reddekopp, Rylan L; Häse, Claudia C

    2014-01-01

    Two virulence factors produced by Vibrio cholerae, cholera toxin (CT) and toxin-corregulated pilus (TCP), are indispensable for cholera infection. ToxT is the central regulatory protein involved in activation of CT and TCP expression. We previously reported that lack of a respiration-linked sodium-translocating NADH-ubiquinone oxidoreductase (Na(+)-NQR) significantly increases toxT transcription. In this study, we further characterized this link and found that Na(+)-NQR affects toxT expression only at the early-log growth phase, whereas lack of Na(+)-NQR decreases CT production after the mid-log growth phase. Such decreased CT production was independent of toxT and ctxB transcription. Supplementing a respiratory substrate, l-lactate, into the growth media restored CT production in the nqrA-F mutant, suggesting that decreased CT production in the Na(+)-NQR mutant is dependent on electron transport chain (ETC) activity. This notion was supported by the observations that two chemical inhibitors, a Na(+)-NQR specific inhibitor 2-n-Heptyl-4-hydroxyquinoline N-oxide (HQNO) and a succinate dehydrogenase (SDH) inhibitor, thenoyltrifluoroacetone (TTFA), strongly inhibited CT production in both classical and El Tor biotype strains of V. cholerae. Accordingly, we propose the main respiratory enzyme of V. cholerae, as a potential drug target to treat cholera because human mitochondria do not contain Na(+)-NQR orthologs.

  9. Roles of the Sodium-Translocating NADH:Quinone Oxidoreductase (Na+-NQR) on Vibrio cholerae Metabolism, Motility and Osmotic Stress Resistance

    PubMed Central

    Minato, Yusuke; Halang, Petra; Quinn, Matthew J.; Faulkner, Wyatt J.; Aagesen, Alisha M.; Steuber, Julia; Stevens, Jan F.; Häse, Claudia C.

    2014-01-01

    The Na+ translocating NADH:quinone oxidoreductase (Na+-NQR) is a unique respiratory enzyme catalyzing the electron transfer from NADH to quinone coupled with the translocation of sodium ions across the membrane. Typically, Vibrio spp., including Vibrio cholerae, have this enzyme but lack the proton-pumping NADH:ubiquinone oxidoreductase (Complex I). Thus, Na+-NQR should significantly contribute to multiple aspects of V. cholerae physiology; however, no detailed characterization of this aspect has been reported so far. In this study, we broadly investigated the effects of loss of Na+-NQR on V. cholerae physiology by using Phenotype Microarray (Biolog), transcriptome and metabolomics analyses. We found that the V. cholerae ΔnqrA-F mutant showed multiple defects in metabolism detected by Phenotype Microarray. Transcriptome analysis revealed that the V. cholerae ΔnqrA-F mutant up-regulates 31 genes and down-regulates 55 genes in both early and mid-growth phases. The most up-regulated genes included the cadA and cadB genes, encoding a lysine decarboxylase and a lysine/cadaverine antiporter, respectively. Increased CadAB activity was further suggested by the metabolomics analysis. The down-regulated genes include sialic acid catabolism genes. Metabolomic analysis also suggested increased reductive pathway of TCA cycle and decreased purine metabolism in the V. cholerae ΔnqrA-F mutant. Lack of Na+-NQR did not affect any of the Na+ pumping-related phenotypes of V. cholerae suggesting that other secondary Na+ pump(s) can compensate for Na+ pumping activity of Na+-NQR. Overall, our study provides important insights into the contribution of Na+-NQR to V. cholerae physiology. PMID:24811312

  10. Roles of the sodium-translocating NADH:quinone oxidoreductase (Na+-NQR) on vibrio cholerae metabolism, motility and osmotic stress resistance.

    PubMed

    Minato, Yusuke; Fassio, Sara R; Kirkwood, Jay S; Halang, Petra; Quinn, Matthew J; Faulkner, Wyatt J; Aagesen, Alisha M; Steuber, Julia; Stevens, Jan F; Häse, Claudia C

    2014-01-01

    The Na+ translocating NADH:quinone oxidoreductase (Na+-NQR) is a unique respiratory enzyme catalyzing the electron transfer from NADH to quinone coupled with the translocation of sodium ions across the membrane. Typically, Vibrio spp., including Vibrio cholerae, have this enzyme but lack the proton-pumping NADH:ubiquinone oxidoreductase (Complex I). Thus, Na+-NQR should significantly contribute to multiple aspects of V. cholerae physiology; however, no detailed characterization of this aspect has been reported so far. In this study, we broadly investigated the effects of loss of Na+-NQR on V. cholerae physiology by using Phenotype Microarray (Biolog), transcriptome and metabolomics analyses. We found that the V. cholerae ΔnqrA-F mutant showed multiple defects in metabolism detected by Phenotype Microarray. Transcriptome analysis revealed that the V. cholerae ΔnqrA-F mutant up-regulates 31 genes and down-regulates 55 genes in both early and mid-growth phases. The most up-regulated genes included the cadA and cadB genes, encoding a lysine decarboxylase and a lysine/cadaverine antiporter, respectively. Increased CadAB activity was further suggested by the metabolomics analysis. The down-regulated genes include sialic acid catabolism genes. Metabolomic analysis also suggested increased reductive pathway of TCA cycle and decreased purine metabolism in the V. cholerae ΔnqrA-F mutant. Lack of Na+-NQR did not affect any of the Na+ pumping-related phenotypes of V. cholerae suggesting that other secondary Na+ pump(s) can compensate for Na+ pumping activity of Na+-NQR. Overall, our study provides important insights into the contribution of Na+-NQR to V. cholerae physiology.

  11. 14N NQR lineshape in nanocrystals: An ab initio investigation of urea

    NASA Astrophysics Data System (ADS)

    Gregorovič, Alan

    2017-05-01

    14N nuclear quadrupole resonance (NQR) lineshapes mostly contain information of low interest, although in nanocrystals they may display some unexpected behaviour. In this work, we present an ab initio computational study of the 14N NQR lineshapes in urea nanocrystals as a function of the nanocrystal size and geometry, focusing on the surface induced broadening of the lineshapes. The lineshapes were obtained through a calculation of the electric field gradient for each nitrogen site in the nanocrystal separately, taking into account the individual crystal field by embedding the molecule of interest in a suitable lattice of point multipoles representing other urea molecules in the nanocrystal. The small influence of distant molecules is found with a series expansion, using the in-crystal Sternheimer shieldings which we also calculated ab initio. We have considered nanocrystals with two geometries: a sphere and a cube, with characteristic sizes between 5 and 100 nm. Our calculations suggest that there is a dramatic difference between the linewidths for the two geometries. For spheres, we find a steep drop in linewidths at ˜10 nm; at 5 nm the linewidth is ˜11 kHz, whereas for sizes above 20 nm the linewidth is practically negligible (<100 Hz). For cubes, on the other hand, we find a steady 1/size decrease, from 12 kHz at 10 nm to 1.2 kHz at 100 nm. This analysis is important for 14N NQR spectroscopy of crystalline pharmaceuticals, where nanoparticles are increasingly more often embedded in some sort of matrix. Although this is only a theoretical analysis, we believe that this work can serve as a guidance for the forthcoming experimental analysis.

  12. (14)N NQR lineshape in nanocrystals: An ab initio investigation of urea.

    PubMed

    Gregorovič, Alan

    2017-05-21

    (14)N nuclear quadrupole resonance (NQR) lineshapes mostly contain information of low interest, although in nanocrystals they may display some unexpected behaviour. In this work, we present an ab initio computational study of the (14)N NQR lineshapes in urea nanocrystals as a function of the nanocrystal size and geometry, focusing on the surface induced broadening of the lineshapes. The lineshapes were obtained through a calculation of the electric field gradient for each nitrogen site in the nanocrystal separately, taking into account the individual crystal field by embedding the molecule of interest in a suitable lattice of point multipoles representing other urea molecules in the nanocrystal. The small influence of distant molecules is found with a series expansion, using the in-crystal Sternheimer shieldings which we also calculated ab initio. We have considered nanocrystals with two geometries: a sphere and a cube, with characteristic sizes between 5 and 100 nm. Our calculations suggest that there is a dramatic difference between the linewidths for the two geometries. For spheres, we find a steep drop in linewidths at ∼10 nm; at 5 nm the linewidth is ∼11 kHz, whereas for sizes above 20 nm the linewidth is practically negligible (<100 Hz). For cubes, on the other hand, we find a steady 1/size decrease, from 12 kHz at 10 nm to 1.2 kHz at 100 nm. This analysis is important for (14)N NQR spectroscopy of crystalline pharmaceuticals, where nanoparticles are increasingly more often embedded in some sort of matrix. Although this is only a theoretical analysis, we believe that this work can serve as a guidance for the forthcoming experimental analysis.

  13. The Structure of Tetrachlorostannate Complexes with Ketones from 35Cl NQR Data

    NASA Astrophysics Data System (ADS)

    Feshin, Valentin P.; Dolgushin, Gennadii V.; Lazarev, Igor M.; Voronkov, Mikhail, G.

    1990-04-01

    35Cl NQR spectra (77 K) of 1:1 and 2:1 RR'CO-SnCl 4 are recorded and discussed. These spectra change in the course of time. At low temperatures either octahedral or trigonal-bipyramidal complexes (depending on the ratio of components and the nature of ligands) are formed. Frequently these systems contain a mixture of steric isomers or a mixture of complexes having different coordination numbers of the tin atom. In the solid state some complexes show a transition from one to another configuration.

  14. 35CI NQR Spectroscopy on Salts and Molecular Compounds of Trichloroacetic Acid

    NASA Astrophysics Data System (ADS)

    Fichtner, Winfried; Markworth, Axel; Weiden, Norbert; Weiss, Alarich

    1986-02-01

    The temperature dependence of salts M(1)H(Cl3CCOO)2 and molecular compounds of trichloroacetic acid with amines and benzaldehydes, TCA · X, was studied, The data fit rather well to the known dependence of the mean frequency shift Δ on the pkadifference of X with respect to TCA. A linear relation is observed between the bleaching out temperature Tb of the 35Cl NQR lines and Δ for M(1)H(Cl3CCOO)2 and for TCA · X, X = benzaldehydes.

  15. /sup 35/Cl NQR spectra of complexes of tetrachlorostannane with substituted benzoyl chlorides

    SciTech Connect

    Feshin, V.P.; Dogushin, G.V.; Lazarev, I.M.; Voronkov, M.G.; Feshina, E.V.

    1987-05-01

    /sup 35/Cl NQR spectra of mixtures of SnCl/sub 4/ with 2-, 3- and 4-XC/sub 6/H/sub 4/COCl were obtained. The electronic and steric structure of the complexes obtained was established. Their formation and structure depend on the nature of substituents X. Complexes with a trigonal-bipyramidal structure are formed with the participation of the carbonyl oxygen atom of the ligand as an electron-donor-center, and complexes with trans-octahedral structure, with the participation of the sulfur atom of the X = CH/sub 3/S substituent.

  16. Ru-NQR Study for Novel Phase Transition in CeRu2Al10

    NASA Astrophysics Data System (ADS)

    Matsumura, Masahiro; Tomita, Naoya; Matsuoka, Junichirou; Kishimoto, Yasuki; Kato, Harukazu; Kitagawa, Kentaro; Nishioka, Takashi; Tanida, Hiroshi; Sera, Masafumi

    2014-10-01

    We have performed Ru-NQR measurements on CeRu2Al10 exhibiting novel phase transition at an abnormally high temperature T0 = 27.3 K and on NdRu2Al10 with a magnetic transition temperature Tm = 2.4 K as a reference RKKY system. The splitting of the NQR line due to internal fields below T0 shows a mean-field-like monotonic increase, indicating no change in the magnetic structure below T0. The internal field strength is one order larger than those at Al sites in CeRu2Al10, and is comparable to that at the Ru site in NdRu2Al10 despite the sevenfold smaller magnitude of the 4f moment, being indicative of an enhanced conduction electron polarization at the Ru site. One of the causes of the high T0 might be the enhanced exchange coupling through the Ce-Ru-Ce path mediated by the enhanced conduction electron polarization. Being similar to that in the Al site, the nuclear spin-lattice relaxation rate 1/T1 shows a gap-like decrease below T0 without enhancement owing to a critical slowing down at T0, in contrast to the mean field 2nd-order transition.

  17. Pseudogap Behavior in Fully Filled Skutterudite YbFe4Sb12 Detected by Sb NQR

    NASA Astrophysics Data System (ADS)

    Magishi, Ko-ichi; Watanabe, Ryo; Hisada, Akihiko; Saito, Takahito; Koyama, Kuniyuki; Saito, Takashi; Higashinaka, Ryuji; Aoki, Yuji; Sato, Hideyuki

    2014-08-01

    We report the results of 121,123Sb-nuclear quadrupole resonance (NQR) measurements on the fully filled skutterudite YbFe4Sb12 synthesized under high pressure, and compare them with those for an Yb-deficient sample synthesized under ambient pressure in order to elucidate the intrinsic behavior and the effects of the Yb-site filling fraction on magnetic properties. The NQR spectra for the fully filled sample remain narrow down to 1.5 K, indicating no sign of a phase transition, in contrast to the results of the Yb-deficient sample. The nuclear spin-lattice relaxation rate divided by temperature, 1/T1T, is composed of two terms as 1/T1T = (1/T1T)χ + (1/T1T)PG. The first term (1/T1T)χ is scaled to the magnetic susceptibility, which is similar to the behavior of nearly ferromagnetic metals. The pseudogap behavior, related to the second term (1/T1T)PG, is consistent with the optical conductivity measurements, and is a characteristic of the filled skutterudites with a divalent filler ion.

  18. TNT detection with 14N NQR: multipulse sequences and matched filter.

    PubMed

    Gregorovic, Alan; Apih, Tomaz

    2009-06-01

    Nuclear quadrupole resonance (NQR) has a distinct potential to verify the presence of nitrogen bearing substances based on the unequivocal signatures of their spectra. Therefore, this technique is especially suitable for remote detection of illicit substances and explosives. Unfortunately, the inherent signal-to-noise of the most abundant explosive trinitrotoluene (TNT) is very low. Here we present an NQR method with improved sensitivity for estimation of the probability of TNT presence in the investigated object. The method consists of a spin-lock spin-echo (SLSE) multipulse sequence for signal excitation and a time domain matched filter for signal detection. We find that the signal-to-noise increases by shortening the pulse spacings, even though this means a decrease in spectral resolution. In our case, the decrease of the pulse spacings from the typical 2 ms to 540 micros resulted in an increase of the signal-to-noise by 14 dB. A theory describing this enhancement is presented and compared to experimental results on TNT. Issues related to temperature and polymorphism variations are also discussed.

  19. Correlation between NQR parameters and residue size of aliphatic amino acids and their dimers.

    PubMed

    Ghaderi, Ali Reza; Sabzyan, Hassan; Hadipour, Nasser L

    2006-03-01

    Nuclear quadrupole coupling constants (NQCC), chi, and asymmetry parameters, eta, of 2D, 14N and 17O nuclei have been calculated for aliphatic amino acids and their dimers using MP2/6-311++G** method to shed some light on the differences between the structural parameters in the aliphatic amino acids and their dimers. For this purpose, electric field gradient (EFG) at the sites of quadrupolar nuclei have been calculated and evaluated for each compound. A correlation is observed between the calculated NQCC parameters and the conformational structures of the compounds, showing that extraction of structural data from the NQR spectra might be promising. Our results showed that 17O NQCC of terminal carboxylic acid and 14N NQCC of the terminal amino groups are, respectively, the least and the most sensitive parameters to the variation of the size of the residue. It is found also that conformation of R (i.e. values of the dihedral angles) plays a very effective role in the determination of the values of the calculated NQCC parameters. Sensitivity of the NQR parameters to the changes in the conformational structure is significantly greater (nearly 20-fold) than that to the changes in the other structural parameters such as bond lengths.

  20. NMR and NQR studies of the heavy fermion superconductors CeTIn{sub 5} (T=Co and Ir)

    SciTech Connect

    Kohori, Y.; Yamato, Y.; Iwamoto, Y.; Kohara, T.; Bauer, E. D.; Maple, M. B.; Sarrao, J. L.

    2001-10-01

    We have carried out {sup 115}In and {sup 59}Co nuclear quadrupole resonance and nuclear magnetic resonance measurements on CeCoIn{sub 5} and CeIrIn{sub 5}. The temperature T dependence of the nuclear spin-lattice relaxation rate 1/T{sub 1} of {sup 115}In in the normal state indicates that CeCoIn{sub 5} is located just at an antiferromagnetic instability, and CeIrIn{sub 5} is in the nearly antiferromagnetic region. In the superconducting state, 1/T{sub 1} has no Hebel-Slichter coherence peak just below T{sub C} and a power-law T dependence (close to T{sup 3}) at very low temperatures, which indicates the existence of line nodes in the superconducting energy gap. The {sup 115}In (Ce-In plane) Knight shift in CeCoIn{sub 5} decreases for both parallel and perpendicular directions to the tetragonal c axis in the superconducting state, which shows that the spin susceptibility decreases in all directions. These results indicate that CeCoIn{sub 5} and CeIrIn{sub 5} exhibit non-s-wave even parity (probably d-wave) superconductivity.

  1. Hybridization-driven gap in U3Bi4Ni3: a 209Bi NMR/NQR study

    SciTech Connect

    Baek, Seung H

    2009-01-01

    We report {sup 209}Bi nuclear-magnetic-resonance and nuclear-quadrupole-resonance measurements on a single crystal of the Kondo insulator U{sub 3}Bi{sub 4}Ni{sub 3}. The {sup 209}Bi nuclear-spin-lattice relaxation rate (T{sub 1}{sup -1}) shows activated behavior and is well fit by a spin gap of 220 K. The {sup 209}Bi Knight shift (K) exhibits a strong temperature dependence arising from 5f electrons, in which K is negative at high temperatures and increases as the temperature is lowered. Below 50 K, K shows a broad maximum and decreases slightly upon further cooling. Our data provide insight into the evolution of the hyperfine fields in a fully gapped Kondo insulator based on 5f electron hybridization.

  2. A mutation in Na(+)-NQR uncouples electron flow from Na(+) translocation in the presence of K(+).

    PubMed

    Shea, Michael E; Mezic, Katherine G; Juárez, Oscar; Barquera, Blanca

    2015-01-20

    The sodium-pumping NADH:ubiquinone oxidoreductase (Na(+)-NQR) is a bacterial respiratory enzyme that obtains energy from the redox reaction between NADH and ubiquinone and uses this energy to create an electrochemical Na(+) gradient across the cell membrane. A number of acidic residues in transmembrane helices have been shown to be important for Na(+) translocation. One of these, Asp-397 in the NqrB subunit, is a key residue for Na(+) uptake and binding. In this study, we show that when this residue is replaced with asparagine, the enzyme acquires a new sensitivity to K(+); in the mutant, K(+) both activates the redox reaction and uncouples it from the ion translocation reaction. In the wild-type enzyme, Na(+) (or Li(+)) accelerates turnover while K(+) alone does not activate. In the NqrB-D397N mutant, K(+) accelerates the same internal electron transfer step (2Fe-2S → FMNC) that is accelerated by Na(+). This is the same step that is inhibited in mutants in which Na(+) uptake is blocked. NqrB-D397N is able to translocate Na(+) and Li(+), but when K(+) is introduced, no ion translocation is observed, regardless of whether Na(+) or Li(+) is present. Thus, this mutant, when it turns over in the presence of K(+), is the first, and currently the only, example of an uncoupled Na(+)-NQR. The fact the redox reaction and ion pumping become decoupled from each other only in the presence of K(+) provides a switch that promises to be a useful experimental tool.

  3. Application of nuclear quadrupole resonance to the study of clathrates. sup 35 Cl NQR and crystallography of clathrated CCl sub 4

    SciTech Connect

    Pang, Li; Lucken, E.A.C.; Bernardinelli, G. )

    1990-11-21

    The {sup 35}Cl nuclear quadrupole resonance (NQR) spectra of CCl{sub 4} in more than 20 clathrates have been measured in the range 4-200 K. The crystal structures of CCl{sub 4}/Dianin's compound (1), CCl{sub 4}/Fe(AcAc){sub 3} (3), CCl{sub 4}/Ni(SCN){sub 2}(3-MePy){sub 4} (4), and CCl{sub 4}/Ni(exan){sub 2}(4,4{prime}-dm-2,2{prime}-bpy) (19) clathrates are also reported. Site symmetry and site multiplicity of the guest molecule in clathrates were determined by NQR spectroscopy and by x-ray crystallography. The degree of host-guest interaction was estimated from the NQR frequency shifts. The libration frequencies of the guest molecules in trigonal cavities were determined from NQR frequencies by Bayer-Kushida theory analysis.

  4. Cr3+ NMR for Multiferroic Chromium spinel ZnCr2Se4

    NASA Astrophysics Data System (ADS)

    Park, Sejun; Kwon, Sangil; Lee, Soonchil; Khim, Seunghyun; Bhoi, Dilip Kumar; Kim, Kee Hoon

    Multiferroic systems including ZnCr2Se4, the chromium spinel with helical spin structure, have been in huge interest for decades due to its physical variety and applicability. In the temperature range between 21K and 80K, this material shows negative thermal expansion. Due to the bond frustration, the spins of the chromium ions order helically below the transition temperature, 21K, though the exchange constant tends to make a ferro-order. The anomalous 1storder-like magnetic transition is yet clarified and still an interesting topic. To probe microscopic origin of these features, we measured zero-field NMR of Cr3+ ions having nuclear spin 3/2. Six peaks were observed revealing Nuclear Quadrupole Resonance(NQR) and anisotropic hyperfine field at chromium sites. The NQR spectrum reveals that the structure is highly distorted below the magnetic transition temperature where the normal Jahn-Teller distortion is absent. Temperature dependence of the spectrum is also measured to obtain the magnetization as a function of temperature.

  5. Riboflavin Is an Active Redox Cofactor in the Na+-pumping NADH:Quinone Oxidoreductase (Na+-NQR) from Vibrio cholerae*

    PubMed Central

    Juárez, Oscar; Nilges, Mark J.; Gillespie, Portia; Cotton, Jennifer; Barquera, Blanca

    2008-01-01

    Here we present new evidence that riboflavin is present as one of four flavins in Na+-NQR. In particular, we present conclusive evidence that the source of the neutral radical is not one of the FMNs and that riboflavin is the center that gives rise to the neutral flavosemiquinone. The riboflavin is a bona fide redox cofactor and is likely to be the last redox carrier of the enzyme, from which electrons are donated to quinone. We have constructed a double mutant that lacks both covalently bound FMN cofactors (NqrB-T236Y/NqrC-T225Y) and have studied this mutant together with the two single mutants (NqrB-T236Y and NqrC-T225Y) and a mutant that lacks the noncovalently bound FAD in NqrF (NqrF-S246A). The double mutant contains riboflavin and FAD in a 0.6:1 ratio, as the only flavins in the enzyme; noncovalently bound flavins were detected. In the oxidized form, the double mutant exhibits an EPR signal consistent with a neutral flavosemiquinone radical, which is abolished on reduction of the enzyme. The same radical can be observed in the FAD deletion mutant. Furthermore, when the oxidized enzyme reacts with ubiquinol (the reduced form of the usual electron acceptor) in a process that reverses the physiological direction of the electron flow, a single kinetic phase is observed. The kinetic difference spectrum of this process is consistent with one-electron reduction of a neutral flavosemiquinone. The presence of riboflavin in the role of a redox cofactor is thus far unique to Na+-NQR. PMID:18832377

  6. NMR of lignins

    Treesearch

    John Ralph; Larry L. Landucci

    2010-01-01

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

  7. NMR analysis of biodiesel

    USDA-ARS?s Scientific Manuscript database

    Biodiesel is usually analyzed by the various methods called for in standards such as ASTM D6751 and EN 14214. Nuclear magnetic resonance (NMR) is not one of these methods. However, NMR, with 1H-NMR commonly applied, can be useful in a variety of applications related to biodiesel. These include monit...

  8. Magnetic field-cycling NMR and (14)N, (17)O quadrupole resonance in the explosive pentaerythritol tetranitrate (PETN).

    PubMed

    Smith, John A S; Rayner, Timothy J; Rowe, Michael D; Barras, Jamie; Peirson, Neil F; Stevens, Andrew D; Althoefer, Kaspar

    2010-05-01

    The explosive pentaerythritol tetranitrate (PETN) C(CH(2)-O-NO(2))(4) has been studied by (1)H NMR and (14)N NQR. The (14)N NQR frequency and spin-lattice relaxation time T(1Q) for the nu(+) line have been measured at temperatures from 255 to 325K. The (1)H NMR spin-lattice relaxation time T(1) has been measured at frequencies from 1.8kHz to 40MHz and at temperatures from 250 to 390K. The observed variations are interpreted as due to hindered rotation of the NO(2) group about the bond to the oxygen atom of the CH(2)-O group, which produces a transient change in the dipolar coupling of the CH(2) protons, generating a step in the (1)H T(1) at frequencies between 2 and 100kHz. The same mechanism could also explain the two minima observed in the temperature variation of the (14)N NQR T(1Q) near 284 and 316K, due in this case to the transient change in the (14)N...(1)H dipolar interaction, the first attributed to hindered rotation of the NO(2) group and the second to an increase in torsional amplitude of the NO(2) group due to molecular distortion of the flexible CH(2)-O-NO(2) chain which produces a 15% increase in the oscillational amplitude of the CH(2) group. The correlation times governing the (1)H T(1) values are approximately 25 times longer than those governing the (14)N NQR T(1Q), explained by the slow spin-lattice cross-coupling between the two spin systems. At higher frequencies, the (1)H T(1) dispersion results show well-resolved dips between 200 and 904kHz assigned to level crossing with (14)N and weaker features between 3 and 5MHz tentatively assigned to level crossing with (17)O. Copyright 2010 Elsevier Inc. All rights reserved.

  9. High radio-frequency field strength nutation NMR of quadrupolar nuclei

    NASA Astrophysics Data System (ADS)

    Franssen, W. M. J.; Rezus, Y. L. A.; Kentgens, A. P. M.

    2016-12-01

    Owing to the introduction of microcoils, high RF field strength nutation NMR is a viable candidate for the study of quadrupolar nuclei with strong quadrupolar couplings, not accessible using contemporary NMR techniques. We show powder 23 Na nutation spectra on sodium nitrite for RF field strengths of up to 1170 kHz, that conform to theoretical predictions. For lanthanum fluoride powder, 139 La nutation spectra taken at elevated RF field amplitudes show clear discrepancies when compared to the theory. These errors are shown to be mainly caused by pulse transients at the end of the pulse, which proved to be detrimental to the shape of the nutation spectra. Using a nutation pulse which ends in a sudden frequency jump, we show that these errors can be reduced, and nutation spectra that conform to theory can be readily acquired. This enables nutation NMR for the study of quadrupolar nuclei with a strong quadrupolar coupling, bridging the gap between NMR, which can only analyse nuclei with a weak to medium quadrupolar coupling, and NQR, were extensive searching for the right quadrupolar frequency is the limiting factor.

  10. Unconventional superconductivity in the itinerant ferromagnet UGe 2: 73Ge-NQR study under pressure

    NASA Astrophysics Data System (ADS)

    Harada, A.; Kawasaki, S.; Mukuda, H.; Kitaoka, Y.; Haga, Y.; Yamamoto, E.; Ōnuki, Y.; Itoh, K. M.; Haller, E. E.; Harima, H.

    2006-05-01

    The superconducting characteristics on the itinerant ferromagnetic superconductor UGe 2 have been investigated via the 73Ge-NQR measurements under pressure ( P) near the critical pressure Px where the first-order transition takes place from the low-temperature ( T) and low- P ferromagnetic phase (FM2) to high- T and high- P one (FM1). The measurements of nuclear spin-lattice relaxation rate 1/T1 have revealed a power-law like behavior as Tn without the coherence peak, whereas at low temperatures, it deviates from the Tn dependence to a T-linear like behavior. These results that depend on the pressure are well understood in terms of non-unitary spin-triplet pairing state where the ferromagnetic up-spin band is gapped, but the down-spin band remains gapless at the Fermi level. We will argue an intimate relationship of the onset of SC with FM1 and FM2.

  11. Three-dimensional high-inductance birdcage coil for NQR applications.

    PubMed

    Peshkovsky, A S; Cerioni, L; Osan, T M; Avdievich, N I; Pusiol, D J

    2006-09-01

    A birdcage coil capable of operating simultaneously and independently in three orthogonal dimensions has been developed. A co-rotational end-ring mode producing an RF field in the longitudinal direction was utilized in addition to the two common transverse orthogonal modes. Two conductor turns were used for each of the coil's windows, increasing its inductance by a factor of four, thereby, making the coil suitable for low-frequency applications. Two or three-frequency detection can be easily carried out with this device. Orthogonality of the coil's channels allows arbitrarily close frequency positioning of each resonant mode, potentially useful in wide-line NQR studies, in which simultaneous excitation/detection of signals from three adjacent regions of a single wide line can be performed. The coil's performance was evaluated using a three-dimensional scheme, in which a circularly polarized experiment was combined with a linearly polarized measurement at another frequency, resulting in SNR improvement by 55%.

  12. First-principles study of (75)As NQR in arsenic-chalcogenide compounds.

    PubMed

    Edwards, Arthur H; Taylor, P C; Campbell, Kristy A; Pineda, Andrew C

    2011-02-09

    We present a theoretical study of the nuclear quadrupole interaction, ν(Q), of (75)As in crystalline and amorphous materials containing sulfur and selenium, and compare them with experiment. We studied a combination of hydrogen-terminated molecular clusters and periodic cells at various levels of quantum chemical theory. The results show clearly that the standard density functional theory (DFT) approximations, LDA and GGA, underestimate the nuclear quadrupole (NQR) interaction systematically, while Hartree-Fock theory overestimates it to an even greater degree. However, various levels of configuration interaction and the B3LYP hybrid exchange-correlation functional, which includes some exact exchange, give very good quantitative agreement for As bonded only to the chalcogen species. As-As bonds require highly converged basis sets. We have performed a systematic study of the effect of local distortions around an arsenic atom on ν(Q) and η. Using a simple, semiclassical model, we have combined our total energy results with our NQR calculations to predict ν(Q) lineshapes for bond angle and bond length distortions. Our predictions for lineshape, including first and second moments, are in excellent agreement with the results of Su et al for a-As(2)S(3), a-As(2)Se(3) and a-AsSe. We offer new insight into the distortions that led to this inhomogeneous broadening. Our results show clearly that, for trivalent arsenic atoms with zero or one arsenic nearest neighbor, symmetric bond stretching is the predominant contributor to the ν(Q) linewidth. However, in the presence of two arsenic nearest neighbors, distortions of the As-As-As apex angle dominates and, in fact, leads to a much larger second moment, in agreement with experiment.

  13. Studies related to primitive chemistry. A proton and nitrogen-14 nuclear magnetic resonance amino acid and nucleic acid constituents and a and their possible relation to prebiotic

    NASA Technical Reports Server (NTRS)

    Manatt, S. L.; Cohen, E. A.; Shiller, A. M.; Chan, S. I.

    1973-01-01

    Preliminary proton nuclear magnetic resonance (NMR) studies were made to determine the applicability of this technique for the study of interactions between monomeric and polymeric amino acids with monomeric nucleic acid bases and nucleotides. Proton NMR results for aqueous solutions (D2O) demonstrated interactions between the bases cytosine and adenine and acidic and aromatic amino acids. Solutions of 5'-AMP admixed with amino acids exhibited more complex behavior but stacking between aromatic rings and destacking at high amino acids concentration was evident. The multisite nature of 5'-AMP was pointed out. Chemical shift changes for adenine and 5'-AMP with three water soluble polypeptides demonstrated that significant interactions exist. It was found that the linewidth-pH profile of each amino acid is unique. It is concluded that NMR techniques can give significant and quantitative data on the association of amino acid and nucleic acid constituents.

  14. 121Sb-NMR Knight shift study of filled skutterudite CeOs4Sb12

    NASA Astrophysics Data System (ADS)

    Yogi, M.; Niki, H.; Mukuda, H.; Kitaoka, Y.; Sugawara, H.; Sato, H.

    2012-12-01

    We carried out an 121Sb nuclear magnetic resonance (NMR) measurement on CeOs4Sb12 to investigate its electric state. The precise temperature (T) dependence of the Knight shift was obtained by using an aligned powdered sample and NQR parameters. The T dependence of the Knight shift below 300 K can not be explained by the c-f hybridization gap model with 2D = 3000 K and 2Δ = 320 K obtained by the 1/T1. This result indicates that there is q-dependence in the gap. It was revealed that a ferromagnetic correlation develops with decreasing temperature below 50 K from an increase of the Knight shift. Considering this result and previous 1/T1 measurements, there are both ferromagnetic and antiferromagnetic fluctuations in CeOs4Sb12.

  15. Intimate interplay between superconductivity and antiferromagnetism in CeNiGe3:A73Ge-NQR study under pressure

    NASA Astrophysics Data System (ADS)

    Harada, A.; Mukuda, H.; Kitaoka, Y.; Thamizhavel, A.; Okuda, Y.; Settai, R.; Ōnuki, Y.; Itoh, K. M.; Haller, E. E.; Harima, H.

    2008-04-01

    We report the 73Ge-NQR studies on the antiferromagnetic (AFM) heavy-fermion compound CeNiGe3 which shows two domes like pressure-induced superconducting phases in the pressure ( P) ranges of 1.7-3.5 GPa and 5.9-7.3 GPa denoted as SC1 and SC2, respectively [M. Nakashima, et al., J. Phys. Condens. Matter. 16 (2004) L255, H. Kotegawa, et al., J. Phys. Soc. Jpn. 75 (2006) 044713]. The NQR spectra have revealed a change from an incommensurate AFM structure at P=0 and 2.0 GPa into a commensurate one at P=2.8 GPa. The onset of the SC1 may be relevant to an intimate evolution from the incommensurate into commensurate AFM-spin structure as P increases.

  16. 115In-NQR study of CeRh1-xIrxIn5 under pressure

    NASA Astrophysics Data System (ADS)

    Mugino, Y.; Kawasaki, S.; Yashima, M.; Mukuda, H.; Kitaoka, Y.; Shishido, H.; Ōnuki, Y.

    2007-03-01

    We report on pressure-induced evolutions of antiferromagnetic spin fluctuations (AFM-SFs) and unconventional superconductivity on the x=0.6 sample in a series of compounds CeRh1-xIrxIn5 via the 115In nuclear-quadrupole-resonance (NQR) experiment. The In-NQR 1/T1 measurements have revealed that the slight application of pressure makes Tc=0.9 K at P=0 increase up to Tc=1.06 K at P=0.47 GPa. Concomitantly, the character of AFM-SF evolves from an isotropic regime to an anisotropic one as P increases. These results suggest that AFM-SFs play vital role in mediating the strong-coupling superconductivity in CeRh1-xIrxIn5.

  17. Dependence of (35)Cl NQR on hydrogen bonding and temperature in dichlorophenol-aniline charge transfer complexes.

    PubMed

    Ramananda, D; Ramesh, K P; Uchil, J

    2007-10-01

    The hydrogen-bonded charge transfer complexes of aniline with pi-acceptors (or proton donors) such as 2,5-, 2,6-, 3,4- and 3,5-dichlorophenol were prepared. The (35)Cl nuclear quadrupole resonance (NQR) frequencies of these charge transfer complexes in the temperature range 77-300 K were measured to ascertain the existence or otherwise of a phase transition upon complex formation. Further, the NQR frequency and asymmetry parameter of the electric field gradient at the site of quadrupole nucleus were used to estimate the chemical bond parameters, namely ionic bond, double bond character of the carbon-chlorine(C--Cl) bond and the percentage charge transfer between the donor-acceptor components in charge transfer complexes. The effect of hydrogen bonding and temperature on the charge transfer process is analysed. (c) 2007 John Wiley & Sons, Ltd.

  18. Effects of nonsinusoidal character of atomic modulation on NQR spin-lattice relaxation time of incommensurate phases

    SciTech Connect

    Perez, Silvina C.; Schurrer, Clemar; Wolfenson, Alberto

    2001-06-01

    The present work is an extention of the theoretical calculation developed by Blinc to explain the temperature and frequency dependence of the spin-lattice relaxation time in incommensurate phases. We have evaluated the influence of the nonsinusoidal character of the atomic modulation, in the linear approximation, over the NQR spectra and over the spin-lattice relaxation due to direct and Raman processes. It is shown that the peak with lower intensity in the NQR spectra always has a larger T{sub 1} and viceversa. The results have been applied to bis(4-chlorophenyl)sulfone T{sub 1} and line-shape data. The temperature and frequency dependence of T{sub 1} are well reproduced if Raman processes are considered.

  19. Electronic structure and biological activity of chosen DDT-type insecticides studied by 35Cl-NQR.

    PubMed

    Jadzyn, Maciej; Nogaj, Bolesław

    2009-02-01

    A correlation between the electronic structure and biological activity of chosen dichlorodiphenyltrichloroethane (DDT)-type insecticides: 1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane, 1,1-dichloro-2,2-bis(4-chlorophenyl)ethane, 2,2-bis(p-chlorophenyl)-1,1-dichloroethylene, 2,2-bis(4-chlorophenyl)ethanoic acid and 4,4'-dichlorobenzophenone (used in agriculture) has been analysed on the basis of the (35)Cl-nuclear quadrupole resonance (NQR) spectroscopy. The (35)Cl-NQR resonance frequencies measured at 77 K have been correlated with the lethal dose (LD(50)) parameter that characterises the biological activity of these insecticides. 2008 John Wiley & Sons, Ltd.

  20. Role of the NAD(P)H quinone oxidoreductase NQR and the cytochrome b AIR12 in controlling superoxide generation at the plasma membrane.

    PubMed

    Biniek, Catherine; Heyno, Eiri; Kruk, Jerzy; Sparla, Francesca; Trost, Paolo; Krieger-Liszkay, Anja

    2017-04-01

    The quinone reductase NQR and the b-type cytochrome AIR12 of the plasma membrane are important for the control of reactive oxygen species in the apoplast. AIR12 and NQR are two proteins attached to the plant plasma membrane which may be important for generating and controlling levels of reactive oxygen species in the apoplast. AIR12 (Auxin Induced in Root culture) is a single gene of Arabidopsis that codes for a mono-heme cytochrome b. The NADPH quinone oxidoreductase NQR is a two-electron-transferring flavoenzyme that contributes to the generation of O 2(•-) in isolated plasma membranes. A. thaliana double knockout plants of both NQR and AIR12 generated more O 2(•-) and germinated faster than the single mutant affected in AIR12. To test whether NQR and AIR12 are able to interact functionally, recombinant purified proteins were added to plasma membranes isolated from soybean hypocotyls. In vitro NADH-dependent O 2(•-) production at the plasma membrane in the presence of NQR was reduced upon addition of AIR12. Electron donation from semi-reduced menadione to AIR12 was shown to take place. Biochemical analysis showed that purified plasma membrane from soybean hypocotyls or roots contained phylloquinone and menaquinone-4 as redox carriers. This is the first report on the occurrence of menaquinone-4 in eukaryotic photosynthetic organisms. We propose that NQR and AIR12 interact via the quinone, allowing an electron transfer from cytosolic NAD(P)H to apoplastic monodehydroascorbate and control thereby the level of reactive oxygen production and the redox state of the apoplast.

  1. Structural and Functional Investigation of Flavin Binding Center of the NqrC Subunit of Sodium-Translocating NADH:Quinone Oxidoreductase from Vibrio harveyi

    PubMed Central

    Bertsova, Yulia; Polovinkin, Vitaly; Gushchin, Ivan; Ishchenko, Andrii; Kovalev, Kirill; Mishin, Alexey; Kachalova, Galina; Popov, Alexander; Bogachev, Alexander; Gordeliy, Valentin

    2015-01-01

    Na+-translocating NADH:quinone oxidoreductase (NQR) is a redox-driven sodium pump operating in the respiratory chain of various bacteria, including pathogenic species. The enzyme has a unique set of redox active prosthetic groups, which includes two covalently bound flavin mononucleotide (FMN) residues attached to threonine residues in subunits NqrB and NqrC. The reason of FMN covalent bonding in the subunits has not been established yet. In the current work, binding of free FMN to the apo-form of NqrC from Vibrio harveyi was studied showing very low affinity of NqrC to FMN in the absence of its covalent bonding. To study structural aspects of flavin binding in NqrC, its holo-form was crystallized and its 3D structure was solved at 1.56 Å resolution. It was found that the isoalloxazine moiety of the FMN residue is buried in a hydrophobic cavity and that its pyrimidine ring is squeezed between hydrophobic amino acid residues while its benzene ring is extended from the protein surroundings. This structure of the flavin-binding pocket appears to provide flexibility of the benzene ring, which can help the FMN residue to take the bended conformation and thus to stabilize the one-electron reduced form of the prosthetic group. These properties may also lead to relatively weak noncovalent binding of the flavin. This fact along with periplasmic location of the FMN-binding domains in the vast majority of NqrC-like proteins may explain the necessity of the covalent bonding of this prosthetic group to prevent its loss to the external medium. PMID:25734798

  2. Investigation of Some New Nonlinear Optical Crystals by Means of NQR, IR and X-Ray Diffraction Methods

    NASA Astrophysics Data System (ADS)

    Petrosyan, A. M.; Terzyan, S. S.; Burbelo, V. M.; Sukiasyan, R. P.

    1998-07-01

    Some new analogues of the nonlinear optical crystal L-arginine phosphate monohydrate (LAP) (Arg • HIO3 , Arg • 2HIO3 , Lys • HIO3 , Lys • 2HIO3 , Lys • 3HIO3 , Bet • 3HIO3) were obtained and investigated by means of IR, NQR, X-ray diffraction and SHG methods. The importance of this class of crystals for revealing new nonlinear optical crystals is pointed out.

  3. Local moments in the heterogeneous electronic state of Cd-substituted CeCoIn 5 : NQR relaxation rates

    DOE PAGES

    Sakai, H.; Ronning, F.; Hattori, T.; ...

    2017-04-06

    Here, we have used nuclear quadrupole resonance (NQR) to probe microscopically the response of a prototypical quantum critical metal CeCoIn5 to substitutions of small amounts of Cd for In. Approximately half of the Cd substituents induce local Ce moments in their close proximity, as observed by site-dependent longitudinal nuclear spin relaxation rates 1/T1. In order to reaffirm that localized f moments are induced around the Cd substituents, we find a Gaussian spin-echo decay rate 1/T2G of transverse nuclear spin relaxation. Furthermore,more » $${T}_{1}T/{T}_{2\\text{G}}^{2}$$ for the NQR subpeak is found to be proportional to temperatures, again indicating local moments fluctuations around the Cd substituents, while that for the NQR main peak shows a T0.7-dependence. The latter temperature dependence is close to 0.75 in pure CeCoIn5 and indicates that the bulk electronic state is located close to a two dimensional quantum critical instability.« less

  4. Possibility of valence-fluctuatsion-mediated superconductivity in Cd-doped CeIrIn(5) probed by In NQR.

    PubMed

    Yashima, M; Tagami, N; Taniguchi, S; Unemori, T; Uematsu, K; Mukuda, H; Kitaoka, Y; Ota, Y; Honda, F; Settai, R; Onuki, Y

    2012-09-14

    We report on a pressure-induced evolution of exotic superconductivity and spin correlations in CeIr(In(1-x)Cd(x))(5) by means of in-nuclear-quadrupole-resonance (NQR) studies. Measurements of an NQR spectrum and nuclear-spin-lattice-relaxation rate 1/T(1) have revealed that antiferromagnetism induced by Cd doping emerges locally around Cd dopants, but superconductivity is suddenly induced at T(c)=0.7 and 0.9 K at 2.34 and 2.75 GPa, respectively. The unique superconducting characteristics with a large fraction of the residual density of state at the Fermi level which increases with T(c) differ from those for anisotropic superconductivity mediated by antiferromagnetic correlations. By incorporating the pressure dependence of the NQR frequency pointing to the valence change of Ce, we suggest that unconventional superconductivity in the CeIr(In(1-x)Cd(x))(5) system may be mediated by valence fluctuations.

  5. NQR study of local structures and cooling rate dependent superconductivity in La sub 2 CuO sub 4+. delta

    SciTech Connect

    Reyes, A.P.; Ahrens, E.T.; Hammel, P.C.; Heffner, R.H.; Thompson, J.D.; Canfield, P.C.; Fisk, Z. ); Schirber, J.E. )

    1992-01-01

    Structural properties of oxygen-annealed polycrystals of La{sub 2}CuO{sub 4 + {delta}} ({delta}{approximately}0.03) have been studied using {sup 139}La NQR spectroscopy. Superconducting critical temperatures were found to depend on the rate of cooling through a narrow temperature range at about 195K. Preliminary analysis of the {sup 139}La NQR spectra suggest that the oxygen-rich phase-separated region is composed of two structurally distinct phases, both of which are metallic and super-conducting. One phase has a structure closely related to the stoichiometric oxygen-poor compound. The second shows a considerable amount of apical oxygen disorder, a large shift in NQR frequency {nu}{sub Q}, and a volume fraction which increases with cooling rate. The formation of the second phase below {minus}200K is indicative of the freezing Of CuO{sub 6} octahedral tilting. Abrupt shifts in {nu}{sub Q} above {Tc} were also observed for both phases, suggestive of a local structural anomaly or charge transfer to the Cu-O plane.

  6. Local moments in the heterogeneous electronic state of Cd-substituted CeCoIn5: NQR relaxation rates

    NASA Astrophysics Data System (ADS)

    Sakai, H.; Ronning, F.; Hattori, T.; Tokunaga, Y.; Kambe, S.; Zhu, J.-X.; Wakeham, N.; Yasuoka, H.; Bauer, E. D.; Thompson, J. D.

    2017-04-01

    We have used nuclear quadrupole resonance (NQR) to probe microscopically the response of a prototypical quantum critical metal CeCoIn5 to substitutions of small amounts of Cd for In. Approximately half of the Cd substituents induce local Ce moments in their close proximity, as observed by site-dependent longitudinal nuclear spin relaxation rates 1/T1. To reaffirm that localized f moments are induced around the Cd substituents, we find a Gaussian spin-echo decay rate 1/T2G of transverse nuclear spin relaxation. Further, {T}1T/{T}2\\text{G}2 for the NQR subpeak is found to be proportional to temperatures, again indicating local moments fluctuations around the Cd substituents, while that for the NQR main peak shows a T0.7-dependence. The latter temperature dependence is close to 0.75 in pure CeCoIn5 and indicates that the bulk electronic state is located close to a two dimensional quantum critical instability.

  7. Correlation between proton transfer and (35)Cl NQR frequency as well as molecular geometry of chloranilic acid in co-crystals with some organic bases.

    PubMed

    Asaji, Tetsuo; Seliger, Janez; Zagar, Veselko; Ishida, Hiroyuki

    2010-07-01

    Proton transfer in hydrogen-bonded organic co-crystals of chloranilic acid with some organic bases was investigated by nuclear quadrupole resonance (NQR) spectroscopy. The (35)Cl NQR frequencies of chloranilic acid molecule as well as (14)N NQR frequencies of the organic base molecule were measured with the conventional pulse methods as well as double-resonance methods, respectively. The extent of proton transfer in the O...H...N hydrogen bond was estimated from Townes-Dailey analysis of the (14)N NQR parameters. The (35)Cl NQR frequency and molecular geometry of chloranilic acid are correlated to the extent of proton transfer in the protonation process of the organic base molecule. It is shown that the hydrogen bond affects the pi-electron system of chloranilic acid. Geometry dependence of the O...H...N hydrogen bond, i.e. the H-N valence bond order versus the hydrogen-bond geometry correlation is also discussed. Copyright (c) 2010 John Wiley & Sons, Ltd.

  8. Space Efficient Opposed-Anvil High-Pressure Cell and Its Application to Optical and NMR Measurements up to 9 GPa

    NASA Astrophysics Data System (ADS)

    Kitagawa, Kentaro; Gotou, Hirotada; Yagi, Takehiko; Yamada, Atsushi; Matsumoto, Takehiko; Uwatoko, Yoshiya; Takigawa, Masashi

    2010-02-01

    We have developed a new type of opposed-anvil high pressure cell with substantially improved space efficiency. The clamp cell and the gasket are made of non-magnetic Ni-Cr-Al alloy. Non-magnetic tungsten carbide (NMWC) is used for the anvils. The assembled cell with the dimension φ 29 mm × 41 mm is capable of generating pressure up to 9 GPa over a relatively large volume of 7 mm3. Our cell is particularly suitable for those experiments which require large sample space to achieve good signal-to-noise ratio, such as the nuclear magnetic resonance (NMR) experiment. Argon is used as the pressure transmitting medium to obtain good hydrostaticity. The pressure was calibrated in situ by measuring the fluorescence from ruby through a transparent moissanite (6H-SiC) window. We have measured the pressure and temperature dependences of the 63Cu nuclear-quadrupole-resonance (NQR) frequency of Cu2O, the in-plane Knight shift of metallic tin, and the Knight shift of platinum. These quantities can be used as reliable manometers to determine the pressure values in situ during the NMR/NQR experiments up to 9 GPa.

  9. Lectures on pulsed NMR

    SciTech Connect

    Pines, A.

    1988-08-01

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

  10. Lectures on pulsed NMR

    SciTech Connect

    Pines, A.

    1986-09-01

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

  11. Rotary echo nutation NMR

    NASA Astrophysics Data System (ADS)

    Janssen, R.; Tijink, G. A. H.; Veeman, W. S.

    1988-01-01

    A two-dimensional solid state NMR experiment which combines rotary echoes and nutation NMR is investigated and used to study different sodium sites in zeolite NaA. It is shown that with this technique sodium ions with different relaxation rates in the rotating frame can be distinguished.

  12. NMR logging apparatus

    SciTech Connect

    Walsh, David O; Turner, Peter

    2014-05-27

    Technologies including NMR logging apparatus and methods are disclosed. Example NMR logging apparatus may include surface instrumentation and one or more downhole probes configured to fit within an earth borehole. The surface instrumentation may comprise a power amplifier, which may be coupled to the downhole probes via one or more transmission lines, and a controller configured to cause the power amplifier to generate a NMR activating pulse or sequence of pulses. Impedance matching means may be configured to match an output impedance of the power amplifier through a transmission line to a load impedance of a downhole probe. Methods may include deploying the various elements of disclosed NMR logging apparatus and using the apparatus to perform NMR measurements.

  13. UC Merced NMR Instrumentation Acquisition

    DTIC Science & Technology

    2015-06-18

    UC Merced NMR Instrumentation Acquisition For the UC Merced NMR Instrumentation Acquisition proposal, a new 400 MHz and an upgraded 500 MHz NMR ...UC Merced NMR Instrumentation Acquisition Report Title For the UC Merced NMR Instrumentation Acquisition proposal, a new 400 MHz and an upgraded 500...MHz NMR have been delivered, installed, and incorporated into research and two lab courses. While no results from these instruments have been

  14. /sup 35/Cl and /sup 79, 81/Br NQR spectra of complexes of group III through group VII halides with chalcogen halides

    SciTech Connect

    Fokina, Z.A.; Kuznetsov, S.I.; Timoshchenko, N.I.; Bryukhova, E.V.

    1982-09-01

    Previously the /sup 35/Cl NQR spectra of complexes of the chlorides of Pt, Pd, and Au, as well s the chlorides of Al, Ga, Nb, and Ta, with the chlorides of S, Se and Te were investigated. In the present work the series of complexes studies have been expanded and the Cl and Br NQR spectra of compounds with the general formula MCl/sub X/.ECl/sub 4/, where M = Al, Ga, Zr, Hf, Ta, Nb, Fe, and Mo are presented. The Raman spectra are known for the series of compounds investigated, and according to them the complexes have the structure m(ECl/sub 3//sup +/)(MCl/sub X//sup -n/) (E = S, Se, Te). According to the NQR spectra studied, an ECl/sub 3/ grouping (E = S, Se, Te) is coordinated as a ligand in most of the coordination compounds investigated. The complexes have the composition MCl/sub n/.mECl/sub 3/.

  15. The NQR observation of spin-Peierls transition in an antiferromagnetic MX-chain complex [NiBr(chxn)2]Br2.

    PubMed

    Takaishi, Shinya; Tobu, Yasuhiro; Kitagawa, Hiroshi; Goto, Atsushi; Shimizu, Tadashi; Okubo, Takashi; Mitani, Tadaoki; Ikeda, Ryuichi

    2004-02-18

    81Br Nuclear quadrupole resonance (NQR) measurement was performed in an S = 1/2 one-dimensional Heisenberg antiferromagnetic metal complex [NiBr(chxn)2]Br2 (chxn: 1R,2R-diaminocyclohexane), having a halogen-bridged MX chain structure -Br-Ni3+-Br-Ni3+-Br-. Two 81Br NQR signals were observed below 40 K, while a single signal was observed above 130 K, showing the presence of two nonequivalent bridging Br sites below 40 K. This NQR result together with previously reported magnetic susceptibility and X-ray results indicate the occurrence of a transition into a spin-Peierls state between 40 and 130 K. This communication reports the first spin-Peierls transition in metal complexes in which pure d electrons contribute to the magnetism. In addition, we demonstrated a new experimental method for studying a spin-Peierls system.

  16. Correlation of /sup 35/Cl NQR frequencies with the populations of the p orbitals of the chlorine atom in molecules of organic, organosilicon, and inorganic chlorinated derivatives

    SciTech Connect

    Feshin, V.P.; Nikitin, P.A.; Voronkov, M.G.

    1985-09-01

    The method of nuclear quadrupole resonance (NQR) provides unique information on the spatial distribution of the electron density of the test atom. This paper attempts to confirm the theoretically established relationship between Cl 35 NQR frequencies and the features of the distribution of the electron density of the Cl atom in its compounds by another method. The authors carried out quantum-mechanical calculations in the CNDO/2 approximation in an all-valence sp basis for a number of organic, organometallic, and inorganic chlorinated derivatives. A comparison of the linear plots corresponding to the correlation equations and the empirical expressions for the molecules of the XC1 series are shown.

  17. Correlation of /sup 35/Cl NQR frequencies with chlorine-atom p-orbital populations and charges in organic, silicoorganic, and inorganic chlorides

    SciTech Connect

    Feshin, V.P.; Nikitin, P.A.; Voronkov, M.G.

    1986-07-01

    SCF MOLCAO calculations in the CNDO/2 approximation (valency sp basis) are presented for organic, heteroorganic, and inorganic chlorine compounds in the XCl series. Satisfactory correlations are obtained between the calculated charges on the Cl atoms, the populations of the psigma orbitals, and the numbers of unbalanced electrons on the one hand with the observed /sup 35/Cl NQR frequencies for the corresponding compounds in the XX'X''CCl and XCl series. These indicate that the Townes-Daly approximation in NQR spectroscopy is completely applicable even in the quantitative evaluation of chlorine-atom electron-density distributions in molecules.

  18. 35Cl-NQR and DFT study of electronic structure of amlodipine and felodipine vascular-selective drugs from the dihydropyridine Ca ++ antagonists group

    NASA Astrophysics Data System (ADS)

    Latosińska, J. N.; Latosińska, M.; Kasprzak, J.

    2008-09-01

    Amlodipine (AM) and felodipine (FL) have been studied in solid state by the nuclear quadrupole resonance (NQR) and density functional theory (DFT). The results have shown that NQR data do not permit a differentiation between R and S enantiomers, which is a consequence of the symmetry of the 4-aryl ring, whereas they permit a differentiation between free bases and salts. The HOMO-LUMO gap is smaller for AM than for FL, which suggests smaller energy of excitation for AM. The absolute hardness, chemical potential and electrophilicity of both AM enantiomers are lower than the corresponding values for FL enantiomers, suggesting that AM should be more reactive than FL in unimolecular reactions.

  19. Renal transplant NMR

    SciTech Connect

    Velchik, M.G.; Kressel, H.; Thickman, D.; Alavi, A.

    1985-05-01

    The preliminary results of NMR evaluation of renal transplants (Txs) are reported including correlation with nuclear medicine (NM) and ultrasound (US). Thirteen Txs (8 cadaver (Cd), 5 living related doner (LRD) in 13 patients (6M, 7F) ranging in age from 25-47 (x 35) were evaluated by NM (32), NMR (15) and US (5). Clinical diagnoses included: rejection (8), ATN (2), infarction (1), and normal (2). Of the 8 patients with rejection (5) Cd; 3 LRD) pathologic proof was obtained in 3. An experimental 0.12 T resistive magnet (GE) was used with a partial saturation technique with repetition time (TR) of 143 and 286 msec to provide T1 weighting. T2 weighted information was obtained with a spin echo technique with echo times (TE) of 20, 40, 60 and 80 msec. The NMR appearance of normal Txs consisted of a uniform signal intensity (Tx> pelvic musculature), well-defined internal architecture with good cortical medullary differentiation and normal appearing vessels. The NMR appearance of abnormal transplants consisted of a heterogeneous or overall decrease in signal intensity (kidney muscle) with poor cortical medullary differentiation with or without a halo of decreased signal intensity. Although NMR was able to differentiate normal from abnormal, it was unable to clearly discriminate between ATN and rejection. Advantages of NMR included the ability to demonstrate regional anatomy, vasculature, post operative fluid collections and hematomas, and associated avascular necrosis of the hips.

  20. Pressure-temperature phase diagram in Ce2RhIn8 studied by In-NQR measurements

    NASA Astrophysics Data System (ADS)

    Yashima, M.; Taniguchi, S.; Miyazaki, H.; Mukuda, H.; Kitaoka, Y.; Shishido, H.; Settai, R.; Ōnuki, Y.

    2010-01-01

    We present a phase diagram for the antiferromagnetism and superconductivity in Ce2RhIn8 probed by In-NQR studies under pressure (P). The quasi-2D character of antiferromagnetic spin fluctuations in the paramagnetic state at P = 0 evolves into a 3D character because of the suppression of antiferromagnetic order for P > PQCP ~ 1.36 GPa (QCP: antiferromagnetic quantum critical point). Nuclear-spin-lattice-relaxation rate 1/T1 measurements revealed that the superconducting order occurs in the P range 1.36 - 1.84 GPa, with maximum Tc ~ 0.9 K (PQCP ~ 1.36 GPa).

  1. Study of quasistationary and stationary states in the short-repetition-time sequences in the NQR of nitrogen.

    PubMed

    Mikhaltsevitch, V T; Rudakov, T N

    2004-01-01

    Experimental and theoretical study of quasistationary and stationary states that are established in the quadrupolar spin system subjected to the steady-state sequences which consist of a chain of identical pulses and can be preceded by a preparatory pulse. We have obtained theoretical expressions for the magnetisation of the spin system that take into account off-resonance conditions during the effect of the pulses. Frequency dependencies of the NQR signal in the quasistationary and stationary states are shown for C3H6N6O6 (RDX) and NaNO2, and compared with theoretical results.

  2. NQR experiments on Sc-Y alloys at very low temperatures. [Absolute thermometry below 500[mu]K

    SciTech Connect

    Pollack, L.; Smith, E.N.; Richardson, R.C. )

    1992-10-01

    The authors performed Nuclear Quadrupole Resonance (NQR) experiments on an alloy of scandium and yttrium. They find that the characteristic resonance frequencies in zero external field are 50% larger than in pure scandium. This increase in frequency makes the Sc-Y alloy a better candidate for absolute thermometry below 500 [mu]K. However, the spin-lattice relaxation time of this alloy is more than an order of magnitude longer than in the pure scandium. In addition, an abrupt increase in the Korringa constant was observed for temperatures below 5mK.

  3. Combining Fourier transform nuclear quadrupole resonance (FT-NQR) spectroscopy and mass spectrometry (MS) to study the electronic structure of titanocene dichlorides.

    PubMed

    Kubišta, Jiří; Civiš, Martin; Spaněl, Patrik; Civiš, Svatopluk

    2012-03-21

    A combination of nuclear quadrupole resonance spectroscopy (NQR) and mass spectrometry (MS) has been used to observe trends in electronic structure in three titanocenes: bis(cyclopentadienyl) titanium dichloride (η(5)-C(5)H(5))(2)TiCl(2), bis(pentamethylcyclopentadienyl) titanium dichloride (η(5)-C(5)(CH(3))(5))(2)TiCl(2) and dimethylsilylene-bridged ansa bis(cyclopentadienyl) titanium dichloride Si(CH(3))(2)(η(5)-C(5)H(5))(2)TiCl(2). Using MS, electron ionisation mass spectra of these compounds are presented within the context of the entire homologous series with one to five methyl groups on each cyclopentadienyl ligand. A dedicated NQR spectrometer was constructed for this study with a sensitivity sufficient to precisely determine the NQR resonant frequency of (35)Cl atoms using 3 g samples of these titanocenes. The observed frequencies are thus 11.784, 11.930 and 10.863 MHz at 298 K. The results demonstrate that NQR using a relatively simple apparatus can be used as a sensitive and cost effective probe into the molecular structure of organometallic chlorides, which complements the information inferred from the mass spectra.

  4. Temperature- and pressure-dependent study of 35Cl NQR frequency and spin lattice relaxation time in 2,3-dichloroanisole.

    PubMed

    Ramu, L; Ramesh, K P; Ramananda, D; Chandramani, R

    2010-08-01

    The temperature and pressure dependence of (35)Cl NQR frequency and spin lattice relaxation time (T(1)) were investigated in 2,3-dichloroanisole. Two NQR signals were observed throughout the temperature and pressure range studied. T(1) were measured in the temperature range from 77 to 300 K and from atmospheric pressure to 5 kbar. Relaxation was found to be due to the torsional motion of the molecule and also reorientation of motion of the CH(3) group. T(1) versus temperature data were analyzed on the basis of Woessner and Gutowsky model, and the activation energy for the reorientation of the CH(3) group was estimated. The temperature dependence of the average torsional lifetimes of the molecules and the transition probabilities were also obtained. NQR frequency shows a nonlinear behavior with pressure, indicating both dynamic and static effects of pressure. The pressure coefficients were observed to be positive for both the lines. A thermodynamic analysis of the data was carried out to determine the constant volume temperature coefficients of the NQR frequency. The variation of spin lattice time with pressure was very small, showing that the relaxation is mainly due to the torsional motions of the molecules. 2010 John Wiley & Sons, Ltd.

  5. NMR imaging microscopy

    SciTech Connect

    Not Available

    1986-10-01

    In the past several years, proton nuclear magnetic resonance (NMR) imaging has become an established technique in diagnostic medicine and biomedical research. Although much of the work in this field has been directed toward development of whole-body imagers, James Aguayo, Stephen Blackband, and Joseph Schoeninger of the Johns Hopkins University School of Medicine working with Markus Hintermann and Mark Mattingly of Bruker Medical Instruments, recently developed a small-bore NMR microscope with sufficient resolution to image a single African clawed toad cell (Nature 1986, 322, 190-91). This improved resolution should lead to increased use of NMR imaging for chemical, as well as biological or physiological, applications. The future of NMR microscopy, like that of many other newly emerging techniques, is ripe with possibilities. Because of its high cost, however, it is likely to remain primarily a research tool for some time. ''It's like having a camera,'' says Smith. ''You've got a way to look at things at very fine levels, and people are going to find lots of uses for it. But it is a very expensive technique - it costs $100,000 to add imaging capability once you have a high-resolution NMR, which itself is at least a $300,000 instrument. If it can answer even a few questions that can't be answered any other way, though, it may be well worth the cost.''

  6. 14N NQR Studies of Impurity Effects on the Local Structure of NaNO2 -based Mixed Systems

    NASA Astrophysics Data System (ADS)

    Song, S. K.; Park, Y. M.; Jung, J. K.; Seo, Y. M.; Choh, S. H.

    2000-02-01

    The influence of impurities on the 14N NQR lineshape of Na1-xAgxNO2 and [NaNO2]1-x-[BNO3]x (B = Na, K) at room temperature has been investigated. Carrying out spectral analysis in conjunction with classification of the local field inhomogeneities according to the structurally isomorphic, Na1-xAgxNO2 , and anisomorphic [NaNO2]1-x[BNO3]x systems, enabled an under-standing of the microscopic nature of impurity-induced local disorder. The iso-and anisomorphic systems reveal their own unique features of the impurity induced local disorder. They are charac-terized by a static, random distribution of impurities in the isomorphic system and a fast motion of the impurity-induced mobile point defects in the anisomorphic system. However, for both systems, neither a change of the 14N NQR frequency nor a multisplitting of the lines is observed because of the relatively low symmetry.

  7. Superconducting state of filled-skutterudite RPt4Ge12 (R = La, Pr): 73Ge-NQR studies

    NASA Astrophysics Data System (ADS)

    Kanetake, F.; Mukuda, H.; Kitaoka, Y.; Sugawara, H.; Magishi, K.; Itoh, K. M.; Haller, E. E.

    2010-12-01

    We report 73Ge-NQR studies on filled-skutterudite superconductors LaPt4Ge12 and PrPt4Ge12 under zero external field. In PrPt4Ge12, the measurement of the nuclear spin-lattice relaxation rate 1/T1 has revealed a distinct coherence peak just below Tc followed by an exponential decrease well below Tc, evidencing that PrPt4Ge12 is an s-wave superconductor with the isotropic gap in a weak-coupling regime. In LaPt4Ge12, the 1/T1 exhibits the exponential decrease well below Tc, suggesting the isotropic s-wave superconductivity. Even though 73Ge-NQR-1/T1 in LaPt4Ge12 has been measured under zero field, its coherence peak was absent, which contrasts with the result in Pr-compound. This may point to a possible anisotropy in the Fermi surface and/or some damping effect of quasiparticles in association with electron-phonon interactions.

  8. Central role of the Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR) in sodium bioenergetics of Vibrio cholerae.

    PubMed

    Steuber, Julia; Halang, Petra; Vorburger, Thomas; Steffen, Wojtek; Vohl, Georg; Fritz, Günter

    2014-12-01

    Vibrio cholerae is a Gram-negative bacterium that lives in brackish or sea water environments. Strains of V. cholerae carrying the pathogenicity islands infect the human gut and cause the fatal disease cholera. Vibrio cholerae maintains a Na(+) gradient at its cytoplasmic membrane that drives substrate uptake, motility, and efflux of antibiotics. Here, we summarize the major Na(+)-dependent transport processes and describe the central role of the Na(+)-translocating NADH:quinone oxidoreductase (Na(+)-NQR), a primary Na(+) pump, in maintaining a Na(+)-motive force. The Na(+)-NQR is a membrane protein complex with a mass of about 220 kDa that couples the exergonic oxidation of NADH to the transport of Na(+) across the cytoplasmic membrane. We describe the molecular architecture of this respiratory complex and summarize the findings how electron transport might be coupled to Na(+)-translocation. Moreover, recent advances in the determination of the three-dimensional structure of this complex are reported.

  9. 35Cl NQR spectra of phosphorus chlorides and their molecular conformations in crystals. Part 1. Phosphorus (III) chlorides RPCl 2

    NASA Astrophysics Data System (ADS)

    Kozlov, E. S.; Kapustin, E. G.; Soifer, G. B.

    2000-09-01

    For the phosphorus chlorides RPCl 2 (R=Cl, Me, ClCH 2, CF 3, Et, i-Pr, Me 2C=CH, PhCH=CH, Me 2N, Et 2N, Pr 2N, MeO, PhO) and R'PCl 2 (R'=Ar, 2-thienyl) two linear correlations between the 35Cl NQR frequencies and charges on the chlorine atoms of the PCl 2 groups calculated by the MNDO procedure have been found. It was shown that the 35Cl NQR spectra and the relative magnitudes of the charges on the chlorine atoms of the PCl 2 groups can be used to determine conformation of the RPCl 2 molecules in crystal. Ab initio (RHF/6-31 G ∗ and MP2/6-31 G ∗) calculations showed that the gauche conformation of Me 2NPCl 2 molecule is more stable than trans conformation. In light of ab initio calculations electron diffraction results (Vilkov L.V., Khaikin L.S., Dokl. Akad. Nauk SSSR, 168 (1966) 810) are erroneous. The NBO analysis confirmed the presence of donor-acceptor interactions between the lone pair orbital of the nitrogen atom and the antibonding orbitals of the P-Cl bonds.

  10. 35Cl NQR and Structural Studies of Chloroacetanilides C6H3Cl2NHCOCH3-xClx, 1 ≤ x ≤ 3

    NASA Astrophysics Data System (ADS)

    Groke, Dirk; Dou, Shi-Qi; Weiss, Alarich

    1992-02-01

    The temperature dependence of 35Cl NQR frequencies and the phase transition behaviour of chloroacetanilides (N-[2,6-dichlorophenyl]-2-chloroacetamide, -2,2-dichloroacetamide, -2,2,2-trichloroacetamide) were investigated. The crystal structure determination of N-[2,6-dichlorophenyl]- 2-chloroacetamide leads to the following: a = 1893.8 pm, b = 1110.7 pm, c = 472.1 pm, space group P212121 = D24 with Z = 4 molecules per unit cell. The arrangement of the molecules and their geometry is comparable to the high temperature phase of the acetyl compound N-[2,6-dichlorophenyl]- acetamide. For N-[2,6-diclorophenyl]-2,2,2-trichloroacetamide it was found: a = 1016.6 pm, b = 1194.3 pm, c = 1006.7 pm, ß= 101.79°, space group P21/c = C52h, Z = 4. The structure is similar to the low temperature phase of N-[2,6-dichlorophenyl]-acetamide. Parallelism between the temperature dependence of the 35C1 NQR lines of the CCl3 group and the X-ray diffraction results concerning the different behaviour of the chlorine atoms was observed. The structures of the compounds show intermolecular hydrogen bonding of the N - H • • • O - C type. The phenyl group and the HNCO function are nearly planar. A bleaching out of several 35Cl NQR lines at a temperature far below the melting point of the substances was observed. The different types of chlorine atoms (aromatic, chloromethyl) can be distinguished by their temperature coefficients of the 35Cl NQR frequencies. All the resonances found show normal "Bayer" temperature behaviour. N-[2,6-dichlorophenyl]-2,2-diehloroacetamide shows several solid phases. One stable low temperature phase and an instable high temperature phase (at room temperature) were observed. The different phases were detected by means of 35Cl NQR spectroscopy and thermal analysis

  11. Optimizing Adiabaticity in NMR

    NASA Astrophysics Data System (ADS)

    Vandermause, Jonathan; Ramanathan, Chandrasekhar

    We demonstrate the utility of Berry's superadiabatic formalism for numerically finding control sequences that implement quasi-adiabatic unitary transformations. Using an iterative interaction picture, we design a shortcut to adiabaticity that reduces the time required to perform an adiabatic inversion pulse in liquid state NMR. We also show that it is possible to extend our scheme to two or more qubits to find adiabatic quantum transformations that are allowed by the control algebra, and demonstrate a two-qubit entangling operation in liquid state NMR. We examine the pulse lengths at which the fidelity of these adiabatic transitions break down and compare with the quantum speed limit.

  12. Shiftless NMR Spectroscopy

    PubMed Central

    Wu, Chin H.; Opella, Stanley J.

    2013-01-01

    The acquisition and analysis of high resolution one- and two- dimensional solid-state NMR spectra without chemical shift frequencies are described. Many variations of Shiftless NMR spectroscopy are feasible. A two-dimensional experiment that correlates 13Cα-15N dipole-dipole and 1H-13Cα dipole-dipole couplings in single crystal and powder samples of the model peptide, 13Cα, 15N-acetylleucine, 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. PMID:18266429

  13. Modern NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Jelinski, Lynn W.

    1984-01-01

    Discusses direct chemical information that can be obtained from modern nuclear magnetic resonance (NMR) methods, concentrating on the types of problems that can be solved. Shows how selected methods provide information about polymers, bipolymers, biochemistry, small organic molecules, inorganic compounds, and compounds oriented in a magnetic…

  14. Modern NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Jelinski, Lynn W.

    1984-01-01

    Discusses direct chemical information that can be obtained from modern nuclear magnetic resonance (NMR) methods, concentrating on the types of problems that can be solved. Shows how selected methods provide information about polymers, bipolymers, biochemistry, small organic molecules, inorganic compounds, and compounds oriented in a magnetic…

  15. Autonomous driving in NMR.

    PubMed

    Perez, Manuel

    2017-01-01

    The automatic analysis of NMR data has been a much-desired endeavour for the last six decades, as it is the case with any other analytical technique. This need for automation has only grown as advances in hardware; pulse sequences and automation have opened new research areas to NMR and increased the throughput of data. Full automatic analysis is a worthy, albeit hard, challenge, but in a world of artificial intelligence, instant communication and big data, it seems that this particular fight is happening with only one technique at a time (let this be NMR, MS, IR, UV or any other), when the reality of most laboratories is that there are several types of analytical instrumentation present. Data aggregation, verification and elucidation by using complementary techniques (e.g. MS and NMR) is a desirable outcome to pursue, although a time-consuming one if performed manually; hence, the use of automation to perform the heavy lifting for users is required to make the approach attractive for scientists. Many of the decisions and workflows that could be implemented under automation will depend on the two-way communication with databases that understand analytical data, because it is desirable not only to query these databases but also to grow them in as much of an automatic manner as possible. How these databases are designed, set up and the data inside classified will determine what workflows can be implemented. Copyright © 2016 John Wiley & Sons, Ltd.

  16. Simultaneously cycled NMR spectroscopy.

    PubMed

    Parish, David M; Szyperski, Thomas

    2008-04-09

    Simultaneously cycled (SC) NMR was introduced and exemplified by implementing a set of 2-D [1H,1H] SC exclusive COSY (E.COSY) NMR experiments, that is, rf pulse flip-angle cycled (SFC), rf pulse phase cycled (SPC), and pulsed field gradient (PFG) strength cycled (SGC) E.COSY. Spatially selective 1H rf pulses were applied as composite pulses such that all steps of the respective cycles were affected simultaneously in different slices of the sample. This increased the data acquisition speed for an n-step cycle n-fold. A high intrinsic sensitivity was achieved by defining the cycles in a manner that the receiver phase remains constant for all steps of the cycle. Then, the signal resulting from applying the cycle corresponded to the sum of the signals from all steps of the cycle. Hence, the detected free induction decay did not have to be separated into the contributions arising from different slices, and read-out PFGs, which not only greatly reduce sensitivity but also negatively impact lineshapes in the direct dimension, were avoided. The current implementation of SFC E.COSY reached approximately 65% of the intrinsic sensitivity of the conventional phase cycled congener, making this experiment highly attractive whenever conventional data acquisition is sampling limited. Highly resolved SC E.COSY yielding accurate 3J-coupling values was recorded for the 416 Da plant alkaloid tomatidine within 80 min, that is, 12 times faster than with conventional phase cycled E.COSY. SC NMR is applicable for a large variety of NMR experiments and thus promises to be a valuable addition to the arsenal of approaches for tackling the NMR sampling problem to avoid sampling limited data acquisition.

  17. 224} studied by NMR

    SciTech Connect

    Furukawa, Y; Fang, X; Kögerler, P

    2014-05-14

    7Li nuclear magnetic resonance (NMR) studies have been performed to investigate magnetic properties and spin dynamics of Mn3+ (S = 2) spins in the giant polyoxometalate molecule {Mn40W224}. The 7Li-NMR line width is proportional to the external magnetic field H as expected in a paramagnetic state above 3 K. Below this temperature the line width shows a sudden increase and is almost independent of H, which indicates freezing of the local Mn3+ spins. The temperature dependence of T1 for both 1H and 7Li reveals slow spin dynamics at low temperatures, consistent with spin freezing. The slow spin dynamics is also evidenced by the observation of a peak of 1/T2 around 3 K, where the fluctuation frequency of spins is of the order of ~200 kHz. An explicit form of the temperature dependence of the fluctuation frequency of Mn3+ spins is derived from the nuclear relaxation data.

  18. NMR imaging of materials

    SciTech Connect

    Vinegar, H.J.; Rothwell, W.P.

    1988-03-01

    A method for obtaining at least one petrophysical property of a porous material containing therein at least one preselected fluid, is described, comprising: NMR imaging the material to generate signals dependent upon both M(0) and T/sub 1/ and M(0) and T/sub 2/, generating separate M(0), T/sub 1/ and T/sub 2/ images from the signals, and determining at least one petrophysical property from at least one of the images.

  19. NMR Studies of Peroxidases.

    NASA Astrophysics Data System (ADS)

    Veitch, Nigel Charles

    Available from UMI in association with The British Library. Requires signed TDF. Peroxidases are a haem-containing group of enzymes with a wide diversity of function within biological systems. While a common characteristic is the ability to catalyse the conversion of hydrogen peroxide to water, it is the accompanying processes of hormone synthesis and degradation which have generated such a high level of interest. However, information at the molecular level is limited to a single well-resolved crystal structure, that of yeast cytochrome c peroxidase. This thesis presents a strategy for the investigation of peroxidase structure and function based on proton nuclear magnetic resonance spectroscopy, a technique which has the ability to address aspects of both protein structure and protein dynamics in solution. The application of one- and two-dimensional NMR techniques has been developed in the context of plant peroxidases, notably the isoenzyme HRP-C derived from the horseradish root. Characterisation of the proton NMR spectra of HRP -C in resting and ligated states provided new information enabling the structure of the binding site for aromatic donor molecules, such as indole-3-propionic, ferulic and benzhydroxamic acids, to be resolved. In order to overcome difficulties encountered with a protein of the complexity of peroxidase, additional information was obtained from chemical shift parameters and the use of peroxidase variants produced by site-directed mutagenesis. A comparative study using NMR spectroscopy was undertaken for wild-type recombinant HRP-C expressed in Escherichia coli, and two protein variants with substitutions made to residues located on the distal side of the haem pocket, Phe41 to Val and Arg38 to Lys. NMR analyses of a plant peroxidase from barley grains and the fungal peroxidase from Coprinus cinereus were also successful using methods conceived with HRP-C. Examination of three specifically constructed recombinant protein variants of C. cinereus

  20. A model to describe the inhomogeneous broadening of NQR lines in chlorohalobenzenes with orientational or substitutional disorder.

    PubMed

    Pérez, Silvina C; Zuriaga, Mariano

    2017-06-20

    A simple model to explain the NQR lineshape in solids with orientational disorder or substitutional disorder is presented. The particular case of m-chlorobromobenzene is studied. It is based on the assumption that Bromine atoms, of m-chlorobromobenzene molecules, behave as point defects in the m-dichlorobenzene lattice that modify the crystalline Electric Field Gradient. The model is also tested successfully in solid solutions of p-dichlorobenzene-p-dibromobenzene, where Bromine atoms of p-dibromobenzene molecules are assumed to be homogeneously distributed in the p-dichlorobenzene lattice. The lineshape, of others disordered chlorohalobenzenes, are also analyzed. Also, a characterization of m-chlorobromobenzene dynamics is included. In particular, there is no evidence of molecular reorientations as it is observed in the disordered phases of o-chlorobromobenzene. Copyright © 2017 Elsevier Inc. All rights reserved.

  1. Magnetic correlations in La(2-x)Sr(x)CuO4 from NQR relaxation and specific heat

    NASA Technical Reports Server (NTRS)

    Borsa, F.; Rigamonti, A.

    1991-01-01

    La-139 and Cu-63 Nuclear Quadrupole Resonance (NQR) relaxation measurements in La(2-x)Sr(x)CuO4 for x ranging from 0 up to 0.3, with particular emphasis on the effect of doping on the Cu(2+) magnetic correlations and dynamics, are reviewed. In the low doping limit, x less than or equal to 0.05, the results can be interpreted consistently in terms of a simple phenomenological 'two-fluids' model whereby the effect of thermally-activated mobile O(2p) holes is the one of disrupting locally the Cu(2+) spin correlations. For x greater than or equal to 0.1, the results indicate the onset, as T approaches T(sub c)(+), of a strong coupling between Cu(2+) spins and the Fermi liquid of O(2p) holes leading to the apparent disappearance of localized Cu(2+) moment in connection with the opening of a superconducting gap.

  2. Novel superconductivity in CeIr(In1-xCdx)5 studied by In-NQR measurements

    NASA Astrophysics Data System (ADS)

    Yashima, M.; Taniguchi, S.; Tagami, N.; Mukuda, H.; Kitaoka, Y.; Ōta, Y.; Shishido, H.; Settai, R.; Ōnuki, Y.

    2010-01-01

    We report the superconducting characters in CeIrIns studied by In-NQR measurements under pressure (P). In CeCoIn5 and CeRhIn5, the occurrence of superconductivity (SC) is related with the antiferrmagnetic spin fluctuations (AFM-SFs) originating from the antiferromagntic quantum-critical point (AFM-QCP). The high-Tc SC (Tcmax > 2 K) is realized in both compounds. However, in CeIrIn5 which is apart from the AFM-QCP, SC occurs even without AFM-SFs and the quite small value of Tcmax (~ 1 K) is observed around P = 3 GPa. The mechanism of SC in CeIrIn5 may be different from that in CeCoIn5 and CeRhIn5.

  3. Unconventional superconductivity and antiferromagnetic quantum phase transition in CeRhIn5: 115In-NQR study under pressure

    NASA Astrophysics Data System (ADS)

    Yashima, M.; Kawasaki, S.; Mukuda, H.; Kitaoka, Y.; Shishido, H.; Settai, R.; Ōnuki, Y.

    2008-04-01

    We report on the pressure ( P)-induced phase diagram of antiferromagnetism (AFM) and superconductivity (SC) which emerges at their border at zero magnetic field. The nuclear-quadrupole-resonance (NQR) measurements have revealed that AFM can take place in the superconducting state with Tc∼2.1 K at P=2.05 GPa and the AFM quantum phase transition (QPT) occurs near P=2.1 GPa. These results reveal the existence of the tetracritical point in the P- T phase diagram of AFM and SC in CeRnIn5. We also found the gapless nature in the uniformly coexisting phase of AFM and SC, indicating an intimate relationship between AFM and SC.

  4. /sup 35/Cl NQR spectra of the complex AuCl/sub 3/SCl/sub 2/

    SciTech Connect

    Fokina, Z.A.; Lapko, V.F.; Kuznetsov, S.I.; Bryukhova, E.V.

    1987-01-10

    The authors studied the /sup 35/Cl NQR spectra of the complex AuCl/sub 5/S. Of interest is the significant splitting in the region of the Au-Cl spectrum, which indicates nonequivalence of one of the Au-Cl bonds in the AuCl/sub 3/ group; the temperature coefficients of the frequencies also differ. Most probably, this frequency corresponds to the Cl atom, which is in the transposition to the coordinated SCl/sub 2/ group in a distorted planar square configuration, which agrees with the assignment of the frequencies for this structure in the Raman spectra and with the structure of the complex AuCl/sub 3/(SCL/sub 2/) where the Au atom is in the unsymmetrical environment of three Cl atoms and one S atom.

  5. Solvent Effects on Stability, Electronic Structure, and 14N NQR Parameters of Fe(CO)4py Isomers

    NASA Astrophysics Data System (ADS)

    Ghiasi, R.; Peikari, A.

    2017-03-01

    The structure, stability, 14N NQR parameters, and hyperpolarizability of Fe(CO)4py isomers in seven different solvents were computed with the MPW1PW91 method based on the polarizable continuum model (PCM). From an energetic standpoint, the Fe(CO)4pyaxial isomer was more stable than the Fe(CO)4pyequatorial isomer. On the other hand, the relative energies decreased in more polar solvents. Molecular orbital analysis showed that the HOMO of the Fe(CO)4py isomer was distributed on the Fe(CO)4 fragment, whereas the LUMO was localized on the pyridine ligand. This study suggests that the nonlinear optical (NLO) properties depend on the solvent polarity.

  6. β-NMR

    NASA Astrophysics Data System (ADS)

    Morris, Gerald D.

    2014-01-01

    The β-NMR facility at ISAC is constructed specifically for experiments in condensed matter physics with radioactive ion beams. Using co-linear optical pumping, a 8Li + ion beam having a large nuclear spin polarisation and low energy (nominally 30 keV) can be generated. When implanted into materials these ions penetrate to shallow depths comparable to length scales of interest in the physics of surfaces and interfaces between materials. Such low-energy ions can be decelerated with simple electrostatic optics to enable depth-resolved studies of near-surface phenomena over the range of about 2-200 nm. Since the β-NMR signal is extracted from the asymmetry intrinsic to beta-decay and therefore monitors the polarisation of the radioactive probe nuclear magnetic moments, this technique is fundamentally a probe of local magnetism. More generally though, any phenomena which affects the polarisation of the implanted spins by, for example, a change in resonance frequency, line width or relaxation rate can be studied. The β-NMR program at ISAC currently supports a number of experiments in magnetism and superconductivity as well as novel ultra-thin heterostructures exhibiting properties that cannot occur in bulk materials. The general purpose zero/low field and high field spectrometers are configured to perform CW and pulsed RF nuclear magnetic resonance and spin relaxation experiments over a range of temperatures (3-300 K) and magnetic fields (0-9 T).

  7. Soils, Pores, and NMR

    NASA Astrophysics Data System (ADS)

    Pohlmeier, Andreas; Haber-Pohlmeier, Sabina; Haber, Agnes; Sucre, Oscar; Stingaciu, Laura; Stapf, Siegfried; Blümich, Bernhard

    2010-05-01

    Within Cluster A, Partial Project A1, the pore space exploration by means of Nuclear Magnetic Resonance (NMR) plays a central role. NMR is especially convenient since it probes directly the state and dynamics of the substance of interest: water. First, NMR is applied as relaxometry, where the degree of saturation but also the pore geometry controls the NMR signature of natural porous systems. Examples are presented where soil samples from the Selhausen, Merzenhausen (silt loams), and Kaldenkirchen (sandy loam) test sites are investigated by means of Fast Field Cycling Relaxometry at different degrees of saturation. From the change of the relaxation time distributions with decreasing water content and by comparison with conventional water retention curves we conclude that the fraction of immobile water is characterized by T1 < 5 ms. Moreover, the dependence of the relaxation rate on magnetic field strength allows the identification of 2D diffusion at the interfaces as the mechanism which governs the relaxation process (Pohlmeier et al. 2009). T2 relaxation curves are frequently measured for the rapid characterization of soils by means of the CPMG echo train. Basically, they contain the same information about the pore systems like T1 curves, since mostly the overall relaxation is dominated by surface relaxivity and the surface/volume ratio of the pores. However, one must be aware that T2 relaxation is additionally affected by diffusion in internal gradients, and this can be overcome by using sufficiently short echo times and low magnetic fields (Stingaciu et al. 2009). Second, the logic continuation of conventional relaxation measurements is the 2-dimensional experiment, where prior to the final detection of the CPMG echo train an encoding period is applied. This can be T1-encoding by an inversion pulse, or T2 encoding by a sequence of 90 and 180° pulses. During the following evolution time the separately encoded signals can mix and this reveals information about

  8. Stability and molecular dynamics of chloroxylenol (API of antiseptics and drugs) in solid state studied by 35Cl-NQR spectroscopy and DFT calculations

    NASA Astrophysics Data System (ADS)

    Latosińska, J. N.; Tomczak, M. A.; Kasprzak, J.

    2009-02-01

    Thermal stability of 4-chloro-3,5-dimethyl-phenol (chloroxylenol) in solid state has been studied by 35Cl-NQR spectroscopy. Two NQR resonance lines at the frequencies 34.348 and 34.415 MHz at 77 K have been assigned to chlorine atoms from two crystallographically inequivalent molecules on the basis of the B3LYP/6-311++G∗∗ results. The temperature dependence of the resonance frequency and full width at half maximum suggest the occurrence of small-angle torsional oscillations of the mean activation energy of 3.83 kJ/mol and rotation of both methyl groups around their symmetry axis C3 with the activation energies 12.49 and 11.27 kJ/mol for CH3 in molecule A and B, respectively. B3LYP/6-311++G∗∗ method reproduced very well the activation energies of both motions.

  9. Studies of the electronic structure and biological activity of chosen 1,4-benzodiazepines by 35Cl NQR spectroscopy and DFT calculations

    NASA Astrophysics Data System (ADS)

    Bronisz, K.; Ostafin, M.; Poleshchuk, O. Kh.; Mielcarek, J.; Nogaj, B.

    2006-11-01

    Selected derivatives of 1,4-benzodiazepine: lorazepam, lormetazepam, oxazepam and temazepam, used as active substances in anxiolytic drugs, have been studied by 35Cl NQR method in order to find the correlation between electronic structure and biological activity. The 35Cl NQR resonance frequencies ( νQ) measured at 77 K have been correlated with the following parameters characterising their biological activity: biological half-life period ( t0.5), affinity to benzodiazepine receptor (IC 50) and mean dose equivalent. The results of experimental study of some benzodiazepine derivatives by nuclear quadrupole resonance of 35Cl nuclei are compared with theoretical results based on DFT calculations which were carried out by means of Gaussian'98 W software.

  10. Determination of the electric field gradient asymmetry from 2D nutation NQR spectra of 75As nuclei in oriented samples of As2Se3 semiconductor.

    PubMed

    Korneva, I; Ostafin, M; Sinyavsky, N; Nogaj, B; Maćkowiak, M

    2007-05-01

    The method of two-dimensional nutation nuclear quadrupole resonance in time domain is used to study the chalcogenide semiconductor As(2)Se(3). In this system, the nuclear quadrupole resonance (NQR) resonance line width is as large as 10 MHz; therefore, the radiofrequency field produced by a pulsed NQR spectrometer can excite only a portion of the nuclear spins. The proposed method relies on polarizing the melted glass specimen in a strong magnetic field so that orientational disorder is partially removed. After hardening the sample is placed in a spectrometer r.f. coil in such a way that that the axes of sample polarization and r.f. coil coincide. We demonstrate the application of this method to determine eta in glassy As(2)Se(3).

  11. 127I NQR and spectroscopic investigation of impurity-doped and mixed lithium iodate Li 1- xH xIO 3 crystals

    NASA Astrophysics Data System (ADS)

    Barabash, A.; Gavrilko, T.; Eshimov, K.; Baran, J.; Ratajczak, H.

    2004-12-01

    The 127I NQR, IR absorption and Raman spectra of impurity-doped and mixed lithium iodate Li 1- xH xIO 3 crystals grown from water solutions with different LiIO 3/HIO 3 ratios were investigated depending on the content of the impurity hydrogen x. The NQR results suggested that, at small concentration of doping iodic acid x<0.22, the lattice dynamics of the crystal grown from water solution changes significantly though the crystal retains hexagonal symmetry. Spectroscopic studies are compatible with average hexagonal symmetry of the grown doped crystals. From the results of Raman studies at room temperature and 100 K, the concentration range of hydrogen dopant 0.22< x<0.36 was found where disordered solid solution crystals Li 1- xH xIO 3 are formed.

  12. Rectangle Surface Coil Array in a Grid Arrangement for Resonance Imaging

    DTIC Science & Technology

    2016-02-13

    switchable array, RF magnetic field, NQR, MRI, NMR , tuning, decoupling I. INTRODUCTION ESONANCE imaging can be accomplished using Nuclear Magnetic...Resonance ( NMR ) or Nuclear Quadrupole Resonance (NQR) techniques. REF [1] and [6] explain the differences between NMR and NQR. What NMR and NQR...4. Ohliger, M. “An introduction to coil array design for parallel MRI” NMR IN BIOMEDICINE NMR Biomed. 2006; 19: 300–315 Published online in Wiley

  13. 35Cl NQR study of lattice dynamic and magnetic property of a crystalline coordination polymer {CuCA(phz)(H 2O) 2} n

    NASA Astrophysics Data System (ADS)

    Gotoh, Kazuma; Terao, Takeshi; Asaji, Tetsuo

    2007-01-01

    Copper(II) compounds {CuCA(phz)(H 2O) 2} n (H 2CA = chloranilic acid, phz = phenazine) having a layer structure of -CuCA(H 2O) 2- polymer chains and phenazine were studied by 35Cl nuclear quadrupole resonance (NQR). The single NQR line observed at 35.635 MHz at 261.5 K increased to 35.918 MHz at 4.2 K. The degree of reduction of electric field gradient due to lattice vibrations was similar to that of chloranilic acid crystal. Temperature dependence of spin-lattice relaxation time, T1, of the 35Cl NQR signal below 20 K, between 20 and 210 K, and above 210 K, was explained by (1) a decrease of effective electron-spin density caused by antiferromagnetic interaction, (2) a magnetic interaction between Cl nuclear-spin and electron-spins on paramagnetic Cu(II) ions, and (3) an increasing contribution from reorientation of ligand molecules, respectively. The electron spin-exchange parameter ∣ J∣ between the neighboring Cu(II) electrons was estimated to be 0.33 cm -1 from the T1 value of the range 20-210 K. Comparing this value with that of J = -1.84 cm -1 estimated from the magnetic susceptibility, it is suggested that the magnetic dipolar coupling with the electron spins on Cu(II) ions must be the principal mechanism for the 35Cl NQR spin-lattice relaxation of {CuCA(phz)(H 2O) 2} n but a delocalization of electron spin over the chloranilate ligand has to be taken into account.

  14. A systematic study on hydrogen bond interactions in sulfabenzamide: DFT calculations of the N-14, O-17, and H-2 NQR parameters.

    PubMed

    Nozad, Ahmad G; Najafi, Hamidreza; Meftah, Sakineh; Aghazadeh, Mustafa

    2009-02-01

    A systematic computational study was carried out to characterize the hydrogen bond, HB, interactions of sulfabenzamide crystal structure by DFT calculations of electric field gradient, EFG, tensors at the sites of 14N, 17O, and 2H nuclei. The computations were performed with the B3LYP and B3PW91 DFT methods and 6-311+G and 6-311++G* standard basis sets using the Gaussian 98 package. To perform the calculations, a hydrogen-bonded heptameric cluster of sulfabenzamide was created by X-ray coordinates where the hydrogen atom positions were optimized and the EFG tensors were calculated for the target molecule. Additional optimization and EFG calculations were also performed for crystalline monomer and an isolated gas-phase sulfabenzamide. The calculated EFG tensors were converted to the experimentally measurable nuclear quadrupole resonance, NQR, parameters: quadrupole coupling constant, C(Q), and asymmetry parameter, eta(Q). The results reveal that the geometrical and NQR parameters of the optimized isolated gas-phase and crystalline phase are different. In addition, the difference between the calculated NQR parameters of the monomer and the target molecule shows how much H-bonding interactions affect the EFG tensors of each nucleus. The evaluated NQR parameters reveal that due to the contribution of the target molecule to N-H...O and C-H...O hydrogen bond interactions, the EFG tensors at the sites of N1, O3 and H1 undergo significant changes from monomer to the target molecule in cluster. These features reveal the major role of N-H...O type intermolecular HBs in cluster model of sulfabenzamide which the presence of these interactions can lead to polymorphism directly related to the drug activity and related properties.

  15. X-Ray and 35Cl NQR Studies on the Trichloroacetyl Group in Covalent and Ionic Compounds of L-Valine and DL-Valine

    NASA Astrophysics Data System (ADS)

    Ofial, A. R.; Dou, S.-q.; Krishnan, V. G.; Paulus, H.; Fuess, H.; Weiss, Al.

    1997-03-01

    The crystal structures and 35Cl NQR of trichloroacetyl-DL-valine (1), trichloroacetyl-L-valine (2), as well as the salts of trichloroacetic acid with DL-valine (3) and L-valine (4) have been investigated. Crystal data are for (1): Monoclinic, C2/c, a= 15.835(4) Å, b= 10.481 (3) Å, c = 14.046(4) Å, β = 103.28(1), Z = 8; (2): Orthorhombic, P212121, a = 12.117(3) Å, 6=10.896(3) Å, c= 8.718(2) Å, Z = 4; (3): Triclinic, P1¯, a= 17.269(3) Å, 6 = 8.504(3) Å, c = 10.427(4) A, a = 105.38(2), β = 96.98(2), γ = 96.24(2), Z = 2; (4): Monoclinic, P21, a = 10.378(4) Å, b = 20.349(8) Å, c= 11.890(5) Å, β = 95.28(2), Z = 8. The onset of rotational motion within the trichloroacetyl groups bleaches out 35Cl NQR lines between 115 K and 185 K for (1)-(4). While TCA-L-valine (1), TCA-DL-valine (2), and TCA(-) · DL-valine(+) (3) do not show any phase transition in the temperature range 77 K to 295 K, TCA(-) · L-valine(+) (4) shows more than one phase transition above 77 K before the three NQR signals bleach out at 164 K.

  16. NQR study of local structures and cooling rate dependent superconductivity in La{sub 2}CuO{sub 4+{delta}}

    SciTech Connect

    Reyes, A.P.; Ahrens, E.T.; Hammel, P.C.; Heffner, R.H.; Thompson, J.D.; Canfield, P.C.; Fisk, Z.; Schirber, J.E.

    1992-10-01

    Structural properties of oxygen-annealed polycrystals of La{sub 2}CuO{sub 4 + {delta}} ({delta}{approximately}0.03) have been studied using {sup 139}La NQR spectroscopy. Superconducting critical temperatures were found to depend on the rate of cooling through a narrow temperature range at about 195K. Preliminary analysis of the {sup 139}La NQR spectra suggest that the oxygen-rich phase-separated region is composed of two structurally distinct phases, both of which are metallic and super-conducting. One phase has a structure closely related to the stoichiometric oxygen-poor compound. The second shows a considerable amount of apical oxygen disorder, a large shift in NQR frequency {nu}{sub Q}, and a volume fraction which increases with cooling rate. The formation of the second phase below {minus}200K is indicative of the freezing Of CuO{sub 6} octahedral tilting. Abrupt shifts in {nu}{sub Q} above {Tc} were also observed for both phases, suggestive of a local structural anomaly or charge transfer to the Cu-O plane.

  17. NMR in biology and medicine

    SciTech Connect

    Chien, S.; Chien, H.

    1986-01-01

    This volume explores the applications of NMR in basic biological research and in clinical diagnosis. The contributors highlight the capabilities of NMR as a tool for studying living organisms at the molecular and cellular levels and detecting abnormalities in various organ systems. Included are solid-state and high-resolution NMR studies of the molecular structure and dynamic interactions of lipids, proteins, and nucleic acids. The latest developments in NMR zeugmatographic imaging and in musculoskeletal and cardiovascular magnetic resonance imaging are detailed. Concluding chapters review the uses of in vivo NMR spectroscopy to study energy metabolism and cellular biochemistry. Emphasis is placed on in vivo NMR spectroscopy studies that elucidate normal metabolic functions and their pathological disturbances.

  18. NMR imaging of the spine

    SciTech Connect

    Han, J.S.; Kaufman, B.; El Yousef, S.J.; Benson, J.E.; Bonstelle, C.T.; Alfidi, R.J.; Haaga, J.R.; Yeung, H.; Huss, R.G.

    1983-12-01

    The usefulness of nuclear magnetic resonance (NMR) images in the evaluation of spinal disorders below the craniocervical junction was studied. Six normal subjects and 41 patients with various spinal abnormalities were examined. NMR proved capable of demonstrating important normal and pathologic anatomic structures; it was useful in the evaluation of syringohydromyelia and cystic spinal cord tumors, and the bright signal intensity of lipoma was quite impressive. In the evaluation of herniated disk, NMR images offered a new perspective by visualizing abnormal degradation of the signal intensity of the nucleus pulposus itself. NMR images were least valuable in the evaluation of spondylosis and spinal stenosis. Although NMR imaging of the spine is still in a very early developmental stage, the absence of both ionizing radiation and risks associated with contrast material makes it especially attractive as a new diagnostic method. This limited experience with currently available equipment suggests that, with technical refinement, the efficacy of NMR of the spine will increase.

  19. Magic Angle Spinning NMR Metabolomics

    SciTech Connect

    Zhi Hu, Jian

    2016-01-01

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

  20. Intermolecular triple proton and deuteron transfer in crystalline 3,5-dimethylpyrazole studied by NMR, NQR, and x-ray methods

    SciTech Connect

    Wehrle, B.; Aguilar-Parrilla, F.; Limbach, H.H. ); de la Concepcion Foces-Foces, M.; Cano, F.H. ); Elguero, J. ); Baldy, A.; Pierrot, M. ); Khurshid, M.M.T.; Larcombe-McDouall, J.B.; Smith, J.A.S. )

    1989-09-13

    A combination of {sup 13}C, {sup 15}N magnetic resonance, {sup 14}N quadrupole double resonance, and x-ray studies of solid 3,5-dimethylpyrazole between 270 and 350 K has shown that the NH...N hydrogen bond units present in the crystal are dynamically disordered, so that each nitrogen atom is on average attached to half a hydrogen atom. The molecules form discrete hydrogen-bonded cyclic trimers, in which the hydrogen atoms move in a double minimum potential energy surface which is symmetrical, to within experimental error. The experimental evidence in this temperature range is consistent with disorder by means of correlated triple hydrogen jumps with an activation energy of 45 kJ mol{sup {minus}1}. There is a large kinetic hydrogen (HHH)/deuterium (DDD) isotope effort of >20 at 299 K and equal to 8 at 347 K.

  1. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, September 14--December 15, 1990

    SciTech Connect

    Not Available

    1991-01-14

    Copper and cobalt are the key elements in syngas conversion catalyst systems used for higher alcohol synthesis. Their proximity and synergy sensitively control the selectivity and efficiency of the process. It is believed that their outer electronic charge distribution which is responsible for their electrical and magnetic properties might be governing their catalytic properties also. To examine the correlation between catalytic and magnetic properties, a series of copper cobalt catalysts (Co/Cu ratio 5:1 to 5:5) with and without a support were prepared. The nuclear quadrupole resonance spectrum of copper and (zero-field) nuclear magnetic resonance spectrum of cobalt and magnetization and hysteresis character of the catalyst were analyzed. Similar to the catalytic results, the magnetic results also were found to be very sensitive to the preparation technique. The results indicate possible electron exchange between copper and cobalt, and cobalt and the support Titania.

  2. Specific features of magnetic order in a multiferroic compound CuCrO2 determined using NMR and NQR data for 63, 65Cu nuclei

    NASA Astrophysics Data System (ADS)

    Smol'nikov, A. G.; Ogloblichev, V. V.; Verkhovskii, S. V.; Mikhalev, K. N.; Yakubovskii, A. Yu.; Furukawa, Y.; Piskunov, Yu. V.; Sadykov, A. F.; Barilo, S. N.; Shiryaev, S. V.

    2017-02-01

    Results of studying the paramagnetic and ordered phases of a CuCrO2 single crystal using nuclear magnetic and nuclear quadrupole resonances on 63,65Cu nuclei are presented. The measurements have been carried out in wide ranges of temperature ( T = 4.2-300 K) and magnetic-field strength ( H = 0-94 kOe), with the magnetic fields being directed along a and c axes of the crystal. The components of the electric-field gradient tensor and the magnetic-shift tensor ( K a,c) have been determined. The temperature dependences K a( H || a) and K c( H || c) for the paramagnetic phase are described by the Curie-Weiss law and reproduce the behavior of the magnetic susceptibility (χa,c). The hyperfine field on a copper nucleus has been determined, which is equal to h hf a,c = 33 kOe/μB. Below the temperature T N = 23.6 K, nuclear magnetic resonance and nuclear quadrupole resonance spectra for 63,65Cu nuclei have been recorded typical of helical magnetic structures, which are incommensurable with the lattice period.

  3. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, March 15--June 15, 1991

    SciTech Connect

    Not Available

    1991-07-15

    The primary objective of the project is to examine the relations between the catalytic and magnetic properties of the copper-cobalt higher alcohol synthesis catalysts. We have undertaken to investigate the magnetic character by studying the Nuclear Quadrupole resonance of copper and (Zerofield) Nuclear Magnetic Resonance of cobalt in copper cobalt catalysts.

  4. Determination of exchange ratios in NMR and NQR spectroscopy from the 1D - relaxation dependences for the T2 - relaxation times

    NASA Astrophysics Data System (ADS)

    Sinyavsky, N. Ya.; Kostrikova, N. A.

    2017-09-01

    The paper proposes a new method for quantitative assessment of the constant exchange of magnetization between different states without registration of cross peaks on the T2-T2 topogram which significantly reduced both the experimental time and the time of computer processing of the results.

  5. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, December 15, 1991--March 15, 1992

    SciTech Connect

    Murty, A.N.

    1992-05-04

    During this period, we focused our attention in analyzing the magnetic nature of the extensively used trimetallic catalyst system Cu-Co-Cr for the production of higher alcohols. We believe that there could be some correspondence between the catalytic and magnetic behaviors of the transition metal catalyst systems. Both the morphology and metallic charge distribution of the particles are known to govern the catalytic as well as the magnetic properties of the system.

  6. A theoretical study on the characteristics of the intermolecular interactions in the active site of human androsterone sulphotransferase: DFT calculations of NQR and NMR parameters and QTAIM analysis.

    PubMed

    Astani, Elahe K; Heshmati, Emran; Chen, Chun-Jung; Hadipour, Nasser L

    2016-07-01

    A theoretical study at the level of density functional theory (DFT) was performed to characterize noncovalent intermolecular interactions, especially hydrogen bond interactions, in the active site of enzyme human androsterone sulphotransferase (SULT2A1/ADT). Geometry optimization, interaction energy, (2)H, (14)N, and (17)O electric field gradient (EFG) tensors, (1)H, (13)C, (17)O, and (15)N chemical shielding (CS) tensors, Natural Bonding Orbital (NBO) analysis, and quantum theory of atoms in molecules (QTAIM) analysis of this active site were investigated. It was found that androsterone (ADT) is able to form hydrogen bonds with residues Ser80, Ile82, and His99 of the active site. The interaction energy calculations and NBO analysis revealed that the ADT molecule forms the strongest hydrogen bond with Ser80. Results revealed that ADT interacts with the other residues through electrostatic and Van der Waals interactions. Results showed that these hydrogen bonds influence on the calculated (2)H, (14)N, and (17)O quadrupole coupling constants (QCCs), as well as (1)H, (13)C, (17)O, and (15)N CS tensors. The magnitude of the QCC and CS changes at each nucleus depends directly on its amount of contribution to the hydrogen bond interaction. Copyright © 2016 Elsevier Inc. All rights reserved.

  7. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, September 15, 1991--December 15, 1991

    SciTech Connect

    Not Available

    1992-01-14

    The primary objective of the project is to examine the relations between the catalytic and magnetic properties of the copper-cobalt higher alcohol synthesis catalysts. We have undertaken to investigate the magnetic character by studying the Nuclear Quadrupole resonance of copper and (Zerofield) Nuclear Magnetic Resonance of cobalt in copper cobalt catalysts.

  8. Coexistence of Antiferromagnetism with Superconductivity in CePt2In7: Microscopic Phase Diagram Determined by In115 NMR and NQR

    NASA Astrophysics Data System (ADS)

    Sakai, H.; Tokunaga, Y.; Kambe, S.; Ronning, F.; Bauer, E. D.; Thompson, J. D.

    2014-05-01

    Single crystals of the heavy-fermion antiferromagnet CePt2In7 with a Néel temperature (TN) of 5.2 K at ambient pressure have been investigated by zero-field In115-nuclear magnetic and quadrupole resonance measurements as a function of applied pressure. Within the antiferromagnetic state, the character of Ce's 4f electron appears to change from localized to itinerantlike at P*˜2.4 GPa, approximately the pressure where superconductivity first emerges. With increased pressure, the superconducting transition Tc reaches a maximum just at or slightly before antiferromagnetic order disappears, and not at the pressure Pc˜3.4 GPa, where the steeply decreasing Néel boundary extrapolates to zero temperature. For P >Pc, the spin relaxation rate drops sharply by more than 2 orders of magnitude at Tc, suggestive of a first-order transition.

  9. NQR-NMR studies of higher alcohol synthesis Cu-Co catalysts. Quarterly technical progress report, June 15--September 15, 1991

    SciTech Connect

    Not Available

    1991-12-17

    The primary objective of the project is to examine the relations between the catalytic and magnetic properties of the copper-cobalt higher alcohol synthesis catalysts. We have undertaken to investigate the magnetic character by studying the Nuclear Quadrupole resonance of copper and (Zerofield) Nuclear Magnetic Resonance of cobalt in copper cobalt catalysts.

  10. Charge fluctuations and nodeless superconductivity in quasi-one-dimensional Ta4Pd3Te16 revealed by 125Te-NMR and 181Ta-NQR

    NASA Astrophysics Data System (ADS)

    Li, Z.; Jiao, W. H.; Cao, G. H.; Zheng, Guo-qing

    2016-11-01

    We report 125Te nuclear magnetic resonance and 181Ta nuclear quadrupole resonance studies on single-crystal Ta4Pd3Te16 , which has a quasi-one-dimensional structure and superconducts below Tc=4.3 K. 181Ta with spin I =7 /2 is sensitive to quadrupole interactions, while 125Te with spin I =1 /2 can only relax by magnetic interactions. By comparing the spin-lattice relaxation rate (1 /T1 ) of 181Ta and 125Te, we found that electric-field-gradient (EFG) fluctuations develop below 80 K. The EFG fluctuations are enhanced with decreasing temperature due to the fluctuations of a charge density wave that sets in at TCDW=20 K, below which the spectra are broadened and 1 /T1T drops sharply. In the superconducting state, 1 /T1 shows a Hebel-Slichter coherence peak just below Tc for 125Te, indicating that Ta4Pd3Te16 is a full-gap superconductor without nodes in the gap function. The coherence peak is absent in the 1 /T1 of 181Ta due to the strong EFG fluctuations.

  11. Solution state NMR of lignins

    Treesearch

    John. Ralph; Jane M. Marita; Sally A. Ralph; Ronald D. Hatfield; Fachuang. Lu; Richard M. Ede; Junpeng. Peng; Larry L. Landucci

    1999-01-01

    Despite the rather random and heterogeneous nature of isolated lignins, many of their intimate structural details are revealed by diagnostic NMR experiments. 13C-NMR was recognized early-on as a high-resolution method for detailed structural characterization, aided by the almost exact agreement between chemical shifts of carbons in good low-molecular...

  12. THz Dynamic Nuclear Polarization NMR

    PubMed Central

    Nanni, Emilio A.; Barnes, Alexander B.; Griffin, Robert G.; Temkin, Richard J.

    2013-01-01

    Dynamic nuclear polarization (DNP) increases the sensitivity of nuclear magnetic resonance (NMR) spectroscopy by using high frequency microwaves to transfer the polarization of the electrons to the nuclear spins. The enhancement in NMR sensitivity can amount to a factor of well above 100, enabling faster data acquisition and greatly improved NMR measurements. With the increasing magnetic fields (up to 23 T) used in NMR research, the required frequency for DNP falls into the THz band (140–600 GHz). Gyrotrons have been developed to meet the demanding specifications for DNP NMR, including power levels of tens of watts; frequency stability of a few megahertz; and power stability of 1% over runs that last for several days to weeks. Continuous gyrotron frequency tuning of over 1 GHz has also been demonstrated. The complete DNP NMR system must include a low loss transmission line; an optimized antenna; and a holder for efficient coupling of the THz radiation to the sample. This paper describes the DNP NMR process and illustrates the THz systems needed for this demanding spectroscopic application. THz DNP NMR is a rapidly developing, exciting area of THz science and technology. PMID:24639915

  13. THz Dynamic Nuclear Polarization NMR.

    PubMed

    Nanni, Emilio A; Barnes, Alexander B; Griffin, Robert G; Temkin, Richard J

    2011-08-29

    Dynamic nuclear polarization (DNP) increases the sensitivity of nuclear magnetic resonance (NMR) spectroscopy by using high frequency microwaves to transfer the polarization of the electrons to the nuclear spins. The enhancement in NMR sensitivity can amount to a factor of well above 100, enabling faster data acquisition and greatly improved NMR measurements. With the increasing magnetic fields (up to 23 T) used in NMR research, the required frequency for DNP falls into the THz band (140-600 GHz). Gyrotrons have been developed to meet the demanding specifications for DNP NMR, including power levels of tens of watts; frequency stability of a few megahertz; and power stability of 1% over runs that last for several days to weeks. Continuous gyrotron frequency tuning of over 1 GHz has also been demonstrated. The complete DNP NMR system must include a low loss transmission line; an optimized antenna; and a holder for efficient coupling of the THz radiation to the sample. This paper describes the DNP NMR process and illustrates the THz systems needed for this demanding spectroscopic application. THz DNP NMR is a rapidly developing, exciting area of THz science and technology.

  14. The financing of NMR equipment.

    PubMed

    Frankel, A N

    1984-01-01

    Cost-containment regulations and possible legislative changes in the tax area are creating new environments for the acquisition of nuclear magnetic resonance (NMR) systems. Shared services, management groups, and free-standing clinics are being established. Creativity in financing will be required to assure the cost-effectiveness of NMR services.

  15. NMR and magnetic susceptibility in superconducting and antiferromagnetic Ga-based cuprates Y 1- xCa xSr 2Cu 2GaO 7 (0≤ x≤0.3)

    NASA Astrophysics Data System (ADS)

    Rykov, Alexandre I.; Ueda, Yutaka; Goto, Atsushi; Yasuoka, Hiroshi

    1996-02-01

    Magnetic susceptibility and NMR/NQR measurements were performed on Y 1- xCa xSr 2Cu 2GaO 7 ( x=0, 0.1, 0.2, 0.3). The single phase samples annealed at 600°C under oxygen pressure of 30 MPa are superconductors with Tc=35 K for x=0.2 and x=0.3. In spite of the presence of a small Curie-like term, we show that the spin susceptibility in the normal state increases with Ca doping and reaches the value χspin≈0.9 cm 3/Cu-mole, which is comparable to other superconducting cuprates. From the observation of Cu zero-field resonance (AFNR) and susceptibility data the parent compound is classified as 2D antiferromagnet ( TN=387 K). The transition from antiferromagnetic insulator to superconductor occurs with increasing concentration of carriers, but extends over several tens percent of Ca. The superconductivity is significantly suppressed by increasing disorder within limits of solubility for Ca. The Ga NQR spectra are narrow in both antiferromagnetic and superconducting regimes, but heavily broadened in the intermediate spin-glass-like domain. From x=0 to x=0.3, the 63Cu quadrupole frequency increases from 24 to 28 MHz due to the charge transfer resulting in superconductivity. Other EFG parameters are not markedly changed from those given in YSr 2Cu 2GaO 7 by Pieper [Physica C190(1992)261].

  16. Glassy spin freezing and NMR wipeout effect in the high-T{sub c} superconductor La{sub 1.90}Sr{sub 0.10}CuO{sub 4}: Critical discussion of the role of stripes

    SciTech Connect

    Julien, M.-H.; Campana, A.; Rigamonti, A.; Carretta, P.; Borsa, F.; Kuhns, P.; Reyes, A. P.; Moulton, W. G.; Horvatic, M.; Berthier, C.

    2001-04-01

    We report on {sup 139}La and {sup 63}Cu NMR/NQR measurements in the high-T{sub c} superconductor La{sub 1.90}Sr{sub 0.10}CuO{sub 4}, with T{sub c}=26.5 K. Spin fluctuations probed by {sup 139}La spin-lattice relaxation (T{sub 1}) continuously slow down on cooling through T{sub c}. We argue that spin freezing and superconductivity are bulk effects in this sample. Thus both phenomena have to coexist microscopically. The distribution of {sup 139}La T{sub 1} values at low temperature reveals a wide spread of spin fluctuation frequencies in CuO{sub 2} planes. A simple estimate shows that {sup 63}Cu nuclei at sites where electronic fluctuations are the slowest are not observable (wipeout effect) because relaxation times are too short. This means that the {sup 63}Cu NQR wipeout, observed in this sample, can be explained primarily by slow magnetic, rather than charge, fluctuations. The magnetic origin of the wipeout is still compatible with a connection between wipeout and charge order [as proposed by Hunt , Phys. Rev. Lett. 82, 4300 (1999)], but this connection is indirect. On the other hand, since the wipeout fraction is not an intensive quantity it cannot define a proper order parameter and cannot be used by itself as a criterion for the existence of a stripe phase.

  17. NQR in La{sub 1.85}Sr{sub 0.15}Cu{sub 1{minus}x}Li{sub x}O{sub 4} under high pressure (1.96GPa)

    SciTech Connect

    Fujiwara, Naoki; Mori, Nobuo; Kageyama, Hiroshi; Ueda, Yutaka

    1999-11-01

    Nuclear quadrupole resonance (NQR) under steady pressure (1.9GPa) was performed on La{sup 1.85}Sr{sub 0.15}Cu{sub 1{minus}x}Li{sub x}O{sub 4} where Li substitution causes metal (x = 0)-insulator (x = 0.5) transition. Two kinds of Cu-NQR signals corresponding to both states have been observed at the intermediate amount of x. Effect of the pressure was investigated for x = 0.25 and 0.3 samples. Possible Li-distribution pattern was proposed for the x = 0.3 sample.

  18. Magnetic correlations in La(2-x)Sr(x)CuO4 from NQR relaxation and specific heat

    NASA Technical Reports Server (NTRS)

    Borsa, F.; Rigamonti, A.

    1990-01-01

    La-139 and Cu-63 Nuclear Quadrupole Resonance (NQR) relaxation measurements in La(2-x)Sr(x)CuO4 for O = to or less than 0.3 and in the temperature range 1.6 + 450 K are analyzed in terms of Cu(++) magnetic correlations and dynamics. It is described how the magnetic correlations that would result from Cu-Cu exchange are reduced by mobile charge defects related to x-doping. A comprehensive picture is given which explains satisfactorily the x and T dependence of the correlation time, of the correlation length and of the Neel temperature T(sub n)(x) as well as being consistent with known electrical resistivity and magnetic susceptibility measurements. It is discussed how, in the superconducting samples, the mobile defects also cause the decrease, for T yields T(sub c)(+) of the hyperfine Cu electron-nucleus effective interaction, leading to the coexistence of quasi-localized, reduced magnetic moments from 3d Cu electrons and mobile oxygen p-hole carriers. The temperature dependence of the effective hyperfine field around the superconducting transition yields an activation energy which could be related to the pairing energy. New specific heat measurements are also presented and discussed in terms of the above picture.

  19. Sb-NQR study on novel superconductivity in (Pr 1-xLa x)Os 4Sb 12

    NASA Astrophysics Data System (ADS)

    Nagai, Takayuki; Yogi, Mamoru; Imamura, Yoju; Mukuda, Hidekazu; Kitaoka, Yoshio; Kikuchi, Daisuke; Sugawara, Hitoshi; Sato, Hideyuki

    2007-03-01

    We report on superconducting (SC) properties in a series of filled-skutterudite compounds (Pr 1-xLa x)Os 4Sb 12 through the Sb nuclear-quadrupole-resonance (NQR). In the SC state, the nuclear spin-lattice relaxation rate 1/ T1Pr at Pr-cage decreases exponentially with no coherence peak below TC, consistent with the results for the pure PrOs 4Sb 12. In the Pr-rich compounds of x=0.05 and 0.2, the residual density of states (RDOS) at the Fermi level are induced below TC due to the La substitution. It is concluded that the RDOS is not due to the impurity effect that used to be observed in unconventional superconductors with line-node gap. Rather, a part of the Fermi surface that contributes to 5.5% of the total is suggested to become gapless for x=0.05 and 0.2, yielding the RDOS. For the La-rich compounds of x=0.4, 0.8 and 1, as the Pr-substitution for La increases, TC increases and a size of energy gap increases. The Pr-substitution for La makes the pairing interaction for forming the Cooper pairs strong and causes an anisotropy in its energy-gap structure.

  20. Enhancement of Tc in CeIr(In1-xCdx)5 studied by In-NQR

    NASA Astrophysics Data System (ADS)

    Yashima, Mitsuharu; Tani, Kyohei; Nishimoto, Kazuhiro; Mukuda, Hidekazu; Kitaoka, Yoshio; Honda, Fuminori; Settai, Rikio; Ōnuki, Yoshichika

    2017-04-01

    We report on superconducting nature under pressure in CeIr(In1-xCdx)5 by In-Nuclear-Quadrupole-Resonance (NQR) studies. In CeIr(In0.925Cd0.075)5, the inhomogeneous antiferromagnetic order at TN ˜ 2.3 K is induced by Cd-dopants and superconductivity disappears at ambient pressure. However, the measurements of a nuclear-spin-lattice-relaxation rate 1/T1 have revealed that the superconductivity suddenly occurs above 2.1 GPa. It is observed that the superconducting gap is enhanced in the Cd-doped sample, indicating that the Cd-doping induces the strong coupling superconductivity leading to the enhancement of Tc in the CeIrIn5 system. Furthermore, we found that the residual density of states at the Fermi level increases with increasing pressure, suggesting that the superconducting nature of CeIrIn5 is quite different from those of CeCoIn5 and CeRhIn5.

  1. Stereoelectronic structure and 35Cl NQR parameters of 4-(trichlorgermyl)butan-2-one using ab initio calculations

    NASA Astrophysics Data System (ADS)

    Feshin, V. P.; Feshina, E. V.

    2012-03-01

    The results of ab initio calculations at the RHF/6-31G(d) and MP2/6-31G(d) levels of two stable structures of the 4-(trichlorgermyl)butan-2-one molecule with total optimization of their geometry have been represented. The structure with pentacoordinated Ge atom is energetically more advantageous as compared with that with tetracoordinated one. Using these results, the 35Cl nuclear quadrupole resonance (NQR) frequencies and asymmetry parameters of the electric field gradient (EFG) at the 35Cl nuclei in molecule with pentacoordinated Ge atom have been assessed, the frequencies satisfactorily agreeing with experimental data. Calculations at the RHF/6-31G(d) level have been performed also at various Ge⋯O distances. It has been demonstrated that convergence of the Ge and O coordination centers leads to the increase of positive charge at the Ge coordination center and of negative charge at the O coordination center, at that, electron density from the Ge atom shifts mainly to the axial Cl atom and from the C atom of carbonyl group - to its O atom. The electron density transfer from the O to Ge atom does not occur.

  2. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1989-01-01

    This report covers the progress made on the title project during the past reporting period. Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concerns how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coals model. Along the same lines the authors are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. The effects of very high MAS rates (>10 kHz) on cross polarization dynamics are also being investigated for similar reasons. The authors have been reinvestigating the prospects of using zero field NMR types of techniques for two dimensional NMR structural analysis of complex organic solids such as coals. Currently MAS spin rates are not sufficiently high to permit zero field in high field NMR for protons in typical organic solids, however they are compatible with {sup 13}C-{sup 13}C dipolar couplings. In collaboration with Dr. Robert Tycko of AT T Bell Laboratories, inventor of the zero field in high field NMR method, the authors have performed the first zero field in high field {sup 13}C NMR experiments. These results are described. 9 refs., 2 figs.

  3. Understanding NMR Chemical Shifts

    NASA Astrophysics Data System (ADS)

    Jameson, Cynthia J.

    1996-10-01

    The NMR chemical shift serves as a paradigm for molecular electronic properties. We consider the factors that determine the general magnitudes of the shifts, the state of the art in theoretical calculations, the nature of the shielding tensor, and the multidimensional shielding surface that describes the variation of the shielding with nuclear positions. We also examine the nature of the intermolecular shielding surface as a general example of a supermolecule property surface. The observed chemical shift in the zero-pressure limit is determined not only by the value of the shielding at the equilibrium geometry, but the dynamic average over the multidimensional shielding surface during rotation and vibration of the molecule. In the gas, solution, or adsorbed phase it is an average of the intermolecular shielding surface over all the configurations of the molecule with its neighbors. The temperature dependence of the chemical shift in the isolated molecule, the changes upon isotopic substitution, the changes with environment, are well characterized experimentally so that quantum mechanical descriptions of electronic structure and theories related to dynamics averaging of any electronic property can be subjected to stringent test.

  4. Polarization transfer NMR imaging

    DOEpatents

    Sillerud, Laurel O.; van Hulsteyn, David B.

    1990-01-01

    A nuclear magnetic resonance (NMR) image is obtained with spatial information modulated by chemical information. The modulation is obtained through polarization transfer from a first element representing the desired chemical, or functional, information, which is covalently bonded and spin-spin coupled with a second element effective to provide the imaging data. First and second rf pulses are provided at first and second frequencies for exciting the imaging and functional elements, with imaging gradients applied therebetween to spatially separate the nuclei response for imaging. The second rf pulse is applied at a time after the first pulse which is the inverse of the spin coupling constant to select the transfer element nuclei which are spin coupled to the functional element nuclei for imaging. In a particular application, compounds such as glucose, lactate, or lactose, can be labeled with .sup.13 C and metabolic processes involving the compounds can be imaged with the sensitivity of .sup.1 H and the selectivity of .sup.13 C.

  5. Integrative NMR for biomolecular research.

    PubMed

    Lee, Woonghee; Cornilescu, Gabriel; Dashti, Hesam; Eghbalnia, Hamid R; Tonelli, Marco; Westler, William M; Butcher, Samuel E; Henzler-Wildman, Katherine A; Markley, John L

    2016-04-01

    NMR spectroscopy is a powerful technique for determining structural and functional features of biomolecules in physiological solution as well as for observing their intermolecular interactions in real-time. However, complex steps associated with its practice have made the approach daunting for non-specialists. We introduce an NMR platform that makes biomolecular NMR spectroscopy much more accessible by integrating tools, databases, web services, and video tutorials that can be launched by simple installation of NMRFAM software packages or using a cross-platform virtual machine that can be run on any standard laptop or desktop computer. The software package can be downloaded freely from the NMRFAM software download page ( http://pine.nmrfam.wisc.edu/download_packages.html ), and detailed instructions are available from the Integrative NMR Video Tutorial page ( http://pine.nmrfam.wisc.edu/integrative.html ).

  6. Compact orthogonal NMR field sensor

    DOEpatents

    Gerald, II, Rex E.; Rathke, Jerome W.

    2009-02-03

    A Compact Orthogonal Field Sensor for emitting two orthogonal electro-magnetic fields in a common space. More particularly, a replacement inductor for existing NMR (Nuclear Magnetic Resonance) sensors to allow for NMR imaging. The Compact Orthogonal Field Sensor has a conductive coil and a central conductor electrically connected in series. The central conductor is at least partially surrounded by the coil. The coil and central conductor are electrically or electro-magnetically connected to a device having a means for producing or inducing a current through the coil and central conductor. The Compact Orthogonal Field Sensor can be used in NMR imaging applications to determine the position and the associated NMR spectrum of a sample within the electro-magnetic field of the central conductor.

  7. Off-resonance effects in (14)N NQR signals from the pulsed spin-locking (PSL) and three-pulse echo sequence; a study for monoclinic TNT.

    PubMed

    Smith, John A S; Rowe, Michael D; Althoefer, Kaspar; Peirson, Neil F; Barras, Jamie

    2015-10-01

    In NQR detection applications signal averaging by the summation of rapidly regenerated signals from multiple pulse sequences of the pulsed spin-locking (PSL) type is often used to improve sensitivity. It is important to characterise and if possible minimise PSL sequence off-resonance effects since they can make it difficult to optimise detection performance. We illustrate this with measurements of the variation of the decay time T2e and the amplitude of PSL signal trains with pulse spacing and excitation offset frequency for the 870 kHz ν+(14)N NQR line of monoclinic TNT under carefully stabilised temperature conditions. We have also carried out a similar study of signals from monoclinic TNT and 1H-1,2,3-triazole generated by a three-pulse echo sequence and the results are shown to agree well with a theoretical treatment appropriate to polycrystalline NQR samples such as TNT for which spin I=1, asymmetry parameter η≠0 and T1≫T2. Based on this theory we derive simple models for calculating TNT PSL signal trains and hence the pulse spacing and off-resonance dependence of signal amplitude and T2e which we compare to our experimental data. We discuss the influence of PSL echo summation on off-resonance effects in detected signal intensity and show how a phase-alternated multiple pulse sequence can be used in combination with the PSL sequence to eliminate variation in detection performance due to off-resonance effects. Copyright © 2015 Elsevier Inc. All rights reserved.

  8. NMR Imaging of Elastomeric Materials

    DTIC Science & Technology

    1990-11-30

    on ’everse if necessary and identify by block number) FIELD GROUP SUB-GROUP nuclear magnetic resonance , imaging, elastomers, tires, composites, porous...correspondence should be addressed 1i ABSTRACT Nuclear magnetic resonance images have been obtained for four porous glass disks of different porosities...INDEX HEADINGS: NMR imaging Porous materials Spin relaxation 2. I0J INTRODUCTION Nuclear magnetic resonance (NMR) imaging has seen increasing use in the

  9. NMR characterization of thin films

    DOEpatents

    Gerald II, Rex E.; Klingler, Robert J.; Rathke, Jerome W.; Diaz, Rocio; Vukovic, Lela

    2010-06-15

    A method, apparatus, and system for characterizing thin film materials. The method, apparatus, and system includes a container for receiving a starting material, applying a gravitational force, a magnetic force, and an electric force or combinations thereof to at least the starting material, forming a thin film material, sensing an NMR signal from the thin film material and analyzing the NMR signal to characterize the thin film of material.

  10. Optical pumping and xenon NMR

    SciTech Connect

    Raftery, M. Daniel

    1991-11-01

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

  11. Optical pumping and xenon NMR

    SciTech Connect

    Raftery, M.D.

    1991-11-01

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

  12. Multispectral Analysis of NMR Imagery

    NASA Technical Reports Server (NTRS)

    Butterfield, R. L.; Vannier, M. W. And Associates; Jordan, D.

    1985-01-01

    Conference paper discusses initial efforts to adapt multispectral satellite-image analysis to nuclear magnetic resonance (NMR) scans of human body. Flexibility of these techniques makes it possible to present NMR data in variety of formats, including pseudocolor composite images of pathological internal features. Techniques do not have to be greatly modified from form in which used to produce satellite maps of such Earth features as water, rock, or foliage.

  13. Multispectral Analysis of NMR Imagery

    NASA Technical Reports Server (NTRS)

    Butterfield, R. L.; Vannier, M. W. And Associates; Jordan, D.

    1985-01-01

    Conference paper discusses initial efforts to adapt multispectral satellite-image analysis to nuclear magnetic resonance (NMR) scans of human body. Flexibility of these techniques makes it possible to present NMR data in variety of formats, including pseudocolor composite images of pathological internal features. Techniques do not have to be greatly modified from form in which used to produce satellite maps of such Earth features as water, rock, or foliage.

  14. NMR characterization of thin films

    DOEpatents

    Gerald, II, Rex E.; Klingler, Robert J.; Rathke, Jerome W.; Diaz, Rocio; Vukovic, Lela

    2008-11-25

    A method, apparatus, and system for characterizing thin film materials. The method, apparatus, and system includes a container for receiving a starting material, applying a gravitational force, a magnetic force, and an electric force or combinations thereof to at least the starting material, forming a thin film material, sensing an NMR signal from the thin film material and analyzing the NMR signal to characterize the thin film of material.

  15. Phase diagram for antiferromagnetism and superconductivity in the pressure-induced heavy-fermion superconductor Ce2RhIn8 probed by I115n-NQR

    NASA Astrophysics Data System (ADS)

    Yashima, M.; Taniguchi, S.; Miyazaki, H.; Mukuda, H.; Kitaoka, Y.; Shishido, H.; Settai, R.; Ōnuki, Y.

    2009-11-01

    We present a phase diagram for the antiferromagnetism and superconductivity in Ce2RhIn8 probed by In-NQR studies under pressure (P) . The quasi-two-dimensional character of antiferromagnetic spin fluctuations in the paramagnetic state at P=0 evolves into a three-dimensional character because of the suppression of antiferromagnetic order for P>PQCP˜1.36GPa (QCP: quantum critical point). Nuclear-spin-lattice relaxation rate 1/T1 measurements revealed that the superconducting order occurs in the P range 1.36-1.84 GPa, with maximum Tc˜0.9K around PQCP˜1.36GPa .

  16. Reorientation of molecules in a Cl/sub 3/P/Dirac h/NCCl/sub 2/CF/sub 3/ crystal according to NQR data

    SciTech Connect

    Kyuntsel', I.A.; Mokeeva, V.A.; Soifer, G.B.

    1988-05-01

    The structural-dynamic inequivalence of the molecules in solid Cl/sub 3/P/Dirac h/NCCl/sub 2/CF/sub 3/ has been established, and their rotational mobility has been studied with the aid of the temperature dependence of the resonance frequency and of the spin-lattice relaxation time of the /sup 35/Cl nuclei. The observed motion has been interpreted with consideration of the molecular structure as reorientation between unequal potential wells in the crystal lattice, and the corresponding activation parameters have been determined from the /sup 35/Cl NQR data.

  17. Distribution of nonequivalent aluminum sites revealed in Al-Cu-Ru and Al-Cu-Fe quasicrystals by [sup 27]Al NQR

    SciTech Connect

    Shastri, A.; Borsa, F.; Torgeson, D.R.; Goldman, A.I. )

    1994-08-01

    The distribution of nonequivalent aluminum sites was studied in Al-Cu-Fe and Al-Cu-Ru stable icosahedral quasicrystalline phases using [sup 27]Al NQR spectra taken at 4.2 K. The observed spectra---which give directly the distribution of nonequivalent aluminum sites---were broad, asymmetric, and structureless. A simple electric-field-gradient model calculation accounted for the spectral width in terms of a wide distribution of local atomic environments, and an estimate for the lower limit on the number of nonequivalent aluminum sites was found.

  18. Synthesis, conformational and NQR analysis of phosphoric triamides containing the P(O)[N]3 skeleton

    NASA Astrophysics Data System (ADS)

    Shariatinia, Zahra; Della Védova, Carlos O.; Erben, Mauricio F.; Tavasolinasab, Vahid; Gholivand, Khodayar

    2012-09-01

    New phosphoric triamides with general formula P(O)X3 where X = N-4-methylpiperazinyl (1), N-4-phenylpiperazinyl (2), N-4-ethoxycarbonyl piperazinyl (3), N-2-tetrahydrofurfuryl (4) were synthesized and characterized by 1H, 13C, 31P NMR, IR, Mass spectroscopy and elemental analysis. The molecular structure for compounds 1-4 were obtained by using quantum chemical calculations (HF and B3LYP methods with the 6-31+G∗∗ basis set). Moreover, optimized structures for previously reported 4-FC6H4C(O)NHP(O)X2 phosphoric triamides, X = pyrrolidin-1-yl (5), piperidin-1-yl (6) and hexamethyleneimin-1-yl (7) were obtained using the solid state structure (CIF files) as a starting point for the gas phase computation in which all independent molecules in structures 6 (seven structures) and 7 (two structures) were included. The computed results were in good agreement with the data obtained from the X-ray crystal structures reported earlier. The nuclear quadrupole coupling constants (NQCCs or χs) were calculated about 5.0 and 10.0 MHz for the 17O atoms of Pdbnd O and Cdbnd O bonds. For nitrogen atoms bonded to the phosphorus the NQCCs were found in the range between 4.0 and 5.5 MHz, whereas for compounds 4-7, the expected values for amidic hydrogen atoms are near 300 kHz.

  19. Investigation of C-H...O=C and N-H...OC hydrogen-bonding interactions in crystalline thymine by DFT calculations of O-17, N-14 and H-2 NQR parameters.

    PubMed

    Mirzaei, Mahmoud; Hadipour, Nasser L; Ahmadi, Kamran

    2007-02-01

    A computational study at the level of density functional theory (DFT) was carried out to investigate C-H...O=C and N-H...O=C hydrogen-bonding interactions (HBs) in the real crystalline cluster of thymine by O-17, N-14 and H-2 calculated nuclear quadrupole resonance (NQR) parameters. To perform the calculations, a hydrogen-bonded pentameric cluster of thymine was created using X-ray coordinates where the hydrogen atoms positions are optimized and the electric field gradient (EFG) tensors were calculated for the target molecule. Additional EFG calculations were also performed for crystalline monomer and an optimized isolated gas-phase thymine. The calculated EFG tensors at the level of B3LYP and B3PW91 DFT methods and 6-311++G**and CC-pVTZ basis sets were converted to those experimentally measurable NQR parameters, quadrupole coupling constants and asymmetry parameters. The results reveal that because of strong contribution to N-H...O=C HBs, NQR parameters of O2, N1 and N3 undergo significant changes from monomer to the target molecule in cluster. Furthermore, the NQR parameters of O2 also undergo some changes because of non-classical C-H...O=C HBs.

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

    SciTech Connect

    Matwiyoff, N.A.

    1983-01-01

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

  1. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1988-01-01

    This report covers the progress made on the title project during the current reporting period. Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concerns how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coals model. Along the same lines we are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. This quarter we have focused on variable temperature spin lattice relaxation measurements for several of the Argonne coals. 5 figs.

  2. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1988-01-01

    This report covers the progress made on the title project during the current reporting period. Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concerns how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coals model. Along the same lines we are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. This quarter we have focussed on spin lattice relaxation measurements for several of the Argonne coals. 2 figs., 1 tab.

  3. Rotating Frame NQR spin-lattice relaxation in the Incommensurate Insulator Rb_2ZnCl_4

    NASA Astrophysics Data System (ADS)

    Subramanian, R. K.; Ailion, David C.; Muntean, Ligia

    1997-03-01

    Measurements of the rotating frame spin-lattice relaxation time T_1ρ can be quite useful in detecting low frequency dipolar or quadrupolar fluctuations arising from translational diffusion or molecular reorientations. Normally, the presence of such low frequency motions causes enhanced relaxation, resulting in T_1ρ being shorter than the laboratory frame spin-lattice relaxation time, T1 (in the appropriate correlation time limit). However, the weak collision theory has been used to predict that T_1ρ can be longer than T1 for quadrupolar systems when low frequency motions are absent (R. Blinc, private communication). We performed pure NQR T_1ρ measurements of ^35Cl in the paraelectric phase of Rb_2ZnCl4 at two different rf fields (13 G and 43 G, corresponding to 5.4 kHz and 18 kHz, respectively) and observed that T_1ρ is longer than T1 at all temperatures studied (302 - 360 K). Furthermore, the relaxation becomes less effective (i.e., T_1ρ became longer) as the rf field increases from 13 G to 43 G. Above 315 K, the reorientational motions of the ZnCl4 anion become more important and T_1ρ for 13 G becomes almost equal to T_1, even though T_1ρ at 43 G still is significantly longer than T_1. These observations clearly indicate the absence of a contribution to the ^35Cl pure quadrupolar T_1ρ in Rb_2ZnCl4 in this temperature region.

  4. NMR planar microcoil for microanalysis

    NASA Astrophysics Data System (ADS)

    Sorli, B.; Chateaux, J. F.; Quiquerez, L.; Bouchet-Fakri, L.; Briguet, A.; Morin, P.

    2006-11-01

    This article deals with the analysis of small sample volume by using a planar microcoil and a micromachined cavity. This microcoil is used as a nuclear magnetic resonance (NMR) radio frequency detection coil in order to perform in vitro NMR analysis of the sample introduced into the microcavity. It is a real challenging task to develop microsystem for NMR spectrum extraction for smaller and smaller sample volume. Moreover, it is advantageous that these microsystems could be integrated in a Micro Total Analysing System (μ -TAS) as an analysing tool. In this paper, NMR theory, description, fabrication process and electrical characterization of planar microcoils receiver are described. Results obtained on NMR microspectroscopy experiments have been performed on water and ethanol, using a 1 mm diameter planar coil. This microcoil is tuned and matched at 85.13 MHz which is the Larmor frequency of proton in a 2 T magnetic field. This paper has been presented at “3e colloque interdisciplinaire en instrumentation (C2I 2004)”, École Normale Supérieure de Cachan, 29 30 janvier 2004.

  5. NMR characterization of shocked quartz

    SciTech Connect

    Boslough, M.B.; Cygan, R.T.; Assink, R.A.; Kirkpatrick, R.J.

    1994-03-01

    We have characterized experimentally and naturally-shocked quartz (both synthetic and natural samples) by solid state nuclear magnetic resonance (NMR) spectroscopy. Relaxation analysis of experimentally-shocked samples provides a means for quantitative characterization of the amorphous/disordered silica component NMR spectra demonstrate that magnetization in both the amorphous and crystalline components follows power-law behavior as a function of recycle time. This observation is consistent with the relaxation of nuclear spins by paramagnetic impurities. A fractal dimension can be extracted from the power-law exponent associated with each phase, and relative abundances can be extracted from integrated intensities of deconvolved peaks. NMR spectroscopy of naturally-shocked sandstone from Meteor Crater, Arizona (USA) led to the discovery of a new amorphous hydroxylated silica phase. Solid state NMR spectra of both experimentally and naturally shocked quartz were unexpectedly rich in microstructural information, especially when combined with relaxation analysis and cross-polarization studies. We suggest solid state NMR as a potentially useful tool for examining shock-induced microstructural changes in other inorganic compounds, with possible implications for shock processing of structural ceramics.

  6. Electronic and spatial structure of some compounds of pentacoordinated phosphorus according to data from /sup 35/Cl NQR and x-ray emission spectroscopy

    SciTech Connect

    Feshin, V.P.; Elin, V.P.; Timokhin, B.V.; Dmitriev, V.K.; Dolgushin, G.V.; Kalabina, A.V.; Voronkov, M.G.

    1987-04-01

    Compounds of pentavalent phosphorus can exist in both molecular and ionic forms, as has frequently easily and reliably been established by /sup 35/Cl NQR. These compounds have not heretofore been studied by x-ray emission spectroscopy. The authors used this method together with NQR to study a number of compounds of pentacoordinated phosphorus. The P K/sub ..beta../ and Cl K/sub ..beta../ x-ray emission spectra of compounds containing P and Cl atoms are caused by the formation of a vacancy under the action of the x radiation in the 1s orbital of the respective atom, which is filled by electrons from MO's formed with the participation of its 3p orbitals. The selection rules, as well as a comparison of the experimental P K/sub ..beta../ spectrum with the results of a quantum-mechanical calculation (in the CNDO/2 approximation), permit the assignment of the lines in the spectrum to transitions from different MO's and the introduction of corrections into the calculation of the contribution of the 3p electrons of the P atom to the corresponding MO's and the difference between their energies.

  7. NQR investigation of pressure-induced charge transfer in oxygen-deficient YBa sub 2 Cu sub 3 O sub 7-. delta. (. delta. = 0. 38)

    SciTech Connect

    Reyes, A.P.; Ahrens, E.T.; Hammel, P.C.; Heffner, R.H. ); Takigawa, M. . Thomas J. Watson Research Center)

    1992-01-01

    Measurements of the pressure dependence of {sup 63}Cu nuclear quadrupole frequency in YBa{sub 2}Cu{sub 3}O{sub 6.62} from ambient pressure up to 1.5 GPa at 4k have been performed. {Tc} was found to increase with pressure: d{Tc}/dp {approximately} 5 K/GPa. All observed NQR lines are linear in pressure: dln{nu}{sub Q}/dp=z. We found positive z for the empty chain sites, consistent with ionic (Cu{sup 1+}) configuration in which the atom simply feels a squeezing lattice. Planar coppers close to the empty chains have positive z, while those that are close to full chains have z {approximately} 0. We present an analysis of the NQR result on the basis of the charge transfer model in which the mobile charges migrate from the chain to the plane sites. We deduced that a transfer of 0.021 holes to the O(2,3) sites would explain the result in YBa{sub 2}Cu{sub 3}O{sub 6.62}, whereas only 0.007 holes transfer in fully oxygenated YBa{sub 2}Cu{sub 3}O{sub 7}.

  8. Unconventional superconductivity near quantum critical point revealed by Co-NQR measurements on Nax(H3O)CoO2·yH2O

    NASA Astrophysics Data System (ADS)

    Ihara, Y.; Takeya, H.; Ishida, K.; Michioka, C.; Yoshimura, K.; Takada, K.; Sasaki, T.; Sakurai, H.; Takayama-Muromachi, E.

    2007-11-01

    The nuclear quadrupole resonance (NQR) frequency of Co nuclei and the nuclear spin lattice relaxation rate 1/T1 were measured on several bilayered hydrate (BLH) Nax(H3O)CoO2·yH2O (y˜1.3) with variety of superconducting (SC) and magnetic transition temperatures, Tc and TM, together with non-SC mono-layered hydrate (MLH) Nax(H3O)CoO2·yH2O (y˜0.7). In the high temperature region above 70 K, 1/T1T in all the samples follows the same temperature dependence which is interpreted as the pseudogap behavior. In the BLH compounds, 1/T1T increases with decreasing temperature below 70 K, and the values of 1/T1T at Tc are large in high-Tc samples. The magnetic ordering is ascertained from the observation of the prominent divergence of 1/T1T at TM in the samples whose NQR frequency is higher than 12.5 MHz. The temperature dependence of 1/T1T is found to be consistently expressed by a unique function with two fitting parameters. We analyze the temperature dependence of 1/T1T on the basis of this function, and investigate the relationship between the magnetic fluctuations and superconductivity in the BLH compounds.

  9. Absence of Magnetic Dipolar Phase Transition and Evolution of Low-Energy Excitations in PrNb2Al20 with Crystal Electric Field Γ3 Ground State: Evidence from 93Nb-NQR Studies

    NASA Astrophysics Data System (ADS)

    Kubo, Tetsuro; Kotegawa, Hisashi; Tou, Hideki; Higashinaka, Ryuji; Nakama, Akihiro; Aoki, Yuji; Sato, Hideyuki

    2015-07-01

    We report measurements of bulk magnetic susceptibility and 93Nb nuclear quadrupole resonance (NQR) in the Pr-based caged compound PrNb2Al20. By analyzing the magnetic susceptibility and magnetization, the crystal electric field (CEF) level scheme of PrNb2Al20 is determined to be Γ3(0 K)-Γ4(21.32 K)-Γ5(43.98 K)-Γ1(51.16 K) within the framework of the localized 4f electron picture. The 93Nb-NQR spectra exhibit neither spectral broadening nor spectral shift upon cooling down to 75 mK. The 93Nb-NQR spin-lattice relaxation rate 1/T1 at 5 K depends on the frequency and remains almost constant below 5 K. The frequency dependence of 1/T1 is attributed to the magnetic fluctuation due to the hyperfine-enhanced 141Pr nuclear moment inherent in the nonmagnetic Γ3 CEF ground state. The present NQR results provide evidence that no symmetry-breaking magnetic dipole order occurs down to 75 mK. Also, considering an invariant form of the quadrupole and octupole couplings between a 93Nb nucleus and Pr 4f electrons, Pr 4f quadrupoles and an octupole can couple with a 93Nb nuclear quadrupole moment and nuclear spin, respectively. Together with the results of bulk measurements, the present NQR results suggest that the possibility of a static quadrupole or octupole ordering can be excluded down to 100 mK. At low temperatures below 500 mK, however, the nuclear spin-echo decay rate gradually increases and the decay curve changes from Gaussian decay to Lorentzian decay, suggesting the evolution of a low-energy excitation.

  10. Temperature variation of ultralow frequency modes and mean square displacements in solid lasamide (diuretic drug) studied by 35Cl-NQR, X-ray and DFT/QTAIM.

    PubMed

    Latosińska, Jolanta Natalia; Latosińska, Magdalena; Kasprzak, Jerzy; Tomczak, Magdalena; Maurin, Jan Krzysztof

    2012-10-25

    The application of combined (35)Cl-NQR/X-ray/DFT/QTAIM methods to study the temperature variation of anisotropic displacement parameters and ultralow frequency modes of anharmonic torsional vibrations in the solid state is illustrated on the example of 2,4-dichloro-5-sulfamolybenzoic acid (lasamide, DSBA) which is a diuretic and an intermediate in the synthesis of furosemide and thus its common impurity. The crystallographic structure of lasamide is solved by X-ray diffraction and refined to a final R-factor of 3.06% at room temperature. Lasamide is found to crystallize in the triclinic space group P-1, with two equivalent molecules in the unit cell a = 7.5984(3) Å, b = 8.3158(3) Å, c = 8.6892(3) Å; α = 81.212(3)°, β = 73.799(3)°, γ = 67.599(3)°. Its molecules form symmetric dimers linked by two short and linear intermolecular hydrogen bonds O-H···O (O-H···O = 2.648 Å and ∠OHO = 171.5°), which are further linked by weaker and longer intermolecular hydrogen bonds N-H···O (N-H···O = 2.965 Å and ∠NHO = 166.4°). Two (35)Cl-NQR resonance frequencies, 36.899 and 37.129 MHz, revealed at room temperature are assigned to chlorine sites at the ortho and para positions, relative to the carboxyl functional group, respectively. The difference in C-Cl(1) and C-Cl(2) bond lengths only slightly affects the value of (35)Cl-NQR frequencies, which results mainly from chemical inequivalence of chlorine atoms but also involvement in different intermolecular interactions pattern. The smooth decrease in both (35)Cl-NQR frequencies with increasing temperature in the range of 77-300 K testifies to the averaging of EFG tensor at each chlorine site due to anharmonic torsional vibrations. Lasamide is thermally stable; no temperature-induced release of chlorine or decomposition of this compound is detected. The temperature dependence of ultralow frequency modes of anharmonic small-angle internal torsional vibrations averaging EFG tensor and mean square angle

  11. 133Cs and 75As NMR investigation of the normal metallic state of quasi-one-dimensional Cs2Cr3As3

    NASA Astrophysics Data System (ADS)

    Zhi, Haizhao; Lee, Drake; Imai, Takashi; Tang, Zhangtu; Liu, Yi; Cao, Guanghan

    2016-05-01

    We report 133Cs NMR and 75As nuclear quadrupole resonance (NQR) measurements on the normal metallic state above Tc of a quasi-one-dimensional superconductor Cs2Cr3As3 (Tc<1.6 K). From the 133Cs NMR Knight shift 133K measured at the Cs1 site, we show that the uniform spin susceptibility χspin increases from 295 K to ˜60 K, followed by a mild suppression; χspin then levels off below ˜10 K. In contrast, a vanishingly small magnitude of 133K indicates that Cs2 sites contribute very little to electrical conduction and the exchange interactions between 3d electrons at Cr sites. Low frequency Cr spin dynamics, reflected on 75As1 /T1T (the nuclear spin-lattice relaxation rate 1 /T1 divided by temperature T ), shows an analogous trend as χspin. Comparison with the results of 1 /T1T near Tc with K2Cr3As3 (Tc=6.1 K) and Rb2Cr3As3 (Tc=4.8 K) establishes a systematic trend that substitution of K+ ions with larger alkali ions progressively suppresses Cr spin fluctuations together with Tc.

  12. Improving NMR Structures of RNA

    PubMed Central

    Bermejo, Guillermo A.; Clore, G. Marius; Schwieters, Charles D.

    2016-01-01

    SUMMARY Here, we show that modern solution NMR structures of RNA exhibit more steric clashes and conformational ambiguities than their crystallographic X-ray counterparts. To tackle these issues, we developed RNA-ff1, a new force field for structure calculation with Xplor-NIH. Using seven published NMR datasets, RNA-ff1 improves covalent geometry and MolProbity validation criteria for clashes and backbone conformation in most cases, relative to both the previous Xplor-NIH force field and the original structures associated with the experimental data. In addition, with smaller base pair step rises in helical stems, RNA-ff1 structures enjoy more favorable base stacking. Finally, structural accuracy improves in the majority cases, as supported by complete residual dipolar coupling cross-validation. Thus, the reported advances show great promise in bridging the quality gap that separates NMR and X-ray structures of RNA. PMID:27066747

  13. Solution NMR conformation of glycosaminoglycans.

    PubMed

    Pomin, Vitor H

    2014-04-01

    Nuclear magnetic resonance (NMR) spectroscopy has been giving a pivotal contribution to the progress of glycomics, mostly by elucidating the structural, dynamical, conformational and intermolecular binding aspects of carbohydrates. Particularly in the field of conformation, NOE resonances, scalar couplings, residual dipolar couplings, and chemical shift anisotropy offsets have been the principal NMR parameters utilized. Molecular dynamics calculations restrained by NMR-data input are usually employed in conjunction to generate glycosidic bond dihedral angles. Glycosaminoglycans (GAGs) are a special class of sulfated polysaccharides extensively studied worldwide. Besides regulating innumerous physiological processes, these glycans are also widely explored in the global market as either clinical or nutraceutical agents. The conformational aspects of GAGs are key regulators to the quality of interactions with the functional proteins involved in biological events. This report discusses the solution conformation of each GAG type analyzed by one or more of the above-mentioned methods.

  14. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1990-01-01

    This report covers the progress made on the title project and summarizes the accomplishments for the project period. Four major areas of inquiry have been pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concerns how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coals model. Along the same lines the authors are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. The effects of very high MAS rates (>10 kHz) on cross polarization dynamics are also being investigated for similar reasons. The authors have concentrated on a theoretical treatment of pairs of tightly coupled spin {1/2} nuclei under magic angle spinning conditions. The average Hamiltonian theory developed here is required for a quantitative understanding of two dimensional NMR experiments of such spin pairs in solids. These experiments in turn provide a means of determining connectivities between resonances in solid state NMR spectra. Development of these techniques will allow us to establish connectivities between functional components in coals. The complete description of these spin dynamics has turned out to be complex, and is necessary to provide a foundation upon which such experiments may be quantitatively interpreted in complex mixtures such as coals. 25 refs., 4 figs., 3 tabs.

  15. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1989-01-01

    This report covers the progress made on the title project and summarizes the accomplishments for the project period. Four major areas of inquiry have been pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concern how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coals model. Along the same lines we are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. The effects of very high MAS rates (>10 kHz) on cross polarization dynamics are also being investigated for similar reasons. During the last quarter the authors have concentrated on improvements in cross polarization (CP) sequences with a goal of making the CP process insensitive to experimental conditions such as the magic angle spinning (MAS) rate. In order to be able to use fields the order of 7.0 T or higher, CP efficiency must be maintained at MAS rates of over 10 kHz. The standard sequences have severe limitations at these rates which lead to intensity distortions in {sup 13}C CPMAS spectra. Thus in order to be able to take advantage of the increases in sensitivity and resolution that accompany high field operation, improvements in the NMR methods are required. The new sequences the authors are developing will be especially important for quantitative analysis of coal structure by {sup 13}C solid state NMR at high field strengths. 13 refs., 7 figs., 2 tabs.

  16. "Solvent Effects" in 1H NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Cavaleiro, Jose A. S.

    1987-01-01

    Describes a simple undergraduate experiment in chemistry dealing with the "solvent effects" in nuclear magnetic resonance (NMR) spectroscopy. Stresses the importance of having students learn NMR spectroscopy as a tool in analytical chemistry. (TW)

  17. "Solvent Effects" in 1H NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Cavaleiro, Jose A. S.

    1987-01-01

    Describes a simple undergraduate experiment in chemistry dealing with the "solvent effects" in nuclear magnetic resonance (NMR) spectroscopy. Stresses the importance of having students learn NMR spectroscopy as a tool in analytical chemistry. (TW)

  18. Protein-Inhibitor Interaction Studies Using NMR

    PubMed Central

    Ishima, Rieko

    2015-01-01

    Solution-state NMR has been widely applied to determine the three-dimensional structure, dynamics, and molecular interactions of proteins. The designs of experiments used in protein NMR differ from those used for small-molecule NMR, primarily because the information available prior to an experiment, such as molecular mass and knowledge of the primary structure, is unique for proteins compared to small molecules. In this review article, protein NMR for structural biology is introduced with comparisons to small-molecule NMR, such as descriptions of labeling strategies and the effects of molecular dynamics on relaxation. Next, applications for protein NMR are reviewed, especially practical aspects for protein-observed ligand-protein interaction studies. Overall, the following topics are described: (1) characteristics of protein NMR, (2) methods to detect protein-ligand interactions by NMR, and (3) practical aspects of carrying out protein-observed inhibitor-protein interaction studies. PMID:26361636

  19. Push-through Direction Injectin NMR Automation

    EPA Science Inventory

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

  20. Push-through Direction Injectin NMR Automation

    EPA Science Inventory

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

  1. Computer Simulation of NMR Spectra.

    ERIC Educational Resources Information Center

    Ellison, A.

    1983-01-01

    Describes a PASCAL computer program which provides interactive analysis and display of high-resolution nuclear magnetic resonance (NMR) spectra from spin one-half nuclei using a hard-copy or monitor. Includes general and theoretical program descriptions, program capability, and examples of its use. (Source for program/documentation is included.)…

  2. Deuterium Exchange Kinetics by NMR.

    ERIC Educational Resources Information Center

    Roper, G. C.

    1985-01-01

    Describes a physical chemistry experiment which allows such concepts as kinetics, catalysis, isotope shifts, coupling constants, and the use of nuclear magnetic resonance (NMR) for quantitative work to be covered in the same exercise. Background information, experimental procedures used, and typical results obtained are included. (JN)

  3. Petrophysical applications of NMR imaging

    SciTech Connect

    Rothwell, W.P.; Vinegar, H.J.

    1985-12-01

    A system for obtaining high-resolution NMR images of oil field cores is described. Separate proton density and T/sub 2/ relaxation images are obtained to distinguish spatial variations of fluid-filled porosity and the physical nature of the pores. Results are presented for typical sandstones.

  4. Deuterium Exchange Kinetics by NMR.

    ERIC Educational Resources Information Center

    Roper, G. C.

    1985-01-01

    Describes a physical chemistry experiment which allows such concepts as kinetics, catalysis, isotope shifts, coupling constants, and the use of nuclear magnetic resonance (NMR) for quantitative work to be covered in the same exercise. Background information, experimental procedures used, and typical results obtained are included. (JN)

  5. Part I. Analyzing the distribution of gas law questions in chemistry textbooks. Part II. Chlorine-35 NQR spectra of group 1 and silver dichloromethanesulfonates

    NASA Astrophysics Data System (ADS)

    Gillette, Gabriel

    Part I. Two studies involving the gas law questions in eight high school and Advanced Placement/college chemistry textbooks were performed using loglinear analysis to look for associations among six variables. These variables included Bloom's Taxonomy (higher-order, lower-order), Book Type (high school, college), Question Format (multiple-choice, problem, short answer), Question Placement (in-chapter, end-of-chapter, test bank), Representation (macroscopic, microscopic, symbolic), and Arkansas Science Standard (conceptual, mathematical; gas laws, pressure conversion, stoichiometry). The first study, involving the conceptual gas law questions, found the Book Type and Question Placement variables had the biggest impact, each appearing in 5 of the 11 significant associations. The second study, involving the mathematical gas law questions, found the Question Placement had the biggest impact, appearing in 7 of the 11 significant associations, followed by Book Type and the Arkansas Science Standard variables, which appeared in 5 of the 11 significant associations. These studies showed that compared to the high school books, college books have fewer multiple-choice questions (compared to short-answer and problem questions), fewer in-chapter questions (compared to end-of-chapter and test bank questions), fewer questions in the chapters and more questions at the end of the chapters and fewer multiple-choice questions in and at the end of the books and more multiple-choice questions in the test banks. Part II. The dichloromethanesulfonate salts of several +1 charged cations, M+Cl2CHSO3 - (M = Li, Na, K, Rb Ag, Cs Tl) were synthesized and studied by 35Cl nuclear quadrupole resonance (NQR). Dichloromethanesulfonic acid was prepared by the methanolysis of dichloromethanesulfonyl chloride, which was neutralized with the metal carbonates to produce the corresponding metal dichloromethanesulfonate salts. This study completed the NQR investigation of the family of chloroacetates

  6. Intermetallic solid solution Fe{sub 1-x}Co{sub x}Ga{sub 3}: Synthesis, structure, NQR study and electronic band structure calculations

    SciTech Connect

    Verchenko, V.Yu.; Likhanov, M.S.; Kirsanova, M.A.; Gippius, A.A; Tkachev, A.V.; Gervits, N.E.; Galeeva, A.V.; Buettgen, N.; Kraetschmer, W.; Lue, C.S.; Okhotnikov, K.S.; Shevelkov, A.V.

    2012-10-15

    Unlimited solid solution Fe{sub 1-x}Co{sub x}Ga{sub 3} was prepared from Ga flux. Its crystal structure was refined for Fe{sub 0.5}Co{sub 0.5}Ga{sub 3} (P4{sub 2}/mnm, a=6.2436(9), c=6.4654(13), Z=4) and showed no ordering of the metal atoms. A combination of the electronic band structure calculations within the density functional theory (DFT) approach and {sup 69,71}Ga nuclear quadrupole resonance (NQR) spectroscopy clearly shows that the Fe-Fe and Co-Co dumbbells are preferred to the Fe-Co dumbbells in the crystals structure. The band structure features a band gap of about 0.4 eV, with the Fermi level crossing peaks of a substantial density of electronic states above the gap for x>0. The solid solution is metallic for x>0.025. The study of the nuclear spin-lattice relaxation shows that the rate of the relaxation, 1/T{sub 1}, is very sensitive to the Co concentration and correlates well with the square of the density of states at the Fermi level, N{sup 2}(E{sub F}). - Graphical abstract: Rate of the nuclear spin-lattice relaxation, 1/T{sub 1}, observed in the {sup 69}Ga NQR experiments for the intermetallic solid solution Fe{sub 1-x}Co{sub x}Ga{sub 3} is the highest for x=0.25 with the highest calculated density of electronic states at the Fermi level, N(E{sub F}); in general, 1/T{sub 1} correlates with N{sup 2}(E{sub F}). Highlights: Black-Right-Pointing-Pointer Fe{sub 1-x}Co{sub x}Ga{sub 3} solid solution is prepared in single crystalline form from Ga flux. Black-Right-Pointing-Pointer In the crystal structure Fe-Fe and Co-Co dumbbells are preferred to Fe-Co dumbbells. Black-Right-Pointing-Pointer Metal-to-semiconductor transition occurs at 0NQR spectra efficiently probe local environment of two independent Ga atoms. Black-Right-Pointing-Pointer Rate of nuclear spin-lattice relaxation follows squared DOS at the Fermi level.

  7. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1992-05-27

    This report covers the progress made on the title project for the project period. Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups that determine the reactivity of coals. Special attention is being paid to methods that are compatible with the very high magic angle sample spinning rates needed for operation at the high magnetic field strengths available today. Polarization inversion methods utilizing the difference in heat capacities of small groups of spins are particularly promising. Methods combining proton-proton spin diffusion with {sup 13}C CPMAS readout are being developed to determine the connectivity of functional groups in coals in a high sensitivity relay type of experiment. Additional work is aimed a delineating the role of methyl group rotation in the proton NMR relaxation behavior of coals.

  8. SEnD NMR: Sensitivity Enhanced n-Dimensional NMR

    NASA Astrophysics Data System (ADS)

    Gledhill, John M.; Wand, A. Joshua

    2010-02-01

    Sparse sampling offers tremendous potential for overcoming the time limitations imposed by traditional Cartesian sampling of indirectly detected dimensions of multidimensional NMR data. However, in many instances sensitivity rather than time remains of foremost importance when collecting data on protein samples. Here we explore how to optimize the collection of radial sampled multidimensional NMR data to achieve maximal signal-to-noise. A method is presented that exploits a rigorous definition of the minimal set of radial sampling angles required to resolve all peaks of interest in combination with a fundamental statistical property of radial sampled data. The approach appears general and can achieve a substantial sensitivity advantage over Cartesian sampling for the same total data acquisition time. Termed Sensitivity Enhanced n-Dimensional or SEnD NMR, the method involves three basic steps. First, data collection is optimized using routines to determine a minimal set of radial sampling angles required to resolve frequencies in the radially sampled chemical shift evolution dimensions. Second, appropriate combinations of experimental parameters (transients and increments) are defined by simple statistical considerations in order to optimize signal-to-noise in single angle frequency domain spectra. Finally, the data is processed with a direct multidimensional Fourier transform and a statistical artifact and noise removal step is employed.

  9. Two dimensional NMR and NMR relaxation studies of coal structure

    SciTech Connect

    Zilm, K.W.

    1989-01-01

    This report covers the progress made on the title project and summarizes the accomplishments for the project period. Four major areas of inquiry have been pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups in coals that determine the reactivity of coals. Other methods are being developed which will also determine how these functional groups are linked together. A third area of investigation concerns how molecular mobility in coals impacts NMR relaxation times, which is important for interpretation of such data in terms of the mobile phase in coal models. Along the same lines the author are also using these studies to establish protocols for obtaining the best quantitative response from coals in solid state C-13 NMR spectra. The effects of very high MAS rates (>10 kHz) on cross polarization dynamics are also being investigated for similar reasons. During the last quarter the authors has concentrated on improvements in cross polarization (CP) sequences with a goal of making the CP process insensitive to experimental conditions such as the Hartmann-Hahn mismatch. It has been found that the usual theories of CP are incorrect, and that the CP process is very heterogeneous in nature. This has significant implications on methods typically used in quantifying {sup 13}C CPMAS spectra of coals. 19 refs., 11 figs.

  10. Recognition of lumbar disk herniation with NMR

    SciTech Connect

    Chafetz, N.I.; Genant, H.K.; Moon, K.L.; Helms, C.A.; Morris, J.M.

    1983-12-01

    Fifteen nuclear magnetic resonance (NMR) studies of 14 patients with herniated lumbar intervertebral disks were performed on the UCSF NMR imager. Computed tomographic (CT) scans done on a GE CT/T 8800 or comparable scanner were available at the time of NMR scan interpretation. Of the 16 posterior disk ruptures seen at CT, 12 were recognized on NMR. Diminished nucleus pulposus signal intensity was present in all ruptured disks. In one patient, NMR scans before and after chymopapain injection showed retraction of the protruding part of the disk and loss of signal intensity after chemonucleolysis. Postoperative fibrosis demonstrated by CT in one patient and at surgery in another showed intermediate to high signal intensity on NMR, easily distinguishing it from nearby thecal sac and disk. While CT remains the method of choice for evaluation of the patient with suspected lumbar disk rupture, the results of this study suggest that NMR may play a role in evaluating this common clinical problem.

  11. Sorption isotherm measurements by NMR.

    PubMed

    Leisen, Johannes; Beckham, Haskell W; Benham, Michael

    2002-01-01

    An experimental setup is described for the automated recording of sorption isotherms by NMR experiments at precisely defined levels of relative humidity (RH). Implementation is demonstrated for a cotton fabric; Bloch decays. T1 and T2* relaxation times were measured at predefined steps of increasing and decreasing relative humidities (RHs) so that a complete isotherm of NMR properties was obtained. Bloch decays were analyzed by fitting to relaxation functions consisting or a slow- and a fast-relaxing component. The fraction of slow-relaxing component was greater than the fraction of sorbed moisture determined from gravimetric sorption data. The excess slow-relaxing component was attributed to plasticized segments of the formerly rigid cellulose matrix. T1 and T2* sorption isotherms exhibit hysteresis similar to gravimetric sorption isotherms. However, correlating RH to moisture content (MC) reveals that both relaxation constants depend only on MC, and not on the history of moisture exposure.

  12. Two-dimensional NMR spectrometry

    SciTech Connect

    Farrar, T.C.

    1987-06-01

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

  13. Functional Studies on Membrane Proteins by Means of H/D Exchange in Infrared: Structural Changes in Na(+) NQR from V. cholerae in the Presence of Lipids.

    PubMed

    Neehaul, Yashvin; Kriegel, Sebastien; Barquera, Blanca; Hellwig, Petra

    2017-01-01

    H/D exchange kinetics at the level of the amide proton in the mid infrared (1700-1500 cm(-1)) make it possible to study the conformational flexibility of membrane proteins, independent of size or the presence of detergent or lipids. Slow, medium, and fast exchanging domains are distinguished, which reveal a different accessibility to the solvent. Whereas amide hydrogens undergo rapid exchange with solvent in an open structure, hydrogens experience much slower exchange when involved in H-bonded structures or when sterically inaccessible to the solvent. Here, we describe the protocol that was used to study the effect of phospholipids on the overall structure of the Na(+) NQR from V. cholerae, a sodium pumping membrane protein.

  14. NMR Hyperpolarization Techniques for Biomedicine

    PubMed Central

    Nikolaou, Panayiotis; Goodson, Boyd M.

    2015-01-01

    Recent developments in NMR hyperpolarization have enabled a wide array of new in vivo molecular imaging modalities—ranging from functional imaging of the lungs to metabolic imaging of cancer. This Concept article explores selected advances in methods for the preparation and use of hyperpolarized contrast agents, many of which are already at or near the phase of their clinical validation in patients. PMID:25470566

  15. Hyperpolarized 131Xe NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Stupic, Karl F.; Cleveland, Zackary I.; Pavlovskaya, Galina E.; Meersmann, Thomas

    2011-01-01

    Hyperpolarized (hp) 131Xe with up to 2.2% spin polarization (i.e., 5000-fold signal enhancement at 9.4 T) was obtained after separation from the rubidium vapor of the spin-exchange optical pumping (SEOP) process. The SEOP was applied for several minutes in a stopped-flow mode, and the fast, quadrupolar-driven T1 relaxation of this spin I = 3/2 noble gas isotope required a rapid subsequent rubidium removal and swift transfer into the high magnetic field region for NMR detection. Because of the xenon density dependent 131Xe quadrupolar relaxation in the gas phase, the SEOP polarization build-up exhibits an even more pronounced dependence on xenon partial pressure than that observed in 129Xe SEOP. 131Xe is the only stable noble gas isotope with a positive gyromagnetic ratio and shows therefore a different relative phase between hp signal and thermal signal compared to all other noble gases. The gas phase 131Xe NMR spectrum displays a surface and magnetic field dependent quadrupolar splitting that was found to have additional gas pressure and gas composition dependence. The splitting was reduced by the presence of water vapor that presumably influences xenon-surface interactions. The hp 131Xe spectrum shows differential line broadening, suggesting the presence of strong adsorption sites. Beyond hp 131Xe NMR spectroscopy studies, a general equation for the high temperature, thermal spin polarization, P, for spin I⩾1/2 nuclei is presented.

  16. Hyperpolarized 131Xe NMR spectroscopy

    PubMed Central

    Stupic, Karl F.; Cleveland, Zackary I.; Pavlovskaya, Galina E.; Meersmann, Thomas

    2011-01-01

    Hyperpolarized (hp) 131Xe with up to 2.2% spin polarization (i.e., 5000-fold signal enhancement at 9.4 T) was obtained after separation from the rubidium vapor of the spin-exchange optical pumping (SEOP) process. The SEOP was applied for several minutes in a stopped-flow mode, and the fast, quadrupolar-driven T1 relaxation of this spin I = 3/2 noble gas isotope required a rapid subsequent rubidium removal and swift transfer into the high magnetic field region for NMR detection. Because of the xenon density dependent 131Xe quadrupolar relaxation in the gas phase, the SEOP polarization build-up exhibits an even more pronounced dependence on xenon partial pressure than that observed in 129Xe SEOP. 131Xe is the only stable noble gas isotope with a positive gyromagnetic ratio and shows therefore a different relative phase between hp signal and thermal signal compared to all other noble gases. The gas phase 131Xe NMR spectrum displays a surface and magnetic field dependent quadrupolar splitting that was found to have additional gas pressure and gas composition dependence. The splitting was reduced by the presence of water vapor that presumably influences xenon-surface interactions. The hp 131Xe spectrum shows differential line broadening, suggesting the presence of strong adsorption sites. Beyond hp 131Xe NMR spectroscopy studies, a general equation for the high temperature, thermal spin polarization, P, for spin I⩾1/2 nuclei is presented. PMID:21051249

  17. Microcoil NMR spectroscopy: a novel tool for biological high throughput NMR spectroscopy.

    PubMed

    Hopson, Russell E; Peti, Wolfgang

    2008-01-01

    Microcoil NMR spectroscopy is based on the increase of coil sensitivity for smaller coil diameters (approximately 1/d). Microcoil NMR probes deliver a remarkable mass-based sensitivity increase (8- to 12-fold) when compared with commonly used 5-mm NMR probes. Although microcoil NMR probes are a well established analytical tool for small molecule liquid-state NMR spectroscopy, after spectroscopy only recently have microcoil NMR probes become available for biomolecular NMR spectroscopy. This chapter highlights differences between commercially available microcoil NMR probes suitable for biomolecular NMR spectroscopy. Furthermore, it provides practical guidance for the use of microcoil probes and shows direct applications for structural biology and structural genomics, such as optimal target screening and structure determination, among others.

  18. Advanced NMR technology for bioscience and biotechnology

    SciTech Connect

    Hammel, P.C.; Hernandez, G.; Trewhella, J.; Unkefer, C.J.; Boumenthal, D.K.; Kennedy, M.A.; Moore, G.J.

    1998-11-01

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

  19. Scalable NMR spectroscopy with semiconductor chips

    PubMed Central

    Ha, Dongwan; Paulsen, Jeffrey; Sun, Nan; Song, Yi-Qiao; Ham, Donhee

    2014-01-01

    State-of-the-art NMR spectrometers using superconducting magnets have enabled, with their ultrafine spectral resolution, the determination of the structure of large molecules such as proteins, which is one of the most profound applications of modern NMR spectroscopy. Many chemical and biotechnological applications, however, involve only small-to-medium size molecules, for which the ultrafine resolution of the bulky, expensive, and high-maintenance NMR spectrometers is not required. For these applications, there is a critical need for portable, affordable, and low-maintenance NMR spectrometers to enable in-field, on-demand, or online applications (e.g., quality control, chemical reaction monitoring) and co-use of NMR with other analytical methods (e.g., chromatography, electrophoresis). As a critical step toward NMR spectrometer miniaturization, small permanent magnets with high field homogeneity have been developed. In contrast, NMR spectrometer electronics capable of modern multidimensional spectroscopy have thus far remained bulky. Complementing the magnet miniaturization, here we integrate the NMR spectrometer electronics into 4-mm2 silicon chips. Furthermore, we perform various multidimensional NMR spectroscopies by operating these spectrometer electronics chips together with a compact permanent magnet. This combination of the spectrometer-electronics-on-a-chip with a permanent magnet represents a useful step toward miniaturization of the overall NMR spectrometer into a portable platform. PMID:25092330

  20. Solid-state NMR of inorganic semiconductors.

    PubMed

    Yesinowski, James P

    2012-01-01

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

  1. Microscopic studies on Y{sub 2}Ba{sub 4}Cu{sub 7}O{sub 15{minus}{delta}} by use of TEM and NQR techniques

    SciTech Connect

    Kato, Masaki; Nakanishi, Makoto; Yoshimura, Kazuyoshi; Kosuge, Koji; Miyano, Toshio; Shimizu, Tadashi; Kakihana, Masato

    1998-09-01

    Y{sub 2}Ba{sub 4}Cu{sub 7}O{sub 15{minus}{delta}} compounds were characterized by microscopic investigation using TEM and NQR techniques. The authors synthesized Y247 compounds by two kinds of preparation methods: the conventional solid-state reaction (sample A) and the polymerized-complex method (sample B). The value of T{sub c} for sample A was found o be 65 K and that for sample B as 93 K by ac-{chi} measurements. As a result of TEM experiments, stacking faults along the c axis were observed more frequently in sample B than in sample A. These stacking faults resulted in microdomains containing pure Y123 or Y124 thin blocks of several unit cells. NQR experiments revealed that the microscopic environment of Cu(2) sites in sample A differed from either of those in the Y123 and Y124 compounds. NQR frequency values ({nu}{sub Q}) of Cu(2) sites agreed well with those calculated by the point charge model applied for the Y247 structure. The spectra of Cu(2) sites in sample B could be regarded, however, as a combination of those of pure Y123, Y124, and also Y247 compounds. This fact was coincident with the result of TEM experiments. The authors concluded that the superconductivity of Y247 with higher T{sub c} originates from the thin block of Y123.

  2. Development of LC-13C NMR

    NASA Technical Reports Server (NTRS)

    Dorn, H. C.; Wang, J. S.; Glass, T. E.

    1986-01-01

    This study involves the development of C-13 nuclear resonance as an on-line detector for liquid chromatography (LC-C-13 NMR) for the chemical characterization of aviation fuels. The initial focus of this study was the development of a high sensitivity flow C-13 NMR probe. Since C-13 NMR sensitivity is of paramount concern, considerable effort during the first year was directed at new NMR probe designs. In particular, various toroid coil designs were examined. In addition, corresponding shim coils for correcting the main magnetic field (B sub 0) homogeneity were examined. Based on these initial probe design studies, an LC-C-13 NMR probe was built and flow C-13 NMR data was obtained for a limited number of samples.

  3. Observation of NMR noise from solid samples

    PubMed Central

    Schlagnitweit, Judith; Dumez, Jean-Nicolas; Nausner, Martin; Jerschow, Alexej; Elena-Herrmann, Bénédicte; Müller, Norbert

    2010-01-01

    We demonstrate that proton NMR noise signals, i.e. NMR spectra without excitation by radio frequency, can be obtained from solid samples. Experimental results are shown for static and magic-angle spinning conditions. In addition, a tuning procedure based on the probes’ NMR noise characteristics and similar to the one described previously for liquids probes can also be used to optimize signal-to-noise ratios in 1H-MAS experiments. PMID:20850362

  4. Solid-state NMR spectroscopy of proteins.

    PubMed

    Müller, Henrik; Etzkorn, Manuel; Heise, Henrike

    2013-01-01

    Solid-state NMR spectroscopy proved to be a versatile tool for characterization of structure and dynamics of complex biochemical systems. In particular, magic angle spinning (MAS) solid-state NMR came to maturity for application towards structural elucidation of biological macromolecules. Current challenges in applying solid-state NMR as well as progress achieved recently will be discussed in the following chapter focusing on conceptual aspects important for structural elucidation of proteins.

  5. Solid-state NMR and Membrane Proteins

    PubMed Central

    Opella, Stanley J.

    2015-01-01

    The native environment for a membrane protein is a phospholipid bilayer. Because the protein is immobilized on NMR timescales by the interactions within a bilayer membrane, solid-state NMR methods are essential to obtain high-resolution spectra. Approaches have been developed for both unoriented and oriented samples, however, they all rest on the foundation of the most fundamental aspects solid-state NMR, and the chemical shift and homo- and hetero-nuclear dipole-dipole interactions. Solid-state NMR has advanced sufficiently to enable the structures of membrane proteins to be determined under near-native conditions in phospholipid bilayers. PMID:25681966

  6. Solid-state NMR and membrane proteins

    NASA Astrophysics Data System (ADS)

    Opella, Stanley J.

    2015-04-01

    The native environment for a membrane protein is a phospholipid bilayer. Because the protein is immobilized on NMR timescales by the interactions within a bilayer membrane, solid-state NMR methods are essential to obtain high-resolution spectra. Approaches have been developed for both unoriented and oriented samples, however, they all rest on the foundation of the most fundamental aspects of solid-state NMR, and the chemical shift and homo- and hetero-nuclear dipole-dipole interactions. Solid-state NMR has advanced sufficiently to enable the structures of membrane proteins to be determined under near-native conditions in phospholipid bilayers.

  7. Quantitative 2D liquid-state NMR.

    PubMed

    Giraudeau, Patrick

    2014-06-01

    Two-dimensional (2D) liquid-state NMR has a very high potential to simultaneously determine the absolute concentration of small molecules in complex mixtures, thanks to its capacity to separate overlapping resonances. However, it suffers from two main drawbacks that probably explain its relatively late development. First, the 2D NMR signal is strongly molecule-dependent and site-dependent; second, the long duration of 2D NMR experiments prevents its general use for high-throughput quantitative applications and affects its quantitative performance. Fortunately, the last 10 years has witnessed an increasing number of contributions where quantitative approaches based on 2D NMR were developed and applied to solve real analytical issues. This review aims at presenting these recent efforts to reach a high trueness and precision in quantitative measurements by 2D NMR. After highlighting the interest of 2D NMR for quantitative analysis, the different strategies to determine the absolute concentrations from 2D NMR spectra are described and illustrated by recent applications. The last part of the manuscript concerns the recent development of fast quantitative 2D NMR approaches, aiming at reducing the experiment duration while preserving - or even increasing - the analytical performance. We hope that this comprehensive review will help readers to apprehend the current landscape of quantitative 2D NMR, as well as the perspectives that may arise from it.

  8. NMR studies of isotopically labeled RNA

    SciTech Connect

    Pardi, A.

    1994-12-01

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

  9. Analytical Applications of NMR: Summer Symposium on Analytical Chemistry.

    ERIC Educational Resources Information Center

    Borman, Stuart A.

    1982-01-01

    Highlights a symposium on analytical applications of nuclear magnetic resonance spectroscopy (NMR), discussing pulse Fourier transformation technique, two-dimensional NMR, solid state NMR, and multinuclear NMR. Includes description of ORACLE, an NMR data processing system at Syracuse University using real-time color graphics, and algorithms for…

  10. Analytical Applications of NMR: Summer Symposium on Analytical Chemistry.

    ERIC Educational Resources Information Center

    Borman, Stuart A.

    1982-01-01

    Highlights a symposium on analytical applications of nuclear magnetic resonance spectroscopy (NMR), discussing pulse Fourier transformation technique, two-dimensional NMR, solid state NMR, and multinuclear NMR. Includes description of ORACLE, an NMR data processing system at Syracuse University using real-time color graphics, and algorithms for…

  11. Access to NMR Spectroscopy for Two-Year College Students: The NMR Site at Trinity University

    ERIC Educational Resources Information Center

    Mills, Nancy S.; Shanklin, Michael

    2011-01-01

    Students at two-year colleges and small four-year colleges have often obtained their exposure to NMR spectroscopy through "canned" spectra because the cost of an NMR spectrometer, particularly a high-field spectrometer, is prohibitive in these environments. This article describes the design of a NMR site at Trinity University in which…

  12. rNMR: open source software for identifying and quantifying metabolites in NMR spectra

    PubMed Central

    Lewis, Ian A; Schommer, Seth C; Markley, John L

    2009-01-01

    Despite the extensive use of nuclear magnetic resonance (NMR) for metabolomics, no publicly available tools have been designed for identifying and quantifying metabolites across multiple spectra. We introduce here a new open source software tool, rNMR, which provides a simple graphics-based method for visualizing, identifying, and quantifying metabolites across multiple one- or two-dimensional NMR spectra. rNMR differs from existing software tools for NMR spectroscopy in that analyses are based on regions of interest (ROIs) rather than peak lists. ROIs contain all of the underlying NMR data within user-defined chemical shift ranges. ROIs can be inspected visually, and they support robust quantification of NMR signals. ROI-based analyses support simultaneous views of metabolite signals from up to hundreds of spectra, and ROI boundaries can be adjusted dynamically to ensure that signals corresponding to assigned atoms are analyzed consistently throughout the dataset. We describe how rNMR greatly reduces the time required for robust bioanalytical analysis of complex NMR data. An rNMR analysis yields a compact and transparent way of archiving the results from a metabolomics study so that it can be examined and evaluated by others. The rNMR website at http://rnmr.nmrfam.wisc.edu offers downloadable versions of rNMR for Windows, Macintosh, and Linux platforms along with extensive help documentation, instructional videos, and sample data. Copyright © 2009 John Wiley & Sons, Ltd. PMID:19821464

  13. jsNMR: an embedded platform-independent NMR spectrum viewer.

    PubMed

    Vosegaard, Thomas

    2015-04-01

    jsNMR is a lightweight NMR spectrum viewer written in JavaScript/HyperText Markup Language (HTML), which provides a cross-platform spectrum visualizer that runs on all computer architectures including mobile devices. Experimental (and simulated) datasets are easily opened in jsNMR by (i) drag and drop on a jsNMR browser window, (ii) by preparing a jsNMR file from the jsNMR web site, or (iii) by mailing the raw data to the jsNMR web portal. jsNMR embeds the original data in the HTML file, so a jsNMR file is a self-transforming dataset that may be exported to various formats, e.g. comma-separated values. The main applications of jsNMR are to provide easy access to NMR data without the need for dedicated software installed and to provide the possibility to visualize NMR spectra on web sites. Copyright © 2015 John Wiley & Sons, Ltd.

  14. Access to NMR Spectroscopy for Two-Year College Students: The NMR Site at Trinity University

    ERIC Educational Resources Information Center

    Mills, Nancy S.; Shanklin, Michael

    2011-01-01

    Students at two-year colleges and small four-year colleges have often obtained their exposure to NMR spectroscopy through "canned" spectra because the cost of an NMR spectrometer, particularly a high-field spectrometer, is prohibitive in these environments. This article describes the design of a NMR site at Trinity University in which…

  15. Picoliter H-1 NMR Spectroscopy

    SciTech Connect

    Minard, Kevin R. ); Wind, Robert A. )

    2002-02-01

    A RF probe that fits inside the bore of a small gradient coil package is described for routine 1H-NMR microscopy measurements on small samples. The probe operates at 500 MHz and houses a 267-um-diameter solenoid transceiver. When used in three dimensional chemical shift imaging (3D-CSI) experiments, the measured signal-to-noise ratio (SNR) is shown to be within 20-30 percent of theoretical limits formulated by only considering the solenoid's resistive losses. This is illustrated using a 100-um-diameter globule of triacylglycerols ({approx}900mM) that may be an oocyte precursor in young Xenopus Laevis frogs, and water sample containing choline at a concentration often found in live cells ({approx}33mM). In chemical shift images generated using a few thousand scans, the choline methyl line is found to have an acceptable SNR in resolved from just 5 picoliters in the Xenopus globule. It is concluded that the probe's sensitivity is sufficient for performing 1H-NMR on picoliter-scale volumes in biological cells and tissues.

  16. NMR studies of oriented molecules

    SciTech Connect

    Sinton, S.W.

    1981-11-01

    Deuterium and proton magnetic resonance are used in experiments on a number of compounds which either form liquid crystal mesophases themselves or are dissolved in a liquid crystal solvent. Proton multiple quantum NMR is used to simplify complicated spectra. The theory of nonselective multiple quantum NMR is briefly reviewed. Benzene dissolved in a liquid crystal are used to demonstrate several outcomes of the theory. Experimental studies include proton and deuterium single quantum (..delta..M = +-1) and proton multiple quantum spectra of several molecules which contain the biphenyl moiety. 4-Cyano-4'-n-pentyl-d/sub 11/-biphenyl (5CB-d/sub 11/) is studied as a pure compound in the nematic phase. The obtained chain order parameters and dipolar couplings agree closely with previous results. Models for the effective symmetry of the biphenyl group in 5CB-d/sub 11/ are tested against the experimental spectra. The dihedral angle, defined by the planes containing the rings of the biphenyl group, is found to be 30 +- 2/sup 0/ for 5DB-d/sub 11/. Experiments are also described for 4,4'-d/sub 2/-biphenyl, 4,4' - dibromo-biphenyl, and unsubstituted biphenyl.

  17. Proton and deuterium NMR experiments in zero field. [Perdeuterated p-demethoxybenzene, perdeuterated malonic acid, diethyl terephthalate-d4, nonadecane-2,2'-D2, sodium propionate-D2

    SciTech Connect

    Millar, J.M.

    1986-02-01

    High field solid-state NMR lineshapes suffer from inhomogeneous broadening since resonance frequencies are a function of molecular orientation. Time domain zero field NMR is a two-dimensional field-cycling technique which removes this broadening by probing the evolution of the spin system under zero applied field. The simplest version, the sudden transition experiment, induces zero field evolution by the sudden removal of the applied magnetic field. Theory and experimental results of this experiment and several variations using pulsed dc magnetic fuelds to initiate zero field evolution are presented. In particular, the pulsed indirect detection method allows detection of the zero field spectrum of one nuclear spin species via another (usually protons) by utilizing the level crossings which occur upon adiabatic demagnetization to zero field. Experimental examples of proton/deuteron systems are presented which demonstrate the method results in enhanced sensitivity relative to that obtained in sudden transition experiments performed directly on deuterium. High resolution /sup 2/H NQR spectra of a series of benzoic acid derivatives are obtained using the sudden transition and indirect detection methods. Librational oscillations in the water molecules of barium chlorate monohydrate are studied using proton and deuterium ZF experiments. 177 refs., 88 figs., 2 tabs.

  18. NMR studies of the internal electric field in a single crystal of the quasi-one-dimensional conductor Li0.9Mo6O17

    NASA Astrophysics Data System (ADS)

    Wu, Guoqing; Wu, Bing

    2015-03-01

    The quasi-one-dimensional (Q1D) conductor Li0.9Mo6O17 is of considerable interest because it has a highly conducting phase with properties likely associated with a Luttinger liquid, a poorly understood ``metal-insulator'' crossover at temperature TMI = 24 K, and a 3D superconducting phase that may involve triplet Cooper pairs at Tc = 2.2 K, while the mechanism for many of its properties has been a long mystery and it presents tremendous experimental challenges. We report the 7Li-NMR measurements of the internal electric field with an externally applied magnetic field B0 = 9 - 12 T, and we also show our theoretically calculated result of the electric field based on the structure of the crystal lattice. We find that the 7Li-NQR frequency (νQ) has a value of ~ 45 kHz and the electric field gradient (EFG) at the Li site due to the charges of the surrounding Mo conduction electrons has an axial symmetry with the principle axis (pz) to be along the lattice a-axis. There is no temperature or field dependence for the value of νQ or EFG, indicating that the ``metal-insulator'' crossover has a magnetic origin, rather than the charge density wave (CDW) as one of the possible mechanisms previously thought in literature.

  19. An Integrated Laboratory Project in NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Hudson, Reggie L.; Pendley, Bradford D.

    1988-01-01

    Describes an advanced NMR project that can be done with a 60-MHz continuous-wave proton spectrometer. Points out the main purposes are to give students experience in second-order NMR analysis, the simplification of spectra by raising the frequency, and the effect of non-hydrogen nuclei on proton resonances. (MVL)

  20. An Inversion Recovery NMR Kinetics Experiment

    ERIC Educational Resources Information Center

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this…

  1. NMR-Profiles of Protein Solutions

    PubMed Central

    Pedrini, Bill; Serrano, Pedro; Mohanty, Biswaranjan; Geralt, Michael; Wüthrich, Kurt

    2014-01-01

    NMR-Profiles are quantitative one-dimensional presentations of two-dimensional [15N,1H]-correlation spectra used to monitor the quality of protein solutions prior to and during NMR structure determinations and functional studies. In our current use in structural genomics projects, a NMR-Profile is recorded at the outset of a structure determination, using a uniformly 15N-labeled micro-scale sample of the protein. We thus assess the extent to which polypeptide backbone resonance assignments can be achieved with given NMR techniques, for example, conventional triple resonance experiments or APSY-NMR. With the availability of sequence-specific polypeptide backbone resonance assignments in the course of the structure determination, an “Assigned NMR-Profile” is generated, which visualizes the variation of the 15N–1H correlation cross peak intensities along the sequence and thus maps the sequence locations of polypeptide segments for which the NMR line shapes are affected by conformational exchange or other processes. The Assigned NMR-Profile provides a guiding reference during later stages of the structure determination, and is of special interest for monitoring the protein during functional studies, where dynamic features may be modulated during physiological functions. PMID:23839514

  2. An Integrated Laboratory Project in NMR Spectroscopy.

    ERIC Educational Resources Information Center

    Hudson, Reggie L.; Pendley, Bradford D.

    1988-01-01

    Describes an advanced NMR project that can be done with a 60-MHz continuous-wave proton spectrometer. Points out the main purposes are to give students experience in second-order NMR analysis, the simplification of spectra by raising the frequency, and the effect of non-hydrogen nuclei on proton resonances. (MVL)

  3. NMR Spectroscopy and Its Value: A Primer

    ERIC Educational Resources Information Center

    Veeraraghavan, Sudha

    2008-01-01

    Nuclear magnetic resonance (NMR) spectroscopy is widely used by chemists. Furthermore, the use of NMR spectroscopy to solve structures of macromolecules or to examine protein-ligand interactions is popular. Yet, few students entering graduate education in biological sciences have been introduced to this method or its utility. Over the last six…

  4. A Guided Inquiry Approach to NMR Spectroscopy

    NASA Astrophysics Data System (ADS)

    Parmentier, Laura E.; Lisensky, George C.; Spencer, Brock

    1998-04-01

    We present a novel way to introduce NMR spectroscopy into the general chemistry curriculum as part of a week-long aspirin project in our one-semester introductory course. Aspirin is synthesized by reacting salicylic acid and acetic anhydride. Purity is determined by titration and IR and NMR spectroscopy. Students compare IR and NMR spectra of their aspirin product to a series of reference spectra obtained by the class. Students are able to interpret the IR spectra of their aspirin using IR data from previous experiments. NMR is introduced by having students collect 1H NMR spectra of a series of reference compounds chosen to include some of the structural features of aspirin and compare spectra and structures of the reference compounds to develop a correlation chart for chemical shifts. This process is done in small groups using shared class data and is guided by a series of questions designed to relate the different kinds of hydrogen atoms to number and position of peaks in the NMR spectrum. Students then identify the peaks in the NMR spectrum of their aspirin product and relate percent purity by titration with spectral results and percent yield. This is an enjoyable project that combines the synthesis of a familiar material with a guided inquiry-based introduction to NMR spectroscopy.

  5. Using Cloud Storage for NMR Data Distribution

    ERIC Educational Resources Information Center

    Soulsby, David

    2012-01-01

    An approach using Google Groups as method for distributing student-acquired NMR data has been implemented. We describe how to configure NMR spectrometer software so that data is uploaded to a laboratory section specific Google Group, thereby removing bottlenecks associated with printing and processing at the spectrometer workstation. Outside of…

  6. Microslot NMR probe for metabolomics studies.

    PubMed

    Krojanski, Hans Georg; Lambert, Jörg; Gerikalan, Yilmaz; Suter, Dieter; Hergenröder, Roland

    2008-11-15

    A NMR microprobe based on microstrip technology suitable for investigations of volume-limited samples in the low nanoliter range was designed. NMR spectra of sample quantities in the 100 pmol range can be obtained with this probe in a few seconds. The planar geometry of the probe is easily adaptable to the size and geometry requirements of the samples.

  7. An Inversion Recovery NMR Kinetics Experiment

    ERIC Educational Resources Information Center

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this…

  8. NMR Spectroscopy and Its Value: A Primer

    ERIC Educational Resources Information Center

    Veeraraghavan, Sudha

    2008-01-01

    Nuclear magnetic resonance (NMR) spectroscopy is widely used by chemists. Furthermore, the use of NMR spectroscopy to solve structures of macromolecules or to examine protein-ligand interactions is popular. Yet, few students entering graduate education in biological sciences have been introduced to this method or its utility. Over the last six…

  9. Using Cloud Storage for NMR Data Distribution

    ERIC Educational Resources Information Center

    Soulsby, David

    2012-01-01

    An approach using Google Groups as method for distributing student-acquired NMR data has been implemented. We describe how to configure NMR spectrometer software so that data is uploaded to a laboratory section specific Google Group, thereby removing bottlenecks associated with printing and processing at the spectrometer workstation. Outside of…

  10. NMR investigations of hydrogen in carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Schmid, M.; Goze-Bac, C.; Krämer, S.; Mehring, M.; Roth, S.; Bernier, P.

    2002-10-01

    We report proton nuclear magnetic resonance (1H-NMR) measurements on hydrogen loaded single walled carbon nanotubes. The carbon nanotubes were produced with different kinds of catalysts and hydrogen loaded under 23 bar hydrogen pressure. The hydrogen adsorption properties of the carbon nanotube materials were investigated by temperature dependent analysis of the 1H-NMR spectra.

  11. Challenges and perspectives in quantitative NMR.

    PubMed

    Giraudeau, Patrick

    2017-01-01

    This perspective article summarizes, from the author's point of view at the beginning of 2016, the major challenges and perspectives in the field of quantitative NMR. The key concepts in quantitative NMR are first summarized; then, the most recent evolutions in terms of resolution and sensitivity are discussed, as well as some potential future research directions in this field. A particular focus is made on methodologies capable of boosting the resolution and sensitivity of quantitative NMR, which could open application perspectives in fields where the sample complexity and the analyte concentrations are particularly challenging. These include multi-dimensional quantitative NMR and hyperpolarization techniques such as para-hydrogen-induced polarization or dynamic nuclear polarization. Because quantitative NMR cannot be dissociated from the key concepts of analytical chemistry, i.e. trueness and precision, the methodological developments are systematically described together with their level of analytical performance. Copyright © 2016 John Wiley & Sons, Ltd.

  12. NMR imaging techniques and applications: A review

    NASA Astrophysics Data System (ADS)

    Bottomley, Paul A.

    1982-09-01

    Over the past ten years, a variety of techniques have been proposed and demonstrated that enable the spatial discrimination and mapping of nuclear-magnetic-resonance (NMR) signals in heterogeneous objects. These NMR imaging techniques are currently finding useful application in clinical medicine and physiological chemistry, where their noninvasive, apparently hazard-free nature, and the sensitivity of the NMR signal to the state of biological tissue, are key advantages. This article reviews the historical development, the conceptual basis, and the applications of the various NMR imaging techniques. Qualitative descriptions and illustrations of each technique and an outline of imaging instrumentation are provided. Proton NMR imaging, in medicine, of pathological states such as cancer, imaging of relaxation time, chemical shift and flow parameters, imaging of nuclei other than hydrogen, and potential hazards are discussed and demonstrated with examples.

  13. Rapid sample injection for hyperpolarized NMR spectroscopy.

    PubMed

    Bowen, Sean; Hilty, Christian

    2010-06-14

    Due to its ability to enhance the signal of a single NMR scan by several orders of magnitude, solid-to-liquid state dynamic nuclear polarization (DNP) appears well suited for the analysis of minimal amounts of compounds, as well as for the study of rapid chemical reactions. A key requirement in enabling the application of DNP-NMR to typical small-molecule substances encountered in chemistry and biochemistry is the ability to obtain high-resolution spectra, while at the same time minimizing the loss of polarization due to spin relaxation between the separate steps of DNP polarization and NMR measurement. Here, we present data demonstrating the capability of measuring DNP enhanced NMR spectra of compounds with comparably short relaxation times, with only minimal line broadening attributable to the sample transfer process. We discuss the performance characteristics of a sample injection apparatus specifically designed to provide high-resolution DNP-NMR spectra of small molecule compounds.

  14. NMR and MRI apparatus and method

    DOEpatents

    Clarke, John; Kelso, Nathan; Lee, SeungKyun; Moessle, Michael; Myers, Whittier; McDermott, Robert; ten Haken, Bernard; Pines, Alexander; Trabesinger, Andreas

    2007-03-06

    Nuclear magnetic resonance (NMR) signals are detected in microtesla fields. Prepolarization in millitesla fields is followed by detection with an untuned dc superconducting quantum interference device (SQUID) magnetometer. Because the sensitivity of the SQUID is frequency independent, both signal-to-noise ratio (SNR) and spectral resolution are enhanced by detecting the NMR signal in extremely low magnetic fields, where the NMR lines become very narrow even for grossly inhomogeneous measurement fields. Additional signal to noise benefits are obtained by use of a low noise polarization coil, comprising litz wire or superconducting materials. MRI in ultralow magnetic field is based on the NMR at ultralow fields. Gradient magnetic fields are applied, and images are constructed from the detected NMR signals.

  15. Unilateral NMR with a barrel magnet.

    PubMed

    Utsuzawa, Shin; Fukushima, Eiichi

    2017-09-01

    Unilateral NMR can examine samples without regard to sample size. It is also an easy path to mobile or portable NMR as well as inexpensive NMR. The objective of this work was to develop unilateral NMR with an improved performance in a sample region that was remote from the apparatus. This was accomplished with the creation of a saddle point where all second derivatives of the main component of the field were nulled. A ∼10cm diameter ∼5cm thick magnet combined with a gradiometer coil on the surface detected signals from a sensitive region that extended ∼2cm from the magnet. The relatively homogeneous field of these unilateral NMR devices allows the measurement of rapidly diffusing spins as well as the use of smaller RF amplifiers, which enhances system mobility. Copyright © 2017 Elsevier Inc. All rights reserved.

  16. Robust, integrated computational control of NMR experiments to achieve optimal assignment by ADAPT-NMR.

    PubMed

    Bahrami, Arash; Tonelli, Marco; Sahu, Sarata C; Singarapu, Kiran K; Eghbalnia, Hamid R; Markley, John L

    2012-01-01

    ADAPT-NMR (Assignment-directed Data collection Algorithm utilizing a Probabilistic Toolkit in NMR) represents a groundbreaking prototype for automated protein structure determination by nuclear magnetic resonance (NMR) spectroscopy. With a [(13)C,(15)N]-labeled protein sample loaded into the NMR spectrometer, ADAPT-NMR delivers complete backbone resonance assignments and secondary structure in an optimal fashion without human intervention. ADAPT-NMR achieves this by implementing a strategy in which the goal of optimal assignment in each step determines the subsequent step by analyzing the current sum of available data. ADAPT-NMR is the first iterative and fully automated approach designed specifically for the optimal assignment of proteins with fast data collection as a byproduct of this goal. ADAPT-NMR evaluates the current spectral information, and uses a goal-directed objective function to select the optimal next data collection step(s) and then directs the NMR spectrometer to collect the selected data set. ADAPT-NMR extracts peak positions from the newly collected data and uses this information in updating the analysis resonance assignments and secondary structure. The goal-directed objective function then defines the next data collection step. The procedure continues until the collected data support comprehensive peak identification, resonance assignments at the desired level of completeness, and protein secondary structure. We present test cases in which ADAPT-NMR achieved results in two days or less that would have taken two months or more by manual approaches.

  17. Robust, Integrated Computational Control of NMR Experiments to Achieve Optimal Assignment by ADAPT-NMR

    PubMed Central

    Bahrami, Arash; Tonelli, Marco; Sahu, Sarata C.; Singarapu, Kiran K.; Eghbalnia, Hamid R.; Markley, John L.

    2012-01-01

    ADAPT-NMR (Assignment-directed Data collection Algorithm utilizing a Probabilistic Toolkit in NMR) represents a groundbreaking prototype for automated protein structure determination by nuclear magnetic resonance (NMR) spectroscopy. With a [13C,15N]-labeled protein sample loaded into the NMR spectrometer, ADAPT-NMR delivers complete backbone resonance assignments and secondary structure in an optimal fashion without human intervention. ADAPT-NMR achieves this by implementing a strategy in which the goal of optimal assignment in each step determines the subsequent step by analyzing the current sum of available data. ADAPT-NMR is the first iterative and fully automated approach designed specifically for the optimal assignment of proteins with fast data collection as a byproduct of this goal. ADAPT-NMR evaluates the current spectral information, and uses a goal-directed objective function to select the optimal next data collection step(s) and then directs the NMR spectrometer to collect the selected data set. ADAPT-NMR extracts peak positions from the newly collected data and uses this information in updating the analysis resonance assignments and secondary structure. The goal-directed objective function then defines the next data collection step. The procedure continues until the collected data support comprehensive peak identification, resonance assignments at the desired level of completeness, and protein secondary structure. We present test cases in which ADAPT-NMR achieved results in two days or less that would have taken two months or more by manual approaches. PMID:22427982

  18. NMR Hyperpolarization Techniques of Gases.

    PubMed

    Barskiy, Danila A; Coffey, Aaron M; Nikolaou, Panayiotis; Mikhaylov, Dmitry M; Goodson, Boyd M; Branca, Rosa T; Lu, George J; Shapiro, Mikhail G; Telkki, Ville-Veikko; Zhivonitko, Vladimir V; Koptyug, Igor V; Salnikov, Oleg G; Kovtunov, Kirill V; Bukhtiyarov, Valerii I; Rosen, Matthew S; Barlow, Michael J; Safavi, Shahideh; Hall, Ian P; Schröder, Leif; Chekmenev, Eduard Y

    2017-01-18

    Nuclear spin polarization can be significantly increased through the process of hyperpolarization, leading to an increase in the sensitivity of nuclear magnetic resonance (NMR) experiments by 4-8 orders of magnitude. Hyperpolarized gases, unlike liquids and solids, can often be readily separated and purified from the compounds used to mediate the hyperpolarization processes. These pure hyperpolarized gases enabled many novel MRI applications including the visualization of void spaces, imaging of lung function, and remote detection. Additionally, hyperpolarized gases can be dissolved in liquids and can be used as sensitive molecular probes and reporters. This Minireview covers the fundamentals of the preparation of hyperpolarized gases and focuses on selected applications of interest to biomedicine and materials science. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Applications of NMR spectroscopy to systems biochemistry.

    PubMed

    Fan, Teresa W-M; Lane, Andrew N

    2016-02-01

    The past decades of advancements in NMR have made it a very powerful tool for metabolic research. Despite its limitations in sensitivity relative to mass spectrometric techniques, NMR has a number of unparalleled advantages for metabolic studies, most notably the rigor and versatility in structure elucidation, isotope-filtered selection of molecules, and analysis of positional isotopomer distributions in complex mixtures afforded by multinuclear and multidimensional experiments. In addition, NMR has the capacity for spatially selective in vivo imaging and dynamical analysis of metabolism in tissues of living organisms. In conjunction with the use of stable isotope tracers, NMR is a method of choice for exploring the dynamics and compartmentation of metabolic pathways and networks, for which our current understanding is grossly insufficient. In this review, we describe how various direct and isotope-edited 1D and 2D NMR methods can be employed to profile metabolites and their isotopomer distributions by stable isotope-resolved metabolomic (SIRM) analysis. We also highlight the importance of sample preparation methods including rapid cryoquenching, efficient extraction, and chemoselective derivatization to facilitate robust and reproducible NMR-based metabolomic analysis. We further illustrate how NMR has been applied in vitro, ex vivo, or in vivo in various stable isotope tracer-based metabolic studies, to gain systematic and novel metabolic insights in different biological systems, including human subjects. The pathway and network knowledge generated from NMR- and MS-based tracing of isotopically enriched substrates will be invaluable for directing functional analysis of other 'omics data to achieve understanding of regulation of biochemical systems, as demonstrated in a case study. Future developments in NMR technologies and reagents to enhance both detection sensitivity and resolution should further empower NMR in systems biochemical research. Copyright © 2016

  20. A microcoil NMR probe for coupling microscale HPLC with on-line NMR spectroscopy.

    PubMed

    Subramanian, R; Kelley, W P; Floyd, P D; Tan, Z J; Webb, A G; Sweedler, J V

    1999-12-01

    An HPLC NMR system is presented that integrates a commercial microbore HPLC system using a 0.5-mm column with a 500-MHz proton NMR spectrometer using a custom NMR probe with an observe volume of 1.1 microL and a coil fill factor of 68%. Careful attention to capillary connections and NMR flow cell design allows on-line NMR detection with no significant loss in separation efficiency when compared with a UV chromatogram. HPLC NMR is performed on mixtures of amino acids and small peptides with analyte injection amounts as small as 750 ng; the separations are accomplished in less than 10 min and individual NMR spectra are acquired with 12 s time resolution. Stopped-flow NMR is achieved by diversion of the chromatographic flow after observation of the beginning of the analyte band within the NMR flow cell. Isolation of the compound of interest within the NMR detection cell allows multidimensional experiments to be performed. A stopped-flow COSY spectrum of the peptide Phe-Ala is acquired in 3.5 h with an injected amount of 5 micrograms.

  1. An introduction to biological NMR spectroscopy.

    PubMed

    Marion, Dominique

    2013-11-01

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

  2. An Introduction to Biological NMR Spectroscopy*

    PubMed Central

    Marion, Dominique

    2013-01-01

    NMR spectroscopy is a powerful tool for biologists interested in the structure, dynamics, and interactions of biological macromolecules. This review aims at presenting in an accessible manner the requirements and limitations of this technique. As an introduction, the history of NMR will highlight how the method evolved from physics to chemistry and finally to biology over several decades. We then introduce the NMR spectral parameters used in structural biology, namely the chemical shift, the J-coupling, nuclear Overhauser effects, and residual dipolar couplings. Resonance assignment, the required step for any further NMR study, bears a resemblance to jigsaw puzzle strategy. The NMR spectral parameters are then converted into angle and distances and used as input using restrained molecular dynamics to compute a bundle of structures. When interpreting a NMR-derived structure, the biologist has to judge its quality on the basis of the statistics provided. When the 3D structure is a priori known by other means, the molecular interaction with a partner can be mapped by NMR: information on the binding interface as well as on kinetic and thermodynamic constants can be gathered. NMR is suitable to monitor, over a wide range of frequencies, protein fluctuations that play a crucial role in their biological function. In the last section of this review, intrinsically disordered proteins, which have escaped the attention of classical structural biology, are discussed in the perspective of NMR, one of the rare available techniques able to describe structural ensembles. This Tutorial is part of the International Proteomics Tutorial Programme (IPTP 16 MCP). PMID:23831612

  3. Pressure-induced anomalous magnetism and unconventional superconductivity in CeRhIn{sub 5}: {sup 115}In-NQR study under pressure

    SciTech Connect

    Mito, T.; Kawasaki, S.; Zheng, G.-q.; Kawasaki, Y.; Ishida, K.; Kitaoka, Y.; Aoki, D.; Haga, Y.; Onuki, Y.

    2001-06-01

    We report {sup 115}In nuclear-quadrupole-resonance (NQR) measurements of the pressure (P)-induced superconductor CeRhIn{sub 5} in the antiferromagnetic (AF) and superconducting (SC) states. In the AF region, the internal field H{sub int} at the In site is substantially reduced from H{sub int}=1.75kOe at P=0 to 0.39 kOe at P=1.23GPa, while the Neel temperature slightly changes with increasing P. This suggests that either the size in the ordered moment M{sub Q}(P) or the angle {theta}(P) between the direction of M{sub Q}(P) and the tetragonal c axis is extrapolated to zero at P{sup *}=1.6{+-}0.1GPa at which a bulk SC transition is no longer emergent. In the SC state at P=2.1GPa, the nuclear spin-lattice relaxation rate {sup 115}(1/T{sub 1}) has revealed a T{sup 3} dependence without the coherence peak just below T{sub c}, giving evidence for the unconventional superconductivity. The dimensionality of the magnetic fluctuations in the normal state is also discussed.

  4. Towards ferromagnetic quantum criticality in FeGa3 -xGex :71Ga NQR as a zero-field microscopic probe

    NASA Astrophysics Data System (ADS)

    Majumder, M.; Wagner-Reetz, M.; Cardoso-Gil, R.; Gille, P.; Steglich, F.; Grin, Y.; Baenitz, M.

    2016-02-01

    71Ga NQR, magnetization, and specific-heat measurements have been performed on polycrystalline Ge-doped FeGa3 samples. A crossover from an insulator to a correlated local moment metal in the low-doping regime and the evolution of itinerant ferromagnet upon further doping is found. For the nearly critical concentration at the threshold of ferromagnetic order, xC=0.15, 71(1 /T1T ) exhibits a pronounced T-4 /3 power law over two orders of magnitude in temperature, which indicates three-dimensional quantum critical ferromagnetic fluctuations. Furthermore, for the ordered x =0.2 sample (TC≈6 K), 71(1 /T1T ) could be fitted well in the frame of Moriya's self-consistent renormalization theory for weakly ferromagnetic systems with 1 /T1T ˜χ . In contrast to this, the low-doping regime nicely displays local moment behavior where 1 /T1T ˜χ2 is valid. For T →0 , the Sommerfeld ratio γ =(C /T ) is enhanced (70 mJ /mole K2 for x =0.1 ) , which indicates the formation of heavy 3 d electrons.

  5. Azotobacter vinelandii lacking the Na(+)-NQR activity: a potential source for producing alginates with improved properties and at high yield.

    PubMed

    Gaytán, Itzel; Peña, Carlos; Núñez, Cinthia; Córdova, María S; Espín, Guadalupe; Galindo, Enrique

    2012-08-01

    The mutant ATCN4 strain of Azotobacter vinelandii, which lacks the Na(+)-NQR activity and results in an alginate overproduction (highly mucoid phenotype), was cultured in shake flasks in minimal and rich medium, and the chemical composition and rheological properties of the alginate were determined. Mutant ATCN4 exhibited a high efficiency for sucrose conversion to alginate and PHB accumulation, reaching yields that were 3.6- and 1.6-fold higher than those obtained from the wildtype cultures in minimal medium (Burk's sucrose, BS). The alginate produced by ATCN4 in the minimal medium had a high degree of acetylation (≥4 %) and a low G/M ratio (=2) with respect to the polymer synthesised in the rich medium (BS with yeast extract) (degree of acetylation = 0 % and G/M ratio of 4.5). The alginate produced in the minimal medium exhibited a pronounced pseudoplastic behaviour and a higher G* module in comparison to that observed in the alginate obtained in the cultures using a rich medium. The ATCN4 mutant culture in the minimal medium promoted the synthesis of a polymer of improved rheological quality in terms of its mechanical properties. These characteristics make this mutant a valuable source for producing alginates with improved or special properties.

  6. Scalar operators in solid-state NMR

    SciTech Connect

    Sun, Boqin

    1991-11-01

    Selectivity and resolution of solid-state NMR spectra are determined by dispersion of local magnetic fields originating from relaxation effects and orientation-dependent resonant frequencies of spin nuclei. Theoretically, the orientation-dependent resonant frequencies can be represented by a set of irreducible tensors. Among these tensors, only zero rank tensors (scalar operators) are capable of providing high resolution NMR spectra. This thesis presents a series of new developments in high resolution solid-state NMR concerning the reconstruction of various scalar operators motion in solid C{sub 60} is analyzed.

  7. An Inversion Recovery NMR Kinetics Experiment.

    PubMed

    Williams, Travis J; Kershaw, Allan D; Li, Vincent; Wu, Xinping

    2011-05-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this article will enable instructors to use inversion recovery as a laboratory activity in applied NMR classes and provide research students with a convenient template with which to acquire inversion recovery data on research samples.

  8. NMR reaction monitoring in flow synthesis

    PubMed Central

    Gomez, M Victoria

    2017-01-01

    Recent advances in the use of flow chemistry with in-line and on-line analysis by NMR are presented. The use of macro- and microreactors, coupled with standard and custom made NMR probes involving microcoils, incorporated into high resolution and benchtop NMR instruments is reviewed. Some recent selected applications have been collected, including synthetic applications, the determination of the kinetic and thermodynamic parameters and reaction optimization, even in single experiments and on the μL scale. Finally, software that allows automatic reaction monitoring and optimization is discussed. PMID:28326137

  9. An Inversion Recovery NMR Kinetics Experiment

    PubMed Central

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this article will enable instructors to use inversion recovery as a laboratory activity in applied NMR classes and provide research students with a convenient template with which to acquire inversion recovery data on research samples. PMID:21552343

  10. MAS-NMR at very high temperatures.

    PubMed

    van Wüllen, Leo; Schwering, Georg; Naumann, Ernst; Jansen, Martin

    2004-09-01

    We report MAS-NMR experiments at temperatures of approx. 1200 K using a CO(2) laser as the heating device. An internal NMR thermometer based on the (7)Li T1 data of Li(0.24)La(0.54)TiO(3) is used for temperature calibration. Using this setup, temperatures as high as 1191 K could be reached under MAS conditions as confirmed by the melting of Li(2)B(4)O(7) at 1191 K which could be followed by (7)Li-MAS-NMR.

  11. Probing porous media with gas diffusion NMR

    NASA Technical Reports Server (NTRS)

    Mair, R. W.; Wong, G. P.; Hoffmann, D.; Hurlimann, M. D.; Patz, S.; Schwartz, L. M.; Walsworth, R. L.

    1999-01-01

    We show that gas diffusion nuclear magnetic resonance (GD-NMR) provides a powerful technique for probing the structure of porous media. In random packs of glass beads, using both laser-polarized and thermally polarized xenon gas, we find that GD-NMR can accurately measure the pore space surface-area-to-volume ratio, S/V rho, and the tortuosity, alpha (the latter quantity being directly related to the system's transport properties). We also show that GD-NMR provides a good measure of the tortuosity of sandstone and complex carbonate rocks.

  12. MAS NMR of HIV-1 protein assemblies

    NASA Astrophysics Data System (ADS)

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

    2015-04-01

    The negative global impact of the AIDS pandemic is well known. In this perspective article, the utility of magic angle spinning (MAS) NMR spectroscopy to answer pressing questions related to the structure and dynamics of HIV-1 protein assemblies is examined. In recent years, MAS NMR has undergone major technological developments enabling studies of large viral assemblies. We discuss some of these evolving methods and technologies and provide a perspective on the current state of MAS NMR as applied to the investigations into structure and dynamics of HIV-1 assemblies of CA capsid protein and of Gag maturation intermediates.

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

    PubMed

    Jang, Richard; Wang, Yan; Xue, Zhidong; Zhang, Yang

    2015-08-01

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

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

    PubMed Central

    Jang, Richard; Wang, Yan

    2015-01-01

    NMR-I-TASSER, an adaption of the I-TASSER algorithm combining NMR data for protein structure determination, recently joined the second round of the CASD-NMR experiment. Unlike many molecular dynamics-based methods, NMR-I-TASSER takes a molecular replacement-like approach to the problem by first threading the target through the PDB to identify structural templates which are then used for iterative NOE assignments and fragment structure assembly refinements. The employment of multiple templates allows NMR-I-TASSER to sample different topologies while convergence to a single structure is not required. Retroactive and blind tests of the CASD-NMR targets from Rounds 1 and 2 demonstrate that even without using NOE peak lists I-TASSER can generate correct structure topology with 15 of 20 targets having a TM-score above 0.5. With the addition of NOE-based distance restraints, NMR-I-TASSER significantly improved the I-TASSER models with all models having the TM-score above 0.5. The average RMSD was reduced from 5.29 to 2.14 Å in Round 1 and 3.18 to 1.71 Å in Round 2. There is no obvious difference in the modeling results with using raw and refined peak lists, indicating robustness of the pipeline to the NOE assignment errors. Overall, despite the low-resolution modeling the current NMR-I-TASSER pipeline provides a coarse-grained structure folding approach complementary to traditional molecular dynamics simulations, which can produce fast near-native frameworks for atomic-level structural refinement. PMID:25737244

  15. A ferromagnetic shim insert for NMR magnets - Towards an integrated gyrotron for DNP-NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Ryan, Herbert; van Bentum, Jan; Maly, Thorsten

    2017-04-01

    In recent years high-field Dynamic Nuclear Polarization (DNP) enhanced NMR spectroscopy has gained significant interest. In high-field DNP-NMR experiments (⩾400 MHz 1H NMR, ⩾9.4 T) often a stand-alone gyrotron is used to generate high microwave/THz power to produce sufficiently high microwave induced B1e fields at the position of the NMR sample. These devices typically require a second, stand-alone superconducting magnet to operate. Here we present the design and realization of a ferroshim insert, to create two iso-centers inside a commercially available wide-bore NMR magnet. This work is part of a larger project to integrate a gyrotron into NMR magnets, effectively eliminating the need for a second, stand-alone superconducting magnet.

  16. A ferromagnetic shim insert for NMR magnets - Towards an integrated gyrotron for DNP-NMR spectroscopy.

    PubMed

    Ryan, Herbert; van Bentum, Jan; Maly, Thorsten

    2017-04-01

    In recent years high-field Dynamic Nuclear Polarization (DNP) enhanced NMR spectroscopy has gained significant interest. In high-field DNP-NMR experiments (⩾400MHz (1)H NMR, ⩾9.4T) often a stand-alone gyrotron is used to generate high microwave/THz power to produce sufficiently high microwave induced B1e fields at the position of the NMR sample. These devices typically require a second, stand-alone superconducting magnet to operate. Here we present the design and realization of a ferroshim insert, to create two iso-centers inside a commercially available wide-bore NMR magnet. This work is part of a larger project to integrate a gyrotron into NMR magnets, effectively eliminating the need for a second, stand-alone superconducting magnet. Copyright © 2017 Elsevier Inc. All rights reserved.

  17. NMR Analysis of Unknowns: An Introduction to 2D NMR Spectroscopy

    ERIC Educational Resources Information Center

    Alonso, David E.; Warren, Steven E.

    2005-01-01

    A study combined 1D (one-dimensional) and 2D (two-dimensional) NMR spectroscopy to solve structural organic problems of three unknowns, which include 2-, 3-, and 4-heptanone. Results showed [to the first power]H NMR and [to the thirteenth power]C NMR signal assignments for 2- and 3-heptanone were more challenging than for 4-heptanone owing to the…

  18. NMR Analysis of Unknowns: An Introduction to 2D NMR Spectroscopy

    ERIC Educational Resources Information Center

    Alonso, David E.; Warren, Steven E.

    2005-01-01

    A study combined 1D (one-dimensional) and 2D (two-dimensional) NMR spectroscopy to solve structural organic problems of three unknowns, which include 2-, 3-, and 4-heptanone. Results showed [to the first power]H NMR and [to the thirteenth power]C NMR signal assignments for 2- and 3-heptanone were more challenging than for 4-heptanone owing to the…

  19. NMR Methods to Study Dynamic Allostery.

    PubMed

    Grutsch, Sarina; Brüschweiler, Sven; Tollinger, Martin

    2016-03-01

    Nuclear magnetic resonance (NMR) spectroscopy provides a unique toolbox of experimental probes for studying dynamic processes on a wide range of timescales, ranging from picoseconds to milliseconds and beyond. Along with NMR hardware developments, recent methodological advancements have enabled the characterization of allosteric proteins at unprecedented detail, revealing intriguing aspects of allosteric mechanisms and increasing the proportion of the conformational ensemble that can be observed by experiment. Here, we present an overview of NMR spectroscopic methods for characterizing equilibrium fluctuations in free and bound states of allosteric proteins that have been most influential in the field. By combining NMR experimental approaches with molecular simulations, atomistic-level descriptions of the mechanisms by which allosteric phenomena take place are now within reach.

  20. Interfaces in polymer nanocomposites - An NMR study

    NASA Astrophysics Data System (ADS)

    Böhme, Ute; Scheler, Ulrich

    2016-03-01

    Nuclear Magnetic Resonance (NMR) is applied for the investigation of polymer nanocomposites. Solid-state NMR is applied to study the modification steps to compatibilize layered double hydroxides with non-polar polymers. 1H relaxation NMR gives insight on the polymer dynamics over a wide range of correlation times. For the polymer chain dynamics the transverse relaxation time T2 is most suited. In this presentation we report on two applications of T2 measurements under external mechanical stress. In a low-field system relaxation NMR studies are performed in-situ under uniaxial stress. High-temperature experiments in a Couette cell permit the investigation of the polymer dynamics in the melt under shear flow.

  1. NMR-Assisted Molecular Docking Methodologies.

    PubMed

    Sturlese, Mattia; Bellanda, Massimo; Moro, Stefano

    2015-08-01

    Nuclear magnetic resonance (NMR) spectroscopy and molecular docking are regularly being employed as helpful tools of drug discovery research. Molecular docking is an extremely rapid method to evaluate possible binders from a large chemical library in a fast and cheap manner. NMR techniques can directly detect a protein-ligand interaction, can determine the corresponding association constant, and can consistently identify the ligand binding cavity. Consequently, molecular docking and NMR techniques are naturally complementary techniques where the combination of the two has the potential to improve the overall efficiency of drug discovery process. In this review, we would like to summarize the state of the art of docking methods which have been recently bridged to NMR experiments to identify novel and effective therapeutic drug candidates.

  2. Relaxation time estimation in surface NMR

    DOEpatents

    Grunewald, Elliot D.; Walsh, David O.

    2017-03-21

    NMR relaxation time estimation methods and corresponding apparatus generate two or more alternating current transmit pulses with arbitrary amplitudes, time delays, and relative phases; apply a surface NMR acquisition scheme in which initial preparatory pulses, the properties of which may be fixed across a set of multiple acquisition sequence, are transmitted at the start of each acquisition sequence and are followed by one or more depth sensitive pulses, the pulse moments of which are varied across the set of multiple acquisition sequences; and apply processing techniques in which recorded NMR response data are used to estimate NMR properties and the relaxation times T.sub.1 and T.sub.2* as a function of position as well as one-dimensional and two-dimension distributions of T.sub.1 versus T.sub.2* as a function of subsurface position.

  3. A New Microcell Technique for NMR Analysis.

    ERIC Educational Resources Information Center

    Yu, Sophia J.

    1987-01-01

    Describes a new laboratory technique for working with small samples of compounds used in nuclear magnetic resonance (NMR) analysis. Demonstrates how microcells can be constructed for each experiment and samples can be recycled. (TW)

  4. A New Microcell Technique for NMR Analysis.

    ERIC Educational Resources Information Center

    Yu, Sophia J.

    1987-01-01

    Describes a new laboratory technique for working with small samples of compounds used in nuclear magnetic resonance (NMR) analysis. Demonstrates how microcells can be constructed for each experiment and samples can be recycled. (TW)

  5. NMR analysis of compositional heterogeneity in polysaccharides

    USDA-ARS?s Scientific Manuscript database

    Many copolysaccharides are compositionally heterogeneous, and the composition determined by the usual analytical or spectroscopic methods provides only an average value. For some polysaccharides, the NMR data contain copolymer sequence information, such as diad, triad, and tetrad sequence intensiti...

  6. NMR Methods to Study Dynamic Allostery

    PubMed Central

    Grutsch, Sarina; Brüschweiler, Sven; Tollinger, Martin

    2016-01-01

    Nuclear magnetic resonance (NMR) spectroscopy provides a unique toolbox of experimental probes for studying dynamic processes on a wide range of timescales, ranging from picoseconds to milliseconds and beyond. Along with NMR hardware developments, recent methodological advancements have enabled the characterization of allosteric proteins at unprecedented detail, revealing intriguing aspects of allosteric mechanisms and increasing the proportion of the conformational ensemble that can be observed by experiment. Here, we present an overview of NMR spectroscopic methods for characterizing equilibrium fluctuations in free and bound states of allosteric proteins that have been most influential in the field. By combining NMR experimental approaches with molecular simulations, atomistic-level descriptions of the mechanisms by which allosteric phenomena take place are now within reach. PMID:26964042

  7. NMR Experiment Factors Numbers with Gauss Sums

    NASA Astrophysics Data System (ADS)

    Mehring, Michael; Müller, Klaus; Averbukh, Ilya Sh.; Merkel, Wolfgang; Schleich, Wolfgang P.

    2007-03-01

    We factor the number 157573 using an NMR implementation of Gauss sums. Although the current implementation is classical and scales exponentially, we believe that an extension to the quantum regime using entangled states is possible.

  8. WHNMR--a universal NMR application package.

    PubMed

    Xiaodong, Z; Hongbin, H; Nian, H; Lianfang, S; Chaohui, Y

    1996-06-01

    A PC-based NMR off-line data processing system is developed and described in detail. With this software system, one-dimensional (1D), two-dimensional (2D), and NMR imaging (MRI) data can be processed easily, and give reliable results. By the applications of this system, a versatile software interface is set up to achieve data exchanging and integrated usage with other PC application software and aids the PC to become an effective and powerful workstation.

  9. Modern NMR spectroscopy: a guide for chemists

    SciTech Connect

    Sanders, J.K.M.; Hunter, B.K.

    1988-01-01

    The aim of the authors of Modern NMR Spectroscopy is to bridge the communication gap between the chemist and the spectroscopist. The approach is nonmathematical, descriptive, and pictorial. To illustrate the ideas introduced in the text, the authors provide original spectra obtained specially for this purpose. Examples include spectroscopy of protons, carbon, and less receptive nuclei of interest to inorganic chemists. The authors succeed in making high-resolution NMR spectroscopy comprehensible for the average student or chemist.

  10. NMR studies of multiphase flows II

    SciTech Connect

    Altobelli, S.A.; Caprihan, A.; Fukushima, E.

    1995-12-31

    NMR techniques for measurements of spatial distribution of material phase, velocity and velocity fluctuation are being developed and refined. Versions of these techniques which provide time average liquid fraction and fluid phase velocity have been applied to several concentrated suspension systems which will not be discussed extensively here. Technical developments required to further extend the use of NMR to the multi-phase flow arena and to provide measurements of previously unobtainable parameters are the focus of this report.

  11. Frontiers of NMR in Molecular Biology

    SciTech Connect

    1999-08-25

    NMR spectroscopy is expanding the horizons of structural biology by determining the structures and describing the dynamics of blobular proteins in aqueous solution, as well as other classes of proteins including membrane proteins and the polypeptides that form the aggregates diagnostic of prion and amyloid diseases. Significant results are also emerging on DNA and RNA oligomers and their complexes with proteins. This meeting focused attention on key structural questions emanating from molecular biology and how NMR spectroscopy can be used to answer them.

  12. Conformations and intermolecular interactions pattern in solid chloroxylenol and triclosan (API of anti-infective agents and drugs). A (35)Cl NQR, (1)H-(14)N NQDR, X-ray and DFT/QTAIM study.

    PubMed

    Latosińska, J N; Latosińska, M; Tomczak, M A; Seliger, J; Zagar, V; Maurin, J K

    2012-02-01

    Two antibacterial and antifungal agents, chloroxylenol (4-chloro-3,5-dimethyl-phenol) and triclosan (5-chloro-2-(2',4'-dichlorophenoxy)-phenol), were studied experimentally in solid state with an X-ray, (35)Cl-nuclear quadrupole resonance (NQR) and (17)O-nuclear quadrupole double resonance (NQDR) spectroscopies and, theoretically, with the density functional theory/quantum theory of atoms in molecules (DFT/QTAIM). The crystallographic structure of triclosan, which crystallises in space group P31 with one molecule in the asymmetric unit [a = 12.64100(10), b = 12.64100(10), c = 6.71630(10) Å], was solved with an X-ray and refined to a final R-factor of 2.81% at room temperature. The NQR frequencies of (35)Cl and (17)O were detected with the help of the density functional theory (DFT) assigned to particular chlorine and oxygen sites in the molecules of both compounds. The NQR frequencies at (35)Cl sites in chloroxylenol and triclosan were found to be more differentiated than frequencies at the (17)O site. The former better describes the substituent withdrawing effects connected to π-electron delocalization within the benzene rings and the influence of temperature; whereas, those at the (17)O site provide more information on O-H bond and intermolecular interactions pattern. The conformation adopted by diphenyl ether of triclosan in solid state was found to be typical of diphenyl ethers, but the opposite to those adopted when it was bound to different inhibitors. According to an X-ray study, temperature had no effect on the conformation of the diphenyl ring of triclosan, which was the same at 90 K and at room temperature (RT). The scattering of NQR frequencies reproduced by the DFT under assumption of the X-ray data at 90 K and RT is found to be a good indicator of the quality of resolution of the crystallographic structure.

  13. {sup 63,65}Cu NQR study of Ba-site occupation in Y{sub 1{minus}x}Pr{sub x}Ba{sub 2}Cu{sub 3}O{sub 7{minus}{delta}}

    SciTech Connect

    Abdelrazek, M.M.; Reyes, A.P.; Kuhns, P.L.; Moulton, W.G.

    1999-12-20

    The authors report measurements of {sup 63,65}Cu nuclear quadrupole resonance (NQR) at ambient temperatures to indirectly probe Ba-site occupation of Pr atoms in doped Y{sub 1{minus}x}Pr{sub x}Ba{sub 2}Cu{sub 3}O{sub 7{minus}{delta}} (0 {le} x {le} 1.0). Preliminary results show anomalous peaks in the spectra attributed to the O(5) atoms as would be expected in the presence of a Pr atom on the adjacent Ba-O plane.

  14. Sparse Sampling Methods In Multidimensional NMR

    PubMed Central

    Mobli, Mehdi; Maciejewski, Mark W.; Schuyler, Adam D.; Stern, Alan S.; Hoch, Jeffrey C.

    2014-01-01

    Although the discrete Fourier transform played an enabling role in the development of modern NMR spectroscopy, it suffers from a well-known difficulty providing high-resolution spectra from short data records. In multidimensional NMR experiments, so-called indirect time dimensions are sampled parametrically, with each instance of evolution times along the indirect dimensions sampled via separate one-dimensional experiments. The time required to conduct multidimensional experiments is directly proportional to the number of indirect evolution times sampled. Despite remarkable advances in resolution with increasing magnetic field strength, multiple dimensions remain essential for resolving individual resonances in NMR spectra of biological macromolecues. Conventional Fourier-based methods of spectrum analysis limit the resolution that can be practically achieved in the indirect dimensions. Nonuniform or sparse data collection strategies, together with suitable non-Fourier methods of spectrum analysis, enable high-resolution multidimensional spectra to be obtained. Although some of these approaches were first employed in NMR more than two decades ago, it is only relatively recently that they have been widely adopted. Here we describe the current practice of sparse sampling methods and prospects for further development of the approach to improve resolution and sensitivity and shorten experiment time in multidimensional NMR. While sparse sampling is particularly promising for multidimensional NMR, the basic principles could apply to other forms of multidimensional spectroscopy. PMID:22481242

  15. Double resonance experiments in low magnetic field: dynamic polarization of protons by (14)N and measurement of low NQR frequencies.

    PubMed

    Seliger, J; Zagar, V

    2009-08-01

    The possibilities of dynamically polarizing proton spin system via the quadrupole (14)N spin system in low magnetic field are analyzed. The increase of the proton magnetization is calculated. The polarization rate of the proton spin system is related to the transition probabilities per unit time between the (14)N quadrupole energy levels and proton energy levels. The experiments performed in 1,3,5-triazine confirm the results of the theoretical analysis. A new double resonance technique is proposed for the measurement of nuclear quadrupole resonance frequencies nu(Q) of the order of 100kHz and lower. The technique is based on magnetic field cycling between a high and a low static magnetic field and observation of the proton NMR signal in the high magnetic field. In the low magnetic field the quadrupole nuclei and protons resonantly interact at the proton Larmor frequency nu(H)=nu(Q)/2. The quadrupole nuclei are simultaneously excited by a resonant rf magnetic field oriented along the direction of the low static magnetic field. The experimental procedure is described and the sensitivity of the new technique is estimated. Some examples of the measurement of low (14)N and (2)H nuclear quadrupole resonance frequencies are presented.

  16. Microflow NMR: concepts and capabilities.

    PubMed

    Olson, Dean L; Norcross, James A; O'Neil-Johnson, Mark; Molitor, Paul F; Detlefsen, David J; Wilson, Aaron G; Peck, Timothy L

    2004-05-15

    The principles and parameters to consider when choosing an NMR probe for analysis of a volume- or mass-limited sample are identified and discussed. In particular, a capillary-based microflow probe is described which has a mass sensitivity comparable to cryoprobes (observe volume approximately 40 microL), but with several distinct advantages. The microflow probe has a flowcell volume of 5 microL and an observe volume of 1.5 microL and is equipped with proton and carbon observe channels, deuterium lock, and z-gradient capability. The entire flow path is fused silica; inlet and outlet capillary inner diameters are 50 microm to minimize sample dispersion, making it well-suited to volume-limited samples. An injected sample of 1 nmol of sucrose (0.34 microg in 3 microL, 0.33 mM; MW = 342 g/mol) yields a 1D proton spectrum in 10 min on a spectrometer of 500 MHz or higher. In another example, 15 microg of sucrose (in 3 microL; 15 mM, 45 nmol) is injected and parked in the probe to yield a heteronuclear multiple-quantum coherence (HMQC) spectrum in less than 15 h. The natural product muristerone A (75 microg in 3 microL, 50 mM, 150 nmol; MW = 497 g/mol) was delivered to the flow cell, and a gradient correlation spectroscopy spectrum was acquired in 7 min, a gradient HMQC in 4 h, and a gradient heteronuclear multiple-bond correlation in 11 h. Four basic modes of sample injection into the probe vary in degree of user intervention, speed, solvent consumption, and sample delivery efficiency. Manual, manual-assisted (employing a micropump), automated (using an autosampler), and capillary HPLC modes of operation are described.

  17. Hypothesis driven assessment of an NMR curriculum

    NASA Astrophysics Data System (ADS)

    Cossey, Kimberly

    The goal of this project was to develop a battery of assessments to evaluate an undergraduate NMR curriculum at Penn State University. As a chemical education project, we sought to approach the problem of curriculum assessment from a scientific perspective, while remaining grounded in the education research literature and practices. We chose the phrase hypothesis driven assessment to convey this process of relating the scientific method to the study of educational methods, modules, and curricula. We began from a hypothesis, that deeper understanding of one particular analytical technique (NMR) will increase undergraduate students' abilities to solve chemical problems. We designed an experiment to investigate this hypothesis, and data collected were analyzed and interpreted in light of the hypothesis and several related research questions. The expansion of the NMR curriculum at Penn State was funded through the NSF's Course, Curriculum, and Laboratory Improvement (CCLI) program, and assessment was required. The goal of this project, as stated in the grant proposal, was to provide NMR content in greater depth by integrating NMR modules throughout the curriculum in physical chemistry, instrumental, and organic chemistry laboratory courses. Hands-on contact with the NMR spectrometer and NMR data and repeated exposure of the analytical technique within different contexts (courses) were unique factors of this curriculum. Therefore, we maintained a focus on these aspects throughout the evaluation process. The most challenging and time-consuming aspect of any assessment is the development of testing instruments and methods to provide useful data. After key variables were defined, testing instruments were designed to measure these variables based on educational literature (Chapter 2). The primary variables measured in this assessment were: depth of understanding of NMR, basic NMR knowledge, problem solving skills (HETCOR problem), confidence for skills used in class (within

  18. 33S NMR cryogenic probe for taurine detection

    NASA Astrophysics Data System (ADS)

    Hobo, Fumio; Takahashi, Masato; Maeda, Hideaki

    2009-03-01

    With the goal of a S33 nuclear magnetic resonance (NMR) probe applicable to in vivo NMR on taurine-biological samples, we have developed the S33 NMR cryogenic probe, which is applicable to taurine solutions. The NMR sensitivity gain relative to a conventional broadband probe is as large as 3.5. This work suggests that improvements in the preamplifier could allow NMR measurements on 100 μM taurine solutions, which is the level of sensitivity necessary for biological samples.

  19. NMR Spectra through the Eyes of a Student: Eye Tracking Applied to NMR Items

    ERIC Educational Resources Information Center

    Topczewski, Joseph J.; Topczewski, Anna M.; Tang, Hui; Kendhammer, Lisa K.; Pienta, Norbert J.

    2017-01-01

    Nuclear magnetic resonance spectroscopy (NMR) plays a key role in introductory organic chemistry, spanning theory, concepts, and experimentation. Therefore, it is imperative that the instruction methods for NMR are both efficient and effective. By utilizing eye tracking equipment, the researchers were able to monitor how second-semester organic…

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

    PubMed

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

    2015-08-01

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

  1. Comparing NMR and X-ray protein structure: Lindemann-like parameters and NMR disorder.

    PubMed

    Faraggi, Eshel; Dunker, A Keith; Sussman, Joel L; Kloczkowski, Andrzej

    2017-08-08

    Disordered protein chains and segments are fast becoming a major pathway for our understanding of biological function, especially in more evolved species. However, the standard definition of disordered residues: the inability to constrain them in X-ray derived structures, is not easily applied to NMR derived structures. We carry out a statistical comparison between proteins whose structure was resolved using NMR and using X-ray protocols. We start by establishing a connection between these two protocols for obtaining protein structure. We find a close statistical correspondence between NMR and X-ray structures if fluctuations inherent to the NMR protocol are taken into account. Intuitively this tends to lend support to the validity of both NMR and X-ray protocols in deriving biomolecular models that correspond to in vivo conditions. We then establish Lindemann-like parameters for NMR derived structures and examine what order/disorder cutoffs for these parameters are most consistent with X-ray data and how consistent are they. Finally, we find critical value of [Formula: see text] for the best correspondence between X-ray and NMR derived order/disorder assignment, judged by maximizing the Matthews correlation, and a critical value [Formula: see text] if a balance between false positive and false negative prediction is sought. We examine a few non-conforming cases, and examine the origin of the structure derived in X-ray. This study could help in assigning meaningful disorder from NMR experiments.

  2. Temperature imaging by 1H NMR and suppression of convection in NMR probes

    PubMed

    Hedin; Furo

    1998-03-01

    A simple arrangement for suppressing convection in NMR probes is tested experimentally. Diffusion experiments are used to determine the onset of convection and 1H temperature imaging helps to rationalize the somewhat surprising results. A convenient new 1H NMR thermometer, CH2Br2 dissolved in a nematic thermotropic liquid crystal, is presented. Copyright 1998 Academic Press.

  3. NMR Spectra through the Eyes of a Student: Eye Tracking Applied to NMR Items

    ERIC Educational Resources Information Center

    Topczewski, Joseph J.; Topczewski, Anna M.; Tang, Hui; Kendhammer, Lisa K.; Pienta, Norbert J.

    2017-01-01

    Nuclear magnetic resonance spectroscopy (NMR) plays a key role in introductory organic chemistry, spanning theory, concepts, and experimentation. Therefore, it is imperative that the instruction methods for NMR are both efficient and effective. By utilizing eye tracking equipment, the researchers were able to monitor how second-semester organic…

  4. Use of NMR and NMR Prediction Software to Identify Components in Red Bull Energy Drinks

    ERIC Educational Resources Information Center

    Simpson, Andre J.; Shirzadi, Azadeh; Burrow, Timothy E.; Dicks, Andrew P.; Lefebvre, Brent; Corrin, Tricia

    2009-01-01

    A laboratory experiment designed as part of an upper-level undergraduate analytical chemistry course is described. Students investigate two popular soft drinks (Red Bull Energy Drink and sugar-free Red Bull Energy Drink) by NMR spectroscopy. With assistance of modern NMR prediction software they identify and quantify major components in each…

  5. Use of NMR and NMR Prediction Software to Identify Components in Red Bull Energy Drinks

    ERIC Educational Resources Information Center

    Simpson, Andre J.; Shirzadi, Azadeh; Burrow, Timothy E.; Dicks, Andrew P.; Lefebvre, Brent; Corrin, Tricia

    2009-01-01

    A laboratory experiment designed as part of an upper-level undergraduate analytical chemistry course is described. Students investigate two popular soft drinks (Red Bull Energy Drink and sugar-free Red Bull Energy Drink) by NMR spectroscopy. With assistance of modern NMR prediction software they identify and quantify major components in each…

  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. Characterization of heroin samples by 1H NMR and 2D DOSY 1H NMR.

    PubMed

    Balayssac, Stéphane; Retailleau, Emmanuel; Bertrand, Geneviève; Escot, Marie-Pierre; Martino, Robert; Malet-Martino, Myriam; Gilard, Véronique

    2014-01-01

    Twenty-four samples of heroin from different illicit drug seizures were analyzed using proton Nuclear Magnetic Resonance ((1)H NMR) and two-dimensional diffusion-ordered spectroscopy (2D DOSY) (1)H NMR. A careful assignment and quantification of (1)H signals enabled a comprehensive characterization of the substances present in the samples investigated: heroin, its main related impurities (6-acetylmorphine, acetylcodeine, morphine, noscapine and papaverine) and cutting agents (caffeine and acetaminophen in nearly all samples as well as lactose, lidocaine, mannitol, piracetam in one sample only), and hence to establish their spectral signatures. The good agreement between the amounts of heroin, noscapine, caffeine and acetaminophen determined by (1)H NMR and gas chromatography, the reference method in forensic laboratories, demonstrates the validity of the (1)H NMR technique. In this paper, 2D DOSY (1)H NMR offers a new approach for a whole characterization of the various components of these complex mixtures.

  8. Calibration of NMR well logs from carbonate reservoirs with laboratory NMR measurements and μXRCT

    SciTech Connect

    Mason, Harris E.; Smith, Megan M.; Hao, Yue; Carroll, Susan A.

    2014-12-31

    The use of nuclear magnetic resonance (NMR) well log data has the potential to provide in-situ porosity, pore size distributions, and permeability of target carbonate CO₂ storage reservoirs. However, these methods which have been successfully applied to sandstones have yet to be completely validated for carbonate reservoirs. Here, we have taken an approach to validate NMR measurements of carbonate rock cores with independent measurements of permeability and pore surface area to volume (S/V) distributions using differential pressure measurements and micro X-ray computed tomography (μXRCT) imaging methods, respectively. We observe that using standard methods for determining permeability from NMR data incorrectly predicts these values by orders of magnitude. However, we do observe promise that NMR measurements provide reasonable estimates of pore S/V distributions, and with further independent measurements of the carbonate rock properties that universally applicable relationships between NMR measured properties may be developed for in-situ well logging applications of carbonate reservoirs.

  9. BOOK REVIEW: NMR Imaging of Materials

    NASA Astrophysics Data System (ADS)

    Blümich, Bernhard

    2003-09-01

    Magnetic resonance imaging (MRI) of materials is a field of increasing importance. Applications extend from fundamental science like the characterization of fluid transport in porous rock, catalyst pellets and hemodialysers into various fields of engineering for process optimization and product quality control. While the results of MRI imaging are being appreciated by a growing community, the methods of imaging are far more diverse for materials applications than for medical imaging of human beings. Blümich has delivered the first book in this field. It was published in hardback three years ago and is now offered as a paperback for nearly half the price. The text provides an introduction to MRI imaging of materials covering solid-state NMR spectroscopy, imaging methods for liquid and solid samples, and unusual MRI in terms of specialized approaches to spatial resolution such as an MRI surface scanner. The book represents an excellent and thorough treatment which will help to grow research in materials MRI. Blümich developed the treatise over many years for his research students, graduates in chemistry, physics and engineering. But it may also be useful for medical students looking for a less formal discussion of solid-state NMR spectroscopy. The structure of this book is easy to perceive. The first three chapters cover an introduction, the fundamentals and methods of solid-state NMR spectroscopy. The book starts at the ground level where no previous knowledge about NMR is assumed. Chapter 4 discusses a wide variety of transformations beyond the Fourier transformation. In particular, the Hadamard transformation and the 'wavelet' transformation are missing from most related books. This chapter also includes a description of noise-correlation spectroscopy, which promises the imaging of large objects without the need for extremely powerful radio-frequency transmitters. Chapters 5 and 6 cover basic imaging methods. The following chapter about the use of relaxation and

  10. SedNMR: on the edge between solution and solid-state NMR.

    PubMed

    Bertini, Ivano; Luchinat, Claudio; Parigi, Giacomo; Ravera, Enrico

    2013-09-17

    Solid-state NMR (SS-NMR) of proteins requires that those molecules be immobilized, usually by crystallization, freezing, or lyophilization. However, self-crowding can also slow molecular rotation sufficiently to prevent the nuclear interactions from averaging. To achieve self-crowding, researchers can use a centrifugal field to create a concentration gradient or use regular ultracentrifugation to produce highly concentrated, gel-like solutions. Thus sedimented solute NMR (SedNMR) provides a simple method to prepare biological samples for SS-NMR experiments with minimal perturbation. This method may also give researchers a way to investigate species that are not otherwise accessible by NMR. We induce the sedimentation in one of two ways: (1) by the extreme centrifugal force exerted during magic angle spinning (MAS-induced sedimentation or in situ) or (2) by an ultracentrifuge (UC-induced sedimentation or ex situ). Sedimentation is particularly useful in situations where it is difficult to obtain protein crystals. Furthermore, because the proteins remain in a largely hydrated state, the sedimented samples may provide SS-NMR spectra that have better resolution than the spectra from frozen solutions or lyophilized powders. If sedimentation is induced in situ, the same protein sample can be used for both solution and SS-NMR studies. Finally, we show that in situ SedNMR can be used to detect the NMR signals of large molecular adducts that have binding constants that are too weak to allow for the selective isolation and crystallization of the complexed species. We can selectively induce sedimentation for the heaviest molecular species. Because the complexed molecules are subtracted from the bulk solution, the reaction proceeds further toward the formation of complexes.

  11. NMR studies of cation transport across membranes

    SciTech Connect

    Shochet, N.R.

    1985-01-01

    /sup 23/Na NMR Studies of cation transport across membranes were conducted both on model and biological membranes. Two ionophores, the carrier monensin and the channel-former gramicidin, were chosen to induce cation transport in large unilamellar phosphatidylcholine vesicles. The distinction between the NMR signals arising from the two sides of the membrane was achieved by the addition of an anionic paramagnetic shift reagent to the outer solution. The kinetics of the cation transport across the membrane was observed simultaneously monitoring the changes in the /sup 23/Na NMR signals of both compartments. Two mathematical models were developed for the estimation of the transport parameters of the monensin- and gramicidin-induced cation transport. The models were able to fit the experimental data very well. A new method for the estimation of the volume trapped inside the vesicles was developed. The method uses the relative areas of the intra- and extravesicular NMR signals arising from a suspension of vesicles bathed in the same medium they contain, as a measure for the relative volumes of these compartments. Sodium transport across biological membranes was studied by /sup 23/ NMR, using suspensions of cultured nerve cells. The sodium influx through voltage-gated channels was studied using the channel modifier batrachotoxin in combination with scorpion toxin.

  12. NMR methodologies in the analysis of blueberries.

    PubMed

    Capitani, Donatella; Sobolev, Anatoly P; Delfini, Maurizio; Vista, Silvia; Antiochia, Riccarda; Proietti, Noemi; Bubici, Salvatore; Ferrante, Gianni; Carradori, Simone; De Salvador, Flavio Roberto; Mannina, Luisa

    2014-06-01

    An NMR analytical protocol based on complementary high and low field measurements is proposed for blueberry characterization. Untargeted NMR metabolite profiling of blueberries aqueous and organic extracts as well as targeted NMR analysis focused on anthocyanins and other phenols are reported. Bligh-Dyer and microwave-assisted extractions were carried out and compared showing a better recovery of lipidic fraction in the case of microwave procedure. Water-soluble metabolites belonging to different classes such as sugars, amino acids, organic acids, and phenolic compounds, as well as metabolites soluble in organic solvent such as triglycerides, sterols, and fatty acids, were identified. Five anthocyanins (malvidin-3-glucoside, malvidin-3-galactoside, delphinidin-3-glucoside, delphinidin-3-galactoside, and petunidin-3-glucoside) and 3-O-α-l-rhamnopyranosyl quercetin were identified in solid phase extract. The water status of fresh and withered blueberries was monitored by portable NMR and fast-field cycling NMR. (1) H depth profiles, T2 transverse relaxation times and dispersion profiles were found to be sensitive to the withering.

  13. Radiation damping in microcoil NMR probes

    NASA Astrophysics Data System (ADS)

    Krishnan, V. V.

    2006-04-01

    Radiation damping arises from the field induced in the receiver coil by large bulk magnetization and tends to selectively drive this magnetization back to equilibrium much faster than relaxation processes. The demand for increased sensitivity in mass-limited samples has led to the development of microcoil NMR probes that are capable of obtaining high quality NMR spectra with small sample volumes (nL-μL). Microcoil probes are optimized to increase sensitivity by increasing either the sample-to-coil ratio (filling factor) of the probe or quality factor of the detection coil. Though radiation damping effects have been studied in standard NMR probes, these effects have not been measured in the microcoil probes. Here a systematic evaluation of radiation damping effects in a microcoil NMR probe is presented and the results are compared with similar measurements in conventional large volume samples. These results show that radiation-damping effects in microcoil probe is much more pronounced than in 5 mm probes, and that it is critically important to optimize NMR experiments to minimize these effects. As microcoil probes provide better control of the bulk magnetization, with good RF and B0 inhomogeneity, in addition to negligible dipolar field effects due to nearly spherical sample volumes, these probes can be used exclusively to study the complex behavior of radiation damping.

  14. Radiation damping in microcoil NMR probes.

    PubMed

    Krishnan, V V

    2006-04-01

    Radiation damping arises from the field induced in the receiver coil by large bulk magnetization and tends to selectively drive this magnetization back to equilibrium much faster than relaxation processes. The demand for increased sensitivity in mass-limited samples has led to the development of microcoil NMR probes that are capable of obtaining high quality NMR spectra with small sample volumes (nL-microL). Microcoil probes are optimized to increase sensitivity by increasing either the sample-to-coil ratio (filling factor) of the probe or quality factor of the detection coil. Though radiation damping effects have been studied in standard NMR probes, these effects have not been measured in the microcoil probes. Here a systematic evaluation of radiation damping effects in a microcoil NMR probe is presented and the results are compared with similar measurements in conventional large volume samples. These results show that radiation-damping effects in microcoil probe is much more pronounced than in 5 mm probes, and that it is critically important to optimize NMR experiments to minimize these effects. As microcoil probes provide better control of the bulk magnetization, with good RF and B0 inhomogeneity, in addition to negligible dipolar field effects due to nearly spherical sample volumes, these probes can be used exclusively to study the complex behavior of radiation damping.

  15. NMR structural studies on antifreeze proteins.

    PubMed

    Sönnichsen, F D; Davies, P L; Sykes, B D

    1998-01-01

    Antifreeze proteins (AFPs) are a structurally diverse class of proteins that bind to ice and inhibit its growth in a noncolligative manner. This adsorption-inhibition mechanism operating at the ice surface results in a lowering of the (nonequilibrium) freezing point below the melting point. A lowering of approximately 1 degree C, which is sufficient to prevent fish from freezing in ice-laden seawater, requires millimolar AFP levels in the blood. The solubility of AFPs at these millimolar concentrations and the small size of the AFPs (typically 3-15 kDa) make them ideal subjects for NMR analysis. Although fish AFPs are naturally abundant, seasonal expression, restricted access to polar fishes, and difficulties in separating numerous similar isoforms have made protein expression the method of choice for producing AFPs for structural studies. Expression of recombinant AFPs has also facilitated NMR analysis by permitting isotopic labeling with 15N and 13C and has permitted mutations to be made to help with the interpretation of NMR data. NMR analysis has recently solved two AFP structures and provided valuable information about the disposition of ice-binding side chains in a third. The potential exists to solve other AFP structures, including the newly described insect AFPs, and to use solid-state NMR techniques to address fundamental questions about the nature of the interaction between AFPs and ice.

  16. Applications of NMR to biological systems

    SciTech Connect

    Baatz, J.E.

    1988-01-01

    This work describes the application of nuclear magnetic resonance spectrometry (NMR) for the study of three biological systems, namely, the pulmonary surfactant-associated protein, SPL(pVal), the myocardial calcium slow channel of the perfused guinea pig heart, and the intracellular buffering system of the Leishmania donovani promastigote. Investigations of structural features of bovine SPL(pVal) were performed using one and two-dimensional {sup 1}H-NMR techniques. Delayed Fourier transform {sup 1}H-NMR has been used to study the effects of bovine SPL(pVal) and temperature upon model membrane structure. A model describing the mechanism by which the SPL(pVal) lowers the membrane surface tension has been proposed. In order to study the dependence of the myocardial calcium slow channel activity on adenosine triphosphate levels and intracellular pH, and in vivo {sup 31}P-NMR probe capable of simultaneously and noninvasively monitoring these three parameters was designed. In vivo {sup 31}P-NMR was also applied for the study of the Leishmania donovani promastigote's ability to maintain a pH gradient across its cellular membrane at low extracellular pH.

  17. Magic angle spinning NMR of paramagnetic proteins.

    PubMed

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

    2013-09-17

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

  18. Neutron diffraction and NQR study of the intermediate turn angle phase formed during AFI to AFII reordering in YBa{sub 2}Cu{sub 3{minus}x}Al{sub x}O{sub 6+{delta}}

    SciTech Connect

    Brecht, E.; Schmahl, W.W.; Fuess, H.; Schmenn, S.; Luetgemeier, H.; Andersen, N.H.; Lebech, B.

    1997-07-01

    The reordering mechanism from the antiferromagnetic phase AFI to the antiferromagnetic phase AFII in an oxygen-deficient YBa{sub 2}Cu{sub 2.94}Al{sub 0.06}O{sub 6+{delta}} single crystal with an oxygen content {delta}=0.18 in the Cu(1) layer has been studied by neutron diffraction and nuclear quadrupole resonance (NQR). The crystal orders magnetically from the paramagnetic state to the antiferromagnetic AFI state at the N{acute e}el temperature T{sub N}=403 K with an empirical critical exponent of {beta}=0.26. Reordering to the antiferromagnetic AFII state sets in at T{sub 2}=12 K. In both the AFI and AFII phases the ordered magnetic moments on the Cu(2) lattice sites are identical and take a value of {l_angle}S{r_angle}{sub Cu(2)}{approx}0.56{mu}{sub B}; no ordered moment is found on the Cu(1) lattice sites. From the temperature dependence of the Cu(1) NQR spectrum, the magnetic hyperfine field at Cu(1) sites is found to vary continuously as a function of temperature. This result indicates unequivocally that the AFI{leftrightarrow}AFII reordering takes place via a noncollinear intermediate turn angle phase AFI{circle_plus}II. {copyright} {ital 1997} {ital The American Physical Society}

  19. NQR investigation of pressure-induced charge transfer in oxygen-deficient YBa{sub 2}Cu{sub 3}O{sub 7-{delta}} ({delta} = 0.38)

    SciTech Connect

    Reyes, A.P.; Ahrens, E.T.; Hammel, P.C.; Heffner, R.H.; Takigawa, M.

    1992-03-01

    Measurements of the pressure dependence of {sup 63}Cu nuclear quadrupole frequency in YBa{sub 2}Cu{sub 3}O{sub 6.62} from ambient pressure up to 1.5 GPa at 4k have been performed. {Tc} was found to increase with pressure: d{Tc}/dp {approximately} 5 K/GPa. All observed NQR lines are linear in pressure: dln{nu}{sub Q}/dp=z. We found positive z for the empty chain sites, consistent with ionic (Cu{sup 1+}) configuration in which the atom simply feels a squeezing lattice. Planar coppers close to the empty chains have positive z, while those that are close to full chains have z {approximately} 0. We present an analysis of the NQR result on the basis of the charge transfer model in which the mobile charges migrate from the chain to the plane sites. We deduced that a transfer of 0.021 holes to the O(2,3) sites would explain the result in YBa{sub 2}Cu{sub 3}O{sub 6.62}, whereas only 0.007 holes transfer in fully oxygenated YBa{sub 2}Cu{sub 3}O{sub 7}.

  20. NMR techniques in the study of cardiovascular structure and functions

    SciTech Connect

    Osbakken, M.; Haselgrove, J.

    1987-01-01

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

  1. Number of CuO2 layers dependence of magnetic quantum criticality in homogeneously doped high-T copper oxides: A 63Cu-NMR study on four-layered high-T compounds HgBa2Ca3Cu4O8+y

    NASA Astrophysics Data System (ADS)

    Itohara, Keita; Shimizu, Sunao; Mukuda, Hidekazu; Kitaoka, Yoshio; Shirage, Parasharam M.; Kito, Hijiri; Iyo, Akira

    2010-12-01

    We report 63Cu-NMR/NQR studies on Hg-based four-layered compounds HgBa2Ca3Cu4 O8+y (Hg-1234) with T=123, 110, and 95 K. The 63Cu Knight shift measurements have revealed that the carrier density (N) monotonously decreases with decreasing T. Although static magnetic order was not observed at N=0.15 for the IP with T=95K, it was revealed that antiferromagnetic correlations critically develop, preventing from observing the NMR spectrum below ˜200 K far above T. Thus, we deduce that a magnetic quantum critical point, where an AFM order collapses, may exist at slightly less than N˜0.15 in the Hg-based four-layered compounds, which is lower than that in Hg-based five-layered compounds, N˜0.17. This result suggests that a magnetic interlayer coupling, which stabilizes an AFM order, becomes weaker in the four-layered compounds than in five-layered compounds.

  2. Asymmetric NMR lineshapes and precision magnetometry

    NASA Astrophysics Data System (ADS)

    Cowan, Brian

    1996-04-01

    In an inhomogeneous magnetic field of asymmetric distribution the observed NMR precession frequency of a liquid will vary with time. We show that the initial frequency corresponds to the mean of the absorption spectrum whereas the final precession frequency corresponds to the peak of the spectrum. Precision magnetometry requires knowledge of the mean so that reliable extrapolation to the zero-time value of the frequency is required. We demonstrate that, as with the narrowing of NMR lines, the effect of atomic motion is to cause the precession frequency to relax in an exponential manner. The importance of these results is discussed in the comparison of proton magnetic resonance in water and NMR in gaseous 0957-0233/7/4/028/img1 for precision magnetometry.

  3. Review of NMR characterization of pyrolysis oils

    DOE PAGES

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; ...

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterizationmore » and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.« less

  4. Review of NMR characterization of pyrolysis oils

    SciTech Connect

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; Adhikari, Sushil; Ragauskas, Arthur J.

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterization and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.

  5. A modularized pulse programmer for NMR spectroscopy

    NASA Astrophysics Data System (ADS)

    Mao, Wenping; Bao, Qingjia; Yang, Liang; Chen, Yiqun; Liu, Chaoyang; Qiu, Jianqing; Ye, Chaohui

    2011-02-01

    A modularized pulse programmer for a NMR spectrometer is described. It consists of a networked PCI-104 single-board computer and a field programmable gate array (FPGA). The PCI-104 is dedicated to translate the pulse sequence elements from the host computer into 48-bit binary words and download these words to the FPGA, while the FPGA functions as a sequencer to execute these binary words. High-resolution NMR spectra obtained on a home-built spectrometer with four pulse programmers working concurrently demonstrate the effectiveness of the pulse programmer. Advantages of the module include (1) once designed it can be duplicated and used to construct a scalable NMR/MRI system with multiple transmitter and receiver channels, (2) it is a totally programmable system in which all specific applications are determined by software, and (3) it provides enough reserve for possible new pulse sequences.

  6. NMR Spectroscopy: Processing Strategies (by Peter Bigler)

    NASA Astrophysics Data System (ADS)

    Mills, Nancy S.

    1998-06-01

    Peter Bigler. VCH: New York, 1997. 249 pp. ISBN 3-527-28812-0. $99.00. This book, part of a four-volume series planned to deal with all aspects of a standard NMR experiment, is almost the exact book I have been hoping to find. My department has acquired, as have hundreds of other undergraduate institutions, high-field NMR instrumentation and the capability of doing extremely sophisticated experiments. However, the training is often a one- or two-day experience in which the material retained by the faculty trained is garbled and filled with holes, not unlike the information our students seem to retain. This text, and the accompanying exercises based on data contained on a CD-ROM, goes a long way to fill in the gaps and clarify misunderstandings about NMR processing.

  7. Review of NMR characterization of pyrolysis oils

    SciTech Connect

    Hao, Naijia; Ben, Haoxi; Yoo, Chang Geun; Adhikari, Sushil; Ragauskas, Arthur J.

    2016-08-24

    Here, pyrolysis of renewable biomass has been developed as a method to produce green fuels and chemicals in response to energy security concerns as well as to alleviate environmental issues incurred with fossil fuel usage. However, pyrolysis oils still have limited commercial application, mainly because unprocessed oils cannot be readily blended with current petroleum-based transportation fuels. To better understand these challenges, researchers have applied diverse characterization techniques in the development of bio-oil studies. In particular, nuclear magnetic resonance (NMR) is a key spectroscopic characterization method through analysis of bio-oil components. This review highlights the NMR strategies for pyrolysis oil characterization and critically discusses the applications of 1H, 13C, 31P, 19F, and two-dimensional (2-D NMR) analyses such as heteronuclear single quantum correlation (HSQC) in representative pyrolysis oil studies.

  8. NMR phase noise in bitter magnets.

    PubMed

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

    2001-02-01

    We have studied the temporal instability of a high field resistive Bitter magnet through nuclear magnetic resonance (NMR). This instability leads to transverse spin decoherence in repeated and accumulated NMR experiments as is normally performed during signal averaging. We demonstrate this effect via Hahn echo and Carr--Purcell--Meiboom--Gill (CPMG) transverse relaxation experiments in a 23-T resistive magnet. Quantitative analysis was found to be consistent with separate measurements of the magnetic field frequency fluctuation spectrum, as well as with independent NMR experiments performed in a magnetic field with a controlled instability. Finally, the CPMG sequence with short pulse delays is shown to be successful in recovering the intrinsic spin--spin relaxation even in the presence of magnetic field temporal instability. Copyright 2001 Academic Press.

  9. Remote tuning of NMR probe circuits.

    PubMed

    Kodibagkar, V D; Conradi, M S

    2000-05-01

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

  10. Solid-state NMR of proteins sedimented by ultracentrifugation

    PubMed Central

    Bertini, Ivano; Luchinat, Claudio; Parigi, Giacomo; Ravera, Enrico; Reif, Bernd; Turano, Paola

    2011-01-01

    Relatively large proteins in solution, spun in NMR rotors for solid samples at typical ultracentrifugation speeds, sediment at the rotor wall. The sedimented proteins provide high-quality solid-state-like NMR spectra suitable for structural investigation. The proteins fully revert to the native solution state when spinning is stopped, allowing one to study them in both conditions. Transiently sedimented proteins can be considered a novel phase as far as NMR is concerned. NMR of transiently sedimented molecules under fast magic angle spinning has the advantage of overcoming protein size limitations of solution NMR without the need of sample crystallization/precipitation required by solid-state NMR. PMID:21670262

  11. Contact replacement for NMR resonance assignment.

    PubMed

    Xiong, Fei; Pandurangan, Gopal; Bailey-Kellogg, Chris

    2008-07-01

    Complementing its traditional role in structural studies of proteins, nuclear magnetic resonance (NMR) spectroscopy is playing an increasingly important role in functional studies. NMR dynamics experiments characterize motions involved in target recognition, ligand binding, etc., while NMR chemical shift perturbation experiments identify and localize protein-protein and protein-ligand interactions. The key bottleneck in these studies is to determine the backbone resonance assignment, which allows spectral peaks to be mapped to specific atoms. This article develops a novel approach to address that bottleneck, exploiting an available X-ray structure or homology model to assign the entire backbone from a set of relatively fast and cheap NMR experiments. We formulate contact replacement for resonance assignment as the problem of computing correspondences between a contact graph representing the structure and an NMR graph representing the data; the NMR graph is a significantly corrupted, ambiguous version of the contact graph. We first show that by combining connectivity and amino acid type information, and exploiting the random structure of the noise, one can provably determine unique correspondences in polynomial time with high probability, even in the presence of significant noise (a constant number of noisy edges per vertex). We then detail an efficient randomized algorithm and show that, over a variety of experimental and synthetic datasets, it is robust to typical levels of structural variation (1-2 AA), noise (250-600%) and missings (10-40%). Our algorithm achieves very good overall assignment accuracy, above 80% in alpha-helices, 70% in beta-sheets and 60% in loop regions. Our contact replacement algorithm is implemented in platform-independent Python code. The software can be freely obtained for academic use by request from the authors.

  12. Contact replacement for NMR resonance assignment

    PubMed Central

    Xiong, Fei; Pandurangan, Gopal; Bailey-Kellogg, Chris

    2008-01-01

    Motivation: Complementing its traditional role in structural studies of proteins, nuclear magnetic resonance (NMR) spectroscopy is playing an increasingly important role in functional studies. NMR dynamics experiments characterize motions involved in target recognition, ligand binding, etc., while NMR chemical shift perturbation experiments identify and localize protein–protein and protein–ligand interactions. The key bottleneck in these studies is to determine the backbone resonance assignment, which allows spectral peaks to be mapped to specific atoms. This article develops a novel approach to address that bottleneck, exploiting an available X-ray structure or homology model to assign the entire backbone from a set of relatively fast and cheap NMR experiments. Results: We formulate contact replacement for resonance assignment as the problem of computing correspondences between a contact graph representing the structure and an NMR graph representing the data; the NMR graph is a significantly corrupted, ambiguous version of the contact graph. We first show that by combining connectivity and amino acid type information, and exploiting the random structure of the noise, one can provably determine unique correspondences in polynomial time with high probability, even in the presence of significant noise (a constant number of noisy edges per vertex). We then detail an efficient randomized algorithm and show that, over a variety of experimental and synthetic datasets, it is robust to typical levels of structural variation (1–2 AA), noise (250–600%) and missings (10–40%). Our algorithm achieves very good overall assignment accuracy, above 80% in α-helices, 70% in β-sheets and 60% in loop regions. Availability: Our contact replacement algorithm is implemented in platform-independent Python code. The software can be freely obtained for academic use by request from the authors. Contact: gopal@cs.purdue.edu; cbk@cs.dartmouth.edu PMID:18586716

  13. An NMR Study of Microvoids in Polymers

    NASA Technical Reports Server (NTRS)

    Toy, James; Mattrix, Larry

    1996-01-01

    An understanding of polymer defect structures, like microvoids in polymeric matrices, is most crucial to their fabrication and application potential. In this project guest atoms are introduced into the microvoids in PMR-15 and NMR is used to determine microvoid sizes and locations. Xenon is a relatively inert probe that would normally not be found naturally in polymer or in NMR probe materials. There are two NMR active Xenon isotopes, Xe-129 and Xe-131. The Xe atom has a very high polarizability, which makes it sensitive to the intracrystalline environment of polymers. Interactions between the Xe atoms and the host matrix perturb and Xe electron cloud, deshielding the nuclei, and thereby expanding the range of the observed NMR chemical shifts. This chemical shift range which may be as large as 5000 ppm, permits subtle structural and chemical effects to be studied with high sensitivity. The Xe-129-NMR line shape has been found to vary in response to changes in the pore symmetry of the framework hosts in Zeolites and Clathrasil compounds. Before exposure to Xe gas, the PMR-15 samples were dried in a vacuum oven at 150 C for 48 hours. The samples were then exposed to Xe gas at 30 psi for 72 hours and sealed in glass tubes with 1 atmosphere of Xenon gas. Xenon gas at 1 atmosphere was used to tune up the spectrometer and to set up the appropriate NMR parameters. A series of spectra were obtained interspersed with applications of vacuum and heating to drive out the adsorbed Xe and determine the role of Xe-Xe interactions in the observed chemical shift.

  14. Hyperpolarized Xenon for NMR and MRI Applications

    PubMed Central

    Witte, Christopher; Kunth, Martin; Döpfert, Jörg; Rossella, Federica; Schröder, Leif

    2012-01-01

    Nuclear magnetic resonance (NMR) spectroscopy and imaging (MRI) suffer from intrinsic low sensitivity because even strong external magnetic fields of ~10 T generate only a small detectable net-magnetization of the sample at room temperature 1. Hence, most NMR and MRI applications rely on the detection of molecules at relative high concentration (e.g., water for imaging of biological tissue) or require excessive acquisition times. This limits our ability to exploit the very useful molecular specificity of NMR signals for many biochemical and medical applications. However, novel approaches have emerged in the past few years: Manipulation of the detected spin species prior to detection inside the NMR/MRI magnet can dramatically increase the magnetization and therefore allows detection of molecules at much lower concentration 2. Here, we present a method for polarization of a xenon gas mixture (2-5% Xe, 10% N2, He balance) in a compact setup with a ca. 16000-fold signal enhancement. Modern line-narrowed diode lasers allow efficient polarization 7 and immediate use of gas mixture even if the noble gas is not separated from the other components. The SEOP apparatus is explained and determination of the achieved spin polarization is demonstrated for performance control of the method. The hyperpolarized gas can be used for void space imaging, including gas flow imaging or diffusion studies at the interfaces with other materials 8,9. Moreover, the Xe NMR signal is extremely sensitive to its molecular environment 6. This enables the option to use it as an NMR/MRI contrast agent when dissolved in aqueous solution with functionalized molecular hosts that temporarily trap the gas 10,11. Direct detection and high-sensitivity indirect detection of such constructs is demonstrated in both spectroscopic and imaging mode. PMID:22986346

  15. An optical NMR spectrometer for Larmor-beat detection and high-resolution POWER NMR

    NASA Astrophysics Data System (ADS)

    Kempf, J. G.; Marohn, J. A.; Carson, P. J.; Shykind, D. A.; Hwang, J. Y.; Miller, M. A.; Weitekamp, D. P.

    2008-06-01

    Optical nuclear magnetic resonance (ONMR) is a powerful probe of electronic properties in III-V semiconductors. Larmor-beat detection (LBD) is a sensitivity optimized, time-domain NMR version of optical detection based on the Hanle effect. Combining LBD ONMR with the line-narrowing method of POWER (perturbations observed with enhanced resolution) NMR further enables atomically detailed views of local electronic features in III-Vs. POWER NMR spectra display the distribution of resonance shifts or line splittings introduced by a perturbation, such as optical excitation or application of an electric field, that is synchronized with a NMR multiple-pulse time-suspension sequence. Meanwhile, ONMR provides the requisite sensitivity and spatial selectivity to isolate local signals within macroscopic samples. Optical NMR, LBD, and the POWER method each introduce unique demands on instrumentation. Here, we detail the design and implementation of our system, including cryogenic, optical, and radio-frequency components. The result is a flexible, low-cost system with important applications in semiconductor electronics and spin physics. We also demonstrate the performance of our systems with high-resolution ONMR spectra of an epitaxial AlGaAs /GaAs heterojunction. NMR linewidths down to 4.1Hz full width at half maximum were obtained, a 103-fold resolution enhancement relative any previous optically detected NMR experiment.

  16. Sensitive detection of NMR for thin films.

    PubMed

    Lee, Soonchil

    2015-10-01

    NMR can provide valuable information about thin films, but its relatively low sensitivity allows data acquisition only from bulk samples. The sensitivity problem is circumvented by detection schemes with higher sensitivity and/or enhanced polarization. In most of these ingenious techniques, electrons play a central role through hyperfine interactions with the nuclei of interest or the conversion of the spin orientation to an electric charge. The state of the art in NMR is the control of a single nuclear spin state, the complete form of which is one of the ultimate goals of nanotechnology. Copyright © 2015 Elsevier Inc. All rights reserved.

  17. (13)C NMR Metabolomics: INADEQUATE Network Analysis.

    PubMed

    Clendinen, Chaevien S; Pasquel, Christian; Ajredini, Ramadan; Edison, Arthur S

    2015-06-02

    The many advantages of (13)C NMR are often overshadowed by its intrinsically low sensitivity. Given that carbon makes up the backbone of most biologically relevant molecules, (13)C NMR offers a straightforward measurement of these compounds. Two-dimensional (13)C-(13)C correlation experiments like INADEQUATE (incredible natural abundance double quantum transfer experiment) are ideal for the structural elucidation of natural products and have great but untapped potential for metabolomics analysis. We demonstrate a new and semiautomated approach called INETA (INADEQUATE network analysis) for the untargeted analysis of INADEQUATE data sets using an in silico INADEQUATE database. We demonstrate this approach using isotopically labeled Caenorhabditis elegans mixtures.

  18. The Quiet Renaissance of Protein NMR

    PubMed Central

    Barrett, Paul J.; Chen, Jiang; Cho, Min-Kyu; Kim, Ji-Hun; Lu, Zhenwei; Mathew, Sijo; Peng, Dungeng; Song, Yuanli; Van Horn, Wade D.; Zhuang, Tiandi; Sönnichsen, Frank D.; Sanders, Charles R.

    2013-01-01

    From roughly 1985 through the start of the new millennium, the cutting edge of solution protein nuclear magnetic resonance (NMR) spectroscopy was to a significant extent driven by the aspiration to determine structures. Here we survey recent advances in protein NMR that herald a renaissance in which a number of its most important applications reflect the broad problem-solving capability displayed by this method during its classical era during the 1970s and early 80s. “Without receivers fitted and kept in order, the air may tingle and thrill with the message, but it will not reach my spirit and consciousness.” Mary Slessor, Calabar, circa 1910 PMID:23368985

  19. Magic Angle Spinning NMR of Viruses

    PubMed Central

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

    2015-01-01

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

  20. New Designs for NMR Core Scanning

    NASA Astrophysics Data System (ADS)

    Bluemich, B.; Anferova, S.; Talnishnikh, E.; Arnold, J.; Clauser, C.

    2006-12-01

    Within the last ten years, mobile magnetic resonance has moved from the oil field to many new areas of application. While the focus of mobile NMR in the past was on single-sided or inside-out NMR, the advent of tube-shaped Halbach magnets has introduced the conventional outside-in NMR concept to mobile NMR where the object is inside a magnet. Our Halbach magnet is constructed from small magnet blocks at light weight and low cost with a magnetic field sufficiently homogeneous. To automatize NMR measurements, the Halbach magnet is mounted on a sliding table to scan long core sections without human interaction. In homogeneous magnetic fields, the longitudinal relaxation time T1 and even the transverse relaxation time T2 are proportional to the pore diameters of rocks. Hence, the T1 and T2 signals map the pore-size distribution of the studied rock cores. For fully saturated samples the integral of the distribution curve is proportional to porosity. The porosity values from NMR measurements with the Halbach magnet are used to estimate permability. The Halbach magnet can be used for certain sample geometries in combination with exchangeable radio frequency (rf) coils with different diameters from 24 mm up to 80 mm. To measure standard Ocean Drilling Program (ODP)/Integrated Ocean Drilling Program (IODP) cores, which have a standard diameter of 60 mm and are split lengthwise after recovery, we use a surface figure-8 rf coil with an inner diameter of 60 mm. Besides 1D T2 measurements, we perform relaxation-relaxation correlation experiments, where T1 and T2 are measured in parallel. In this way, the influence of diffusion on the shape of the T2 distribution function is probed. A gradient coil system was designed to perform Pulsed Field Gradients (PFG) experiments. As the gradient coils restrict the axial access to the magnet, only cylindrical core plugs with 20 mm in diameter can be analysed by PFG NMR methods. The homogeneity of the magnetic field in the sensitive volume