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Sample records for 7li nmr spectroscopic

  1. Report for in-situ 7Li NMR experiment in PNNL Phase -1

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi [Pacific Northwest National Laboratory

    2014-08-19

    To understand the detailed local structural evolution, an in-situ 7Li NMR study was performed. An operando identification of the lithium germanide phases under various cycling regimens permitted understanding of the kinetics of phase transition between different structural phases, including the amorphous phases, and how these correlated with capacity retention. Combining data from TEM and in-situ 7Li NMR, we discovered that the phase inter-conversion during cycling was mediated by co-existing amorphous and crystalline phases, and that the high capacity observed was correlated with an over-lithiated lithium germanide phase.

  2. Probing the location and distribution of paramagnetic centers in alkali metal-loaded zeolites through (7)Li MAS NMR.

    Science.gov (United States)

    Terskikh, Victor V; Ratcliffe, Christopher I; Ripmeester, John A; Reinhold, Catherine J; Anderson, Paul A; Edwards, Peter P

    2004-09-15

    The nature and surroundings of lithium cations in lithium-exchanged X and A zeolites following loading with the alkali metals Na, K, Rb, and Cs have been studied through (7)Li solid-state NMR spectroscopy. It is demonstrated that the lithium in these zeolites is stable with respect to reduction by the other alkali metals. Even though the lithium cations are not directly involved in chemical interactions with the excess electrons introduced in the doping process, the corresponding (7)Li NMR spectra are extremely sensitive to paramagnetic species that are located inside the zeolite cavities. This sensitivity makes (7)Li NMR a useful probe to study the formation, distribution, and transformation of such species.

  3. Structural investigation of aryllithium clusters in solution. I. A 13C and 7Li NMR studyof phenyllithium and some methyl-substituted phenyllithium derivatives

    NARCIS (Netherlands)

    Koten, G. van; Wehman, E.; Jastrzebski, J.T.B.H.; Ernsting, J.M.; Grove, D.M.

    1988-01-01

    }1{}3{C and }7{Li NMR spectra of phenyllithium and several methyl subsituted phenyllithium derivatives have been recorded in the presence of known amounts of coordinating solvents such as monodentate diethyl ether and THF and the potentially bidentate TMEDA (tetramethylethylenediamine). The relative

  4. Accurate Analytic Potential Energy Function and Spectroscopic Study for G1 ∏g State of Dimer 7Li2

    Institute of Scientific and Technical Information of China (English)

    SHI De-Heng; MA Heng; SUN Jin-Feng; ZHU Zun-Lue

    2007-01-01

    The reasonable dissociation limit for the G1∏g state of dimer 7Li2 is determined. The equilibrium internuclear distance, dissociation energy, harmonic frequency, vibrational zero energy, and adiabatic excitation energy are calculated using a symmetry-adapted-cluster configuration-interaction method in complete active space in Gaussian03 program package at such numerous basis sets as 6-311++G, 6-311++G(2df, 2pd), 6-311++G(2df, p), cc-PVTZ, 6-311++G(3df, 3pd), CEP-121G, 6-311++G(2df, pd), 6-311++G(d,p),6-311G(3df,3pd), D95(3df,3pd), 6-311++G(3df, 2p),6-311++G(2df), 6-311++G(df, pd) D95V++, and DGDZVP. The complete potential energy curves are obtained at these sets over a wide internuclear distance range and have least squares fitted to Murrell-Sorbie function. The conclusion shows that the basis set 6-311++G(2df, p) is a most suitable one for the G1∏g state. At this basis set, the calculated spectroscopic constants Te, De, Eo, Re, ωe, ωeXe, αe, and Be are of 3.9523 eV, 0.813 06 eV, 113.56 cm-1, 0.320 15 nm,227.96 cm-1, 1.6928 cm-1, 0.004 436 cm-1, and 0.4689 cm-1, respectively, which are in good agreement with measurements whenever available. The total 50 vibrational levels and corresponding inertial rotation constants are for the first time calculated and compared with available RKR data. And good agreement with measurements is obtained.

  5. Lithium ion micrometer diffusion in a garnet-type cubic Li7La3Zr2O12 (LLZO) studied using 7Li NMR spectroscopy

    Science.gov (United States)

    Hayamizu, Kikuko; Seki, Shiro; Haishi, Tomoyuki

    2017-01-01

    Mobile lithium ions in a cubic garnet Li7La3Zr2O12 (Al-stabilized) were studied using 7Li NMR spectroscopy for membrane and powder samples, the latter of which was ground from the membrane. Lithium diffusion in a micrometer space was measured using the pulsed-gradient spin-echo 7Li NMR method between 70 and 130 °C. When the observation time (Δ ) was shorter than 20 ms, the echo attenuation showed diffusive diffraction patterns, indicating that the Li+ diffusing space is not free but restricted. For longer Δ, the values of apparent diffusion constant (Dapparent) became gradually smaller to approach an equilibrated value (close to a tracer diffusion constant). In addition, the Dapparent depends on the pulse field gradient strength (g) and became smaller as g became larger. These experimental results suggest that the lithium ions diffuse through Li+ pathways surrounded by stationary anions and lithium ions, and are affected by collisions and diffractions. One-dimensional profiles of the membrane sample of thickness 0.5 mm were observed from 65 to 110 °C and the area intensity, as well as the lithium occurrence near the surface, increased with the increase in temperature. The temperature-dependent area intensity showed a correspondence to the number of Li+ carrier ions estimated from the ionic conductivity and the equilibrated diffusion constant through the Nernst-Einstein relationship.

  6. Lithium ion micrometer diffusion in a garnet-type cubic Li7La3Zr2O12 (LLZO) studied using (7)Li NMR spectroscopy.

    Science.gov (United States)

    Hayamizu, Kikuko; Seki, Shiro; Haishi, Tomoyuki

    2017-01-14

    Mobile lithium ions in a cubic garnet Li7La3Zr2O12 (Al-stabilized) were studied using (7)Li NMR spectroscopy for membrane and powder samples, the latter of which was ground from the membrane. Lithium diffusion in a micrometer space was measured using the pulsed-gradient spin-echo (7)Li NMR method between 70 and 130 °C. When the observation time (Δ) was shorter than 20 ms, the echo attenuation showed diffusive diffraction patterns, indicating that the Li(+) diffusing space is not free but restricted. For longer Δ, the values of apparent diffusion constant (Dapparent) became gradually smaller to approach an equilibrated value (close to a tracer diffusion constant). In addition, the Dapparent depends on the pulse field gradient strength (g) and became smaller as g became larger. These experimental results suggest that the lithium ions diffuse through Li(+) pathways surrounded by stationary anions and lithium ions, and are affected by collisions and diffractions. One-dimensional profiles of the membrane sample of thickness 0.5 mm were observed from 65 to 110 °C and the area intensity, as well as the lithium occurrence near the surface, increased with the increase in temperature. The temperature-dependent area intensity showed a correspondence to the number of Li(+) carrier ions estimated from the ionic conductivity and the equilibrated diffusion constant through the Nernst-Einstein relationship.

  7. Lithium diffusion in a new cathode material Li0.8[Ni0.6Sb0.4]O2 studied by 7Li NMR

    Directory of Open Access Journals (Sweden)

    Salikhov T., Klysheva E., Zvereva E., Nalbandyan V., Shukaev I., Medvedev B., Vavilova E.

    2016-12-01

    Full Text Available A rhombohedral layered α-NaFeO2-type compound, Lix[Ni(1+x/3Sb(2-x/3]O2 (x=0.8 has been prepared from the sodium analogue by ion exchange at 570 K. In contrast to the stoichiometric composition Li3Ni2SbO6, it shows considerable Li/Ni inversion and no long-range Ni/Sb ordering. The temperature dependence of the 7Li NMR spin-lattice relaxation rate and linewidth data measured at temperature range from 30-450 K show the sharp increase of lithium ions mobility comparing to the stoichiometric compound Li3Ni2SbO6. From the NMR data the activation energy was estimated by different methods.

  8. Two phase morphology limits lithium diffusion in TiO(2)(anatase): a (7)Li MAS NMR study.

    Science.gov (United States)

    Wagemaker, M; van de Krol, R; Kentgens, A P; van Well, A A; Mulder, F M

    2001-11-21

    7Li magic angle spinning solid-state nuclear magnetic resonance is applied to investigate the lithium local environment and lithium ion mobility in tetragonal anatase TiO(2) and orthorhombic lithium titanate Li(0.6)TiO(2). Upon lithium insertion, an increasing fraction of the material changes its crystallographic structure from anatase TiO(2) to lithium titanate Li(0.6)TiO(2). Phase separation occurs, and as a result, the Li-rich lithium titanate phase is coexisting with the Li-poor TiO(2) phase containing only small Li amounts approximately equal to 0.01. In both the anatase and the lithium titanate lattice, Li is found to be hopping over the available sites with activation energies of 0.2 and 0.09 eV, respectively. This leads to rapid microscopic diffusion rates at room temperature (D(micr) = 4.7 x 10(-12) cm(2)s(-1) in anatase and D(micr) = 1.3 x 10(-11) cm(2)s(-1) in lithium titanate). However, macroscopic intercalation data show activation energies of approximately 0.5 eV and smaller diffusion coefficients. We suggest that the diffusion through the phase boundary is determining the activation energy of the overall diffusion and the overall diffusion rate itself. The chemical shift of lithium in anatase is independent of temperature up to approximately 250 K but decreases at higher temperatures, reflecting a change in the 3d conduction electron densities. The Li mobility becomes prominent from this same temperature showing that such electronic effects possibly facilitate the mobility.

  9. {sup 7}Li NMR spectroscopy and ion conduction mechanism of composite gel polymer electrolyte: A comparative study with variation of salt and plasticizer with filler

    Energy Technology Data Exchange (ETDEWEB)

    Saikia, D. [Department of Chemistry, Center for Nanotechnology and R and D Center for Membrane Technology, Chung Yuan Christian University, Chung Li 32023, Taiwan (China); Chen-Yang, Y.W. [Department of Chemistry, Center for Nanotechnology and R and D Center for Membrane Technology, Chung Yuan Christian University, Chung Li 32023, Taiwan (China)], E-mail: yuiwhei@cycu.edu.tw; Chen, Y.T.; Li, Y.K.; Lin, S.I. [Department of Chemistry, Center for Nanotechnology and R and D Center for Membrane Technology, Chung Yuan Christian University, Chung Li 32023, Taiwan (China)

    2009-01-30

    Microporous composite gel polymer electrolyte (CGPE) has been prepared by incorporating the home-made silica aerogel (SAG) particles into the poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF-HFP) copolymer/LiClO{sub 4} matrix. The ionic transport behavior of the electrolyte is studied with various experimental techniques such as AC impedance, X-ray diffraction (XRD), infrared (IR) spectra, nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), differential scanning calorimetry (DSC) and thermogravimetric analyzer (TGA), etc. The results reveal that the SAG particles are well dispersed in the electrolytes and incorporate with the other components of the CGPEs. The solid-state {sup 7}Li NMR study has confirmed the interactions of lithium ion with SAG, polymer and plasticizers, causing to form the microporous structure and reduce the glass transition temperature and crystallinity, resulting in an increase in ionic conductivity of the CGPE. The best ionic conductivity (1.04 x 10{sup -2} S/cm at room temperature) is obtained from the composite polymer electrolyte containing 4 wt% of SAG, which is approximately four times higher than the ionic conductivity of the electrolyte without the filler.

  10. Relation of short-range and long-range lithium ion dynamics in glass-ceramics: Insights from 7Li NMR field-cycling and field-gradient studies

    Science.gov (United States)

    Haaks, Michael; Martin, Steve W.; Vogel, Michael

    2017-09-01

    We use various 7Li NMR methods to investigate lithium ion dynamics in 70Li 2S-30 P 2S5 glass and glass-ceramic obtained from this glass after heat treatment. We employ 7Li spin-lattice relaxometry, including field-cycling measurements, and line-shape analysis to investigate short-range ion jumps as well as 7Li field-gradient approaches to characterize long-range ion diffusion. The results show that ceramization substantially enhances the lithium ion mobility on all length scales. For the 70Li 2S-30 P 2S5 glass-ceramic, no evidence is found that bimodal dynamics result from different ion mobilities in glassy and crystalline regions of this sample. Rather, 7Li field-cycling relaxometry shows that dynamic susceptibilities in broad frequency and temperature ranges can be described by thermally activated jumps governed by a Gaussian distribution of activation energies g (Ea) with temperature-independent mean value Em=0.43 eV and standard deviation σ =0.07 eV . Moreover, use of this distribution allows us to rationalize 7Li line-shape results for the local ion jumps. In addition, this information about short-range ion dynamics further explains 7Li field-gradient results for long-range ion diffusion. In particular, we quantitatively show that, consistent with our experimental results, the temperature dependence of the self-diffusion coefficient D is not described by the mean activation energy Em of the local ion jumps, but by a significantly smaller apparent value whenever the distribution of correlation times G (logτ ) of the jump motion derives from an invariant distribution of activation energies and, hence, continuously broadens upon cooling. This effect occurs because the harmonic mean, which determines the results of diffusivity or also conductivity studies, continuously separates from the peak position of G (logτ ) when the width of this distribution increases.

  11. Ab initio calculations on the spectroscopic constants,vibrational levels and classical turning points for the 21Πu state of dimer 7Li2

    Institute of Scientific and Technical Information of China (English)

    Liu Yu-Fang; Sun Jin-Feng; Ma Heng; Zhu Zun-Lue

    2007-01-01

    The accurate dissociation energy and harmonic frequency for the highly excited 21 Πu state of dimer 7Li2 have been calculated using a symmetry-adapted-cluster configuration-interaction method in complete active space.The calculated results are in excellent agreement with experimental measurements.The potential energy curves at numerous basis sets for this state are obtained over a wide internuclear separation range from about 2.4ao to 37.0ao.And the conclusion is gained that the basis set 6-311++G(d,p) is a most suitable one.The calculated spectroscopic constants De,Re,ωe,ωeχe,αe and Be at 6-311++G(d,p) are 0.9670 eV,0.3125 nm,238.6 cm-1,1.3705cm-1,0.0039 cm-1 and 0.4921 cm-1.respectively.The vibrational levels are calculated by solving the radial Schr(o)dinger equation of nuclear motion.A total of 53 vibrational levels are found and reported for the first time.The classical turning points have been computed.Comparing with the measurements,in which only the first nine vibrational levels have been obtained so far,the present calculations are very encouraging.A careful comparison of the present results of the parameters De and ωe with those obtained from previous theories clearly shows that the present calculations are much closer to the measurements than previous theoretical results,thus representing an improvement on the accuracy of the ab initio calculations of the potentials for this state.

  12. 7Li NMR chemical shift titration and theoretical DFT calculation studies: solvent and anion effects on second-order complexation of 12-crown-4 and 1-aza-12-crown-4 with lithium cation in several aprotic solvents.

    Science.gov (United States)

    Masiker, Marilyn C; Mayne, Charles L; Boone, Brian J; Orendt, Anita M; Eyring, Edward M

    2010-02-01

    (7)Li NMR titration was used to determine stepwise complexation constants for the second-order complexation of lithium cation with 12-crown-4 in acetonitrile, propylene carbonate and a binary mixture of propylene carbonate and dimethyl carbonate. The anions used were perchlorate, hexaflurophosphate and trifluromethanesulfonate. A second ligand 1-aza-12-crown-4 was similarly investigated. The exchange between the free and complexed cation in these reactions is fast on an NMR timescale resulting in a single lithium peak which is a concentration-weighted average of the free and bound species. Solvent effects show that the 1:1 complex is much more stable in acetonitrile than in propylene carbonate or in the propylene carbonate dimethyl carbonate mixture. Anion effects for a given solvent were small. Optimized geometries of the free ligands and the 1:1 and 1:2 (sandwich) metal-ligand complexes were predicted by hybrid-density functional theory using the Gaussian 03 software package. Results were compared to literature values for 1:1 stability constants found by microcalorimetry for several of these systems and are found to be in good agreement. Although microcalorimetry only considered the formation of 1:1 complexes, (7)Li NMR shows evidence that both 1:1 and 1:2 complexes should be considered.

  13. nmr spectroscopic study and dft calculations of giao nmr shieldings ...

    African Journals Online (AJOL)

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    various fields of science and industry such as microelectronic and aerospace ... GIAO/DFT (Gauge Including Atomic Orbitals/Density Functional Theory) approach is .... successfully by using NMR and quantum chemical calculations.

  14. 2D NMR-spectroscopic screening reveals polyketides in ladybugs

    OpenAIRE

    Deyrup, Stephen T.; Eckman, Laura E.; McCarthy, Patrick H.; Smedley, Scott R.; Meinwald, Jerrold; Schroeder, Frank C.

    2011-01-01

    Small molecules of biological origin continue to yield the most promising leads for drug design, but systematic approaches for exploring nature’s cache of structural diversity are lacking. Here, we demonstrate the use of 2D NMR spectroscopy to screen a library of biorationally selected insect metabolite samples for partial structures indicating the presence of new chemical entities. This NMR-spectroscopic survey enabled detection of novel compounds in complex metabolite mixtures without prior...

  15. NMR spin-lattice relaxation study of 7Li and 93Nb nuclei in Ti- or Fe-doped LiNbO3:Mg single crystals

    Directory of Open Access Journals (Sweden)

    Tae Ho Yeom

    2016-04-01

    Full Text Available In this study, to understand the effects of paramagnetic impurities, we investigated the temperature dependent of the spin-lattice relaxation times of pure LiNbO3, LiNbO3:Mg, LiNbO3:Mg/Ti, LiNbO3:Mg/Fe, and LiNbO3:Mg/Fe (thermally treated at 500°C single crystals. The results for the LiNbO3:Mg single crystals doped with Fe3+ or Ti3+ are discussed with respect to the site distribution and atomic mobility of Li and Nb. In addition, the effects of a thermal treatment on LiNbO3:Mg/Fe single crystals were examined based on the T1 analysis of 7Li and 93Nb. It was found that the presence of impurities in the crystals induced systematic changes of activation energies concerning atomic mobility.

  16. Electrochemical performance and 7Li NMR studies on an inverse spinel LiNi 1/3Co 1/3Mn 1/3VO 4 for Li-ion batteries

    Science.gov (United States)

    Fey, George Ting-Kuo; Muralidharan, P.; Cho, Yung-Da; Chang, Pai-Ching; Kao, Hsien-Ming

    A new inverse spinel LiNi 1/3Co 1/3Mn 1/3VO 4 cathode material was synthesized through a citric acid assisted polyethylene glycol (CA:PEG; 3:1, 3:0.5 and 3:0) polymeric method, followed by calcination at 723 K for 5 h in air. The synthesized compound was characterized by TG/DTGA, XRD, FTIR, TEM, and 7Li NMR techniques. TG/DTGA curves showed that the formation of LiNi 1/3Co 1/3Mn 1/3VO 4 occurred between 523 and 673 K and the phase pure crystalline formed at 723 K, as also confirmed by XRD analysis which showed that the crystalline phase peaks formed when heated at 723 K for 5 h in air. TEM images revealed that nanosized particles ranged ∼170-190 nm. FTIR spectra showed that all organic residues were removed and LiNi 1/3Co 1/3Mn 1/3VO 4 formed. The 7Li MAS NMR spectrum of the LiNi 1/3Co 1/3Mn 1/3VO 4 sample revealed that the paramagnetic effect is small and small side band manifolds were observed. The galvanostatic cycling study suggests that the cycle stability and capacity retention were enhanced for LiNi 1/3Co 1/3Mn 1/3VO 4 prepared with a CA:PEG molar ratio of 3:1 when it was cycled between 2.8 and 4.9 V (versus Li) at a 0.15 C rate. The electrochemical impedance behavior suggested that a passive layer was formed on the surface of the cathode materials during continuous cycling.

  17. Lithium Ion Mobility in Lithium Phosphidosilicates: Crystal Structure, (7) Li, (29) Si, and (31) P MAS NMR Spectroscopy, and Impedance Spectroscopy of Li8 SiP4 and Li2 SiP2.

    Science.gov (United States)

    Toffoletti, Lorenzo; Kirchhain, Holger; Landesfeind, Johannes; Klein, Wilhelm; van Wüllen, Leo; Gasteiger, Hubert A; Fässler, Thomas F

    2016-12-05

    The need to improve electrodes and Li-ion conducting materials for rechargeable all-solid-state batteries has drawn enhanced attention to the investigation of lithium-rich compounds. The study of the ternary system Li-Si-P revealed a series of new compounds, two of which, Li8 SiP4 and Li2 SiP2 , are presented. Both phases represent members of a new family of Li ion conductors that display Li ion conductivity in the range from 1.15(7)×10(-6) Scm(-1) at 0 °C to 1.2(2)×10(-4) Scm(-1) at 75 °C (Li8 SiP4 ) and from 6.1(7)×10(-8) Scm(-1) at 0 °C to 6(1)×10(-6) Scm(-1) at 75 °C (Li2 SiP2 ), as determined by impedance measurements. Temperature-dependent solid-state (7) Li NMR spectroscopy revealed low activation energies of about 36 kJ mol(-1) for Li8 SiP4 and about 47 kJ mol(-1) for Li2 SiP2 . Both compounds were structurally characterized by X-ray diffraction analysis (single crystal and powder methods) and by (7) Li, (29) Si, and (31) P MAS NMR spectroscopy. Both phases consist of tetrahedral SiP4 anions and Li counterions. Li8 SiP4 contains isolated SiP4 units surrounded by Li atoms, while Li2 SiP2 comprises a three-dimensional network based on corner-sharing SiP4 tetrahedra, with the Li ions located in cavities and channels.

  18. Fast Li ion dynamics in the solid electrolyte Li7 P3 S11 as probed by (6,7) Li NMR spin-lattice relaxation.

    Science.gov (United States)

    Wohlmuth, Dominik; Epp, Viktor; Wilkening, Martin

    2015-08-24

    The development of safe and long-lasting all-solid-state batteries with high energy density requires a thorough characterization of ion dynamics in solid electrolytes. Commonly, conductivity spectroscopy is used to study ion transport; much less frequently, however, atomic-scale methods such as nuclear magnetic resonance (NMR) are employed. Here, we studied long-range as well as short-range Li ion dynamics in the glass-ceramic Li7 P3 S11 . Li(+) diffusivity was probed by using a combination of different NMR techniques; the results are compared with those obtained from electrical conductivity measurements. Our NMR relaxometry data clearly reveal a very high Li(+) diffusivity, which is reflected in a so-called diffusion-induced (6) Li NMR spin-lattice relaxation peak showing up at temperatures as low as 313 K. At this temperature, the mean residence time between two successful Li jumps is in the order of 3×10(8) s(-1) , which corresponds to a Li(+) ion conductivity in the order of 10(-4) to 10(-3) S cm(-1) . Such a value is in perfect agreement with expectations for the crystalline but metastable glass ceramic Li7 P3 S11 . In contrast to conductivity measurements, NMR analysis reveals a range of activation energies with values ranging from 0.17 to 0.26 eV, characterizing Li diffusivity in the bulk. In our case, through-going Li ion transport, when probed by using macroscopic conductivity spectroscopy, however, seems to be influenced by blocking grain boundaries including, for example, amorphous regions surrounding the Li7 P3 S11 crystallites. As a result of this, long-range ion transport as seen by impedance spectroscopy is governed by an activation energy of approximately 0.38 eV. The findings emphasize how surface and grain boundary effects can drastically affect long-range ionic conduction. If we are to succeed in solid-state battery technology, such effects have to be brought under control by, for example, sophisticated densification or through the preparation

  19. Electric dipolarizability of 7Li

    Indian Academy of Sciences (India)

    Sudhir R Jain; Arun K Jain; S Kailas

    2008-12-01

    We calculate the electric dipolarizability of 7Li nucleus within the cluster model and estimate a value of about 0.0188 fm3. We also discuss the possibility of observing this in the scattering of 7Li from a 208Pb target at energies about 30 MeV.

  20. 2D NMR-spectroscopic screening reveals polyketides in ladybugs.

    Science.gov (United States)

    Deyrup, Stephen T; Eckman, Laura E; McCarthy, Patrick H; Smedley, Scott R; Meinwald, Jerrold; Schroeder, Frank C

    2011-06-14

    Small molecules of biological origin continue to yield the most promising leads for drug design, but systematic approaches for exploring nature's cache of structural diversity are lacking. Here, we demonstrate the use of 2D NMR spectroscopy to screen a library of biorationally selected insect metabolite samples for partial structures indicating the presence of new chemical entities. This NMR-spectroscopic survey enabled detection of novel compounds in complex metabolite mixtures without prior fractionation or isolation. Our screen led to discovery and subsequent isolation of two families of tricyclic pyrones in Delphastus catalinae, a tiny ladybird beetle that is employed commercially as a biological pest control agent. The D. catalinae pyrones are based on 23-carbon polyketide chains forming 1,11-dioxo-2,6,10-trioxaanthracene and 4,8-dioxo-1,9,13-trioxaanthracene derivatives, representing ring systems not previously found in nature. This study highlights the utility of 2D NMR-spectroscopic screening for exploring nature's structure space and suggests that insect metabolomes remain vastly underexplored.

  1. NMR, MRI, and spectroscopic MRI in inhomogeneous fields

    Science.gov (United States)

    Demas, Vasiliki; Pines, Alexander; Martin, Rachel W; Franck, John; Reimer, Jeffrey A

    2013-12-24

    A method for locally creating effectively homogeneous or "clean" magnetic field gradients (of high uniformity) for imaging (with NMR, MRI, or spectroscopic MRI) both in in-situ and ex-situ systems with high degrees of inhomogeneous field strength. THe method of imaging comprises: a) providing a functional approximation of an inhomogeneous static magnetic field strength B.sub.0({right arrow over (r)}) at a spatial position {right arrow over (r)}; b) providing a temporal functional approximation of {right arrow over (G)}.sub.shim(t) with i basis functions and j variables for each basis function, resulting in v.sub.ij variables; c) providing a measured value .OMEGA., which is an temporally accumulated dephasing due to the inhomogeneities of B.sub.0({right arrow over(r)}); and d) minimizing a difference in the local dephasing angle .phi.({right arrow over (r)},t)=.gamma..intg..sub.0.sup.t{square root over (|{right arrow over (B)}.sub.1({right arrow over (r)},t')|.sup.2+({right arrow over (r)}{right arrow over (G)}.sub.shimG.sub.shim(t')+.parallel.{right arrow over (B)}.sub.0({right arrow over (r)}).parallel..DELTA..omega.({right arrow over (r)},t'/.gamma/).sup.2)}dt'-.OMEGA. by varying the v.sub.ij variables to form a set of minimized v.sub.ij variables. The method requires calibration of the static fields prior to minimization, but may thereafter be implemented without such calibration, may be used in open or closed systems, and potentially portable systems.

  2. /sup 7/Li production in Nova explosions

    Energy Technology Data Exchange (ETDEWEB)

    Starrfield, S.; Truran, J.W.; Sparks, W.M.; Arnould, M.

    1978-06-01

    Calculations of /sup 7/Li production occurring as a concomitant of thermonuclear runaways in hydrogen envelopes of white dwarfs are reported. It is found that sufficient /sup 7/Li can be produced in models displaying fast--nova-like features to suggest that the corresponding objects represent significant contributors to the /sup 7/Li enrichment of galactic matter. The sensitivities of these results to various assumptions and uncertainties are discussed.

  3. Complexation of roxatidine acetate hydrochloride with beta-cyclodextrin: NMR spectroscopic study.

    Science.gov (United States)

    Ali, S M; Maheshwari, A; Asmat, F

    2004-08-01

    A NMR spectroscopic study of mixtures of varying ratios of roxatidine acetate hydrochloride (RAH) and beta-cyclodextrin (beta-CD) in D2O revealed the formation of a 1:1 inclusion compound. The aromatic ring of RAH selectively penetrates the beta-CD cavity in preference to the piperidine ring.

  4. Spectroscopic correlation analysis of NMR-based metabonomics in exercise science.

    Science.gov (United States)

    Kirwan, Gemma M; Coffey, Vernon G; Niere, Julie O; Hawley, John A; Adams, Michael J

    2009-10-12

    Spectroscopic studies of complex clinical fluids have led to the application of a more holistic approach to their chemical analysis becoming more popular and widely employed. The efficient and effective interpretation of multidimensional spectroscopic data relies on many chemometric techniques and one such group of tools is represented by so-called correlation analysis methods. Typical of these techniques are two-dimensional correlation analysis and statistical total correlation spectroscopy (STOCSY). Whilst the former has largely been applied to optical spectroscopic analysis, STOCSY was developed and has been applied almost exclusively to NMR metabonomic studies. Using a (1)H NMR study of human blood plasma, from subjects recovering from exhaustive exercise trials, the basic concepts and applications of these techniques are examined. Typical information from their application to NMR-based metabonomics is presented and their value in aiding interpretation of NMR data obtained from biological systems is illustrated. Major energy metabolites are identified in the NMR spectra and the dynamics of their appearance and removal from plasma during exercise recovery are illustrated and discussed. The complementary nature of two-dimensional correlation analysis and statistical total correlation spectroscopy are highlighted.

  5. NMR spectroscopic study on methanolysis reaction of vegetable oil

    Energy Technology Data Exchange (ETDEWEB)

    Fangming Jin; Kohei Kawasaki; Hisanori Kishida; Kazuyuki Tohji; Takehoko Moriya; Heiji Enomoto [Tohoku University, Sendai (Japan). Graduate School of Environmental Studies

    2007-05-15

    This study is to clarify the pathways of the transesterification of vegetable oil by applying NMR to the identification of intermediates in the transesterification reaction. Results showed that the significant methanolysis product was sn-1,3-diglycerides in diglycerides, and sn-2-monoglycerides was not found. These analytical results suggest that the methanolysis reaction may occur easily at the sn-2-position for both sn-tri- and sn-1,2-diglycerides. Short communication. 16 refs., 6 figs., 2 tabs.

  6. Study of the poly-aniline complexed with Li Cl O{sub 4} by Lithium-7 NMR; Estudo da polianilina complexada com Li Cl O{sub 4} por RMN do {sup 7} Li

    Energy Technology Data Exchange (ETDEWEB)

    Giotto, M.V.; Bonagamba, T.J.; Panepucci, H. [Sao Paulo Univ., Sao Carlos, SP (Brazil). Inst. de Fisica e Quimica; Mattoso, L.H.C.; Valenciano, G.R. [EMBRAPA, Sao Carlos, SP (Brazil). CNPDIA

    1997-12-31

    This work presents the chemical structure study of poly-aniline. The chemical preparation of the samples is presented. Also studied are the electric conductivity of the complexes of poly-aniline with Lithium. The samples were analysed by NMR. The spectra are presented 3 refs., 11 figs., 3 tabs.

  7. Substitution of lithium for magnesium, zinc, and aluminum in Li{sub 15}Si{sub 4}: crystal structures, thermodynamic properties, as well as {sup 6}Li and {sup 7}Li NMR spectroscopy of Li{sub 15}Si{sub 4} and Li{sub 15-x}M{sub x}Si{sub 4} (M=Mg, Zn, and Al)

    Energy Technology Data Exchange (ETDEWEB)

    Baran, Volodymyr; Faessler, Thomas F. [Department Chemie, Technische Universitaet Muenchen, Garching (Germany); Wuellen, Leo van [Department of Physics, University of Augsburg (Germany)

    2016-05-04

    An investigation into the substitution effects in Li{sub 15}Si{sub 4}, which is discussed as metastable phase that forms during electrochemical charging and discharging cycles in silicon anode materials, is presented. The novel partial substitution of lithium by magnesium and zinc is reported and the results are compared to those obtained for aluminum substitution. The new lithium silicides Li{sub 14}MgSi{sub 4} (1) and Li{sub 14.05}Zn{sub 0.95}Si{sub 4} (2) were synthesized by high-temperature reactions and their crystal structures were determined from single-crystal data. The magnetic properties and thermodynamic stabilities were investigated and compared with those of Li{sub 14.25}Al{sub 0.75}Si{sub 4} (3). The substitution of a small amount of Li in metastable Li{sub 15}Si{sub 4} for more electron-rich metals, such as Mg, Zn, or Al, leads to a vast increase in the thermodynamic stability of the resulting ternary compounds{sub .} The {sup 6,7}Li NMR chemical shift and spin relaxation time T{sub 1}-NMR spectroscopy behavior at low temperatures indicate an increasing contribution of the conduction electrons to these NMR spectroscopy parameters in the series for 1-3. However, the increasing thermal stability of the new ternary phases is accompanied by a decrease in Li diffusivity, with 2 exhibiting the lowest activation energy for Li mobility with values of 56, 60, and 62 kJ mol{sup -1} for 2, Li{sub 14.25}Al{sub 0.75}Si{sub 14}, and 1, respectively. The influence of the metastable property of Li{sub 15}Si{sub 4} on NMR spectroscopy experiments is highlighted. (copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. Lattice dynamics in Bosonic 7 Li

    Science.gov (United States)

    Chen, Huiyao Y.; Jung, Minwoo; Rabinowitz, Jacob; Madjarov, Ivaylo S.; Cheung, Hil F. H.; Patil, Yogesh Sharad; Vengalattore, Mukund

    2016-05-01

    The light mass and strong spin-dependent interactions in 7 Li make it an attractive candidate to study Bosonic quantum magnetism and lattice dynamics in regimes where rapid dynamics is favored, e.g. percolative transport and entropy segregation. Such studies require large ensembles of quantum degenerate 7 Li atoms which has proved to be a technical challenge. We describe our ongoing efforts to overcome this challenge using Raman sideband cooling (RSC). In addition to enabling the rapid production of large degenerate gases, RSC is also a very powerful means of local control of lattice gas dynamics. Extending this to a spinful 7 Li Bose gas will also enable studies of transport and defect dynamics in F=1 lattice gases. This work is supported by the ARO MURI on non-equilibrium dynamics.

  9. Single-Crystal Time-of-Flight Neutron Diffraction and Magic-Angle-Spinning NMR Spectroscopy Resolve the Structure and (1)H and (7)Li Dynamics of the Uranyl Peroxide Nanocluster U60.

    Science.gov (United States)

    Olds, Travis A; Dembowski, Mateusz; Wang, Xiaoping; Hoffman, Christina; Alam, Todd M; Hickam, Sarah; Pellegrini, Kristi L; He, Junhong; Burns, Peter C

    2017-08-21

    Single-crystal time-of-flight neutron diffraction has provided atomic resolution of H atoms of H2O molecules and hydroxyl groups, as well as Li cations in the uranyl peroxide nanocluster U60. Solid-state magic-angle-spinning nuclear magnetic resonance (MAS NMR) spectroscopy was used to confirm the dynamics of these constituents, revealing the transportation of Li atoms and H2O through cluster walls. H atoms of hydroxyl units that are located on the cluster surface are involved in the transfer of H2O and Li cations from inside to outside and vice versa. This exchange occurs as a concerted motion and happens rapidly even in the solid state. As a consequence of its large size and open hexagonal pores, U60 exchanges Li cations more rapidly compared to other uranyl nanoclusters.

  10. Magnetic structure of low-dimensional LiCu{sub 2}O{sub 2} multiferroic according to {sup 63,65}Cu and {sup 7}Li NMR studies

    Energy Technology Data Exchange (ETDEWEB)

    Sadykov, A. F., E-mail: sadykov@imp.uran.ru; Gerashchenko, A. P.; Piskunov, Yu. V.; Ogloblichev, V. V.; Smol' nikov, A. G.; Verkhovskii, S. V. [Russian Academy of Sciences, Institute of Metal Physics, Ural Division (Russian Federation); Yakubovskii, A. Yu. [National Research Centre Kurchatov Institute (Russian Federation); Tishchenko, E. A. [Russian Academy of Sciences, Kapitza Institute for Physical Problems (Russian Federation); Bush, A. A. [Moscow State Technical University of Radio Engineering, Electronics, and Automation (Russian Federation)

    2012-10-15

    The complex NMR study of the magnetic structure of LiCu{sub 2}O{sub 2} multiferroic has been performed. It has been shown that the spin spirals in LiCu{sub 2}O{sub 2} are beyond the ab, bc, and ac crystallographic planes. The external magnetic field applied along the c axis of the crystal does not change the spatial orientation of spirals in Cu{sup 2+} chains. A magnetic field of H{sub 0} = 94 kOe applied along the a and b axes rotates the planes of spin spirals in chains, tending to orient the normal n of spirals along the external magnetic field. The rotation angle of the planes of the magnetic moments are maximal at H{sub 0} Double-Vertical-Line b.

  11. Perturbed Angular Correlation (PAC)/NMR spectroscopic properties and dynamics of compounds containing metal ions

    DEFF Research Database (Denmark)

    Arcisauskaité, Vaida

    steps towards understanding how Zn(II) reaches its target position in biological systems in vivo and in vitro experiments in aqueous solution, is the detailed investigation of water exchange reactions for Zn(II)(aq). A very advanced (albeit not complete) picture of structure and dynamics of solvated Zn......199mHg PAC and 199Hg NMR spectroscopic properties, nuclear quadrupole coupling constants, Q, asymmetry parameters, , and chemical shifts, , respectively, are the fingerprint of the local molecular and electronic structure, at the probed Hg nuclei. For this reason, these spectroscopic techniques...... compounds in terms of the atomic constituents. The analysis provided a chemophysical interpretation of changes in Vzz upon structural distortions and ligand exchange. The gained insights can be useful when predicting and understanding changes in Q values for Hg binding sites in proteins. One of the first...

  12. {sup 1}H NMR spectroscopic studies establish that heparanase is a retaining glycosidase

    Energy Technology Data Exchange (ETDEWEB)

    Wilson, Jennifer C., E-mail: jennifer.wilson@griffith.edu.au [Institute for Glycomics, Griffith University Gold Coast Campus, QLD 4222 (Australia); Laloo, Andrew Elohim [School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, QLD 4072 (Australia); Singh, Sanjesh [Institute for Glycomics, Griffith University Gold Coast Campus, QLD 4222 (Australia); Ferro, Vito, E-mail: v.ferro@uq.edu.au [School of Chemistry and Molecular Biosciences, The University of Queensland, Brisbane, QLD 4072 (Australia)

    2014-01-03

    Highlights: •{sup 1}H and {sup 13}C NMR chemical shifts of fondaparinux were fully assigned by 1D and 2D NMR techniques. •Hydrolysis of fondaparinux by heparanase was monitored by {sup 1}H NMR spectroscopy. •Heparanase is established to be a retaining glycosidase. -- Abstract: Heparanase is an endo-β-glucuronidase that cleaves heparan sulfate side chains of proteoglycans in basement membranes and the extracellular matrix (ECM). Heparanase is implicated in several diverse pathological processes associated with ECM degradation such as metastasis, inflammation and angiogenesis and is thus an important target for anti-cancer and anti-inflammatory drug discovery. Heparanase has been classed as belonging to the clan A glycoside hydrolase family 79 based on sequence analysis, secondary structure predictions and mutagenic analysis, and thus it has been inferred that it is a retaining glycosidase. However, there has been no direct experimental evidence to support this conclusion. Herein we describe {sup 1}H NMR spectroscopic studies of the hydrolysis of the pentasaccharide substrate fondaparinux by heparanase, and provide conclusive evidence that heparanase hydrolyses its substrate with retention of configuration and is thus established as a retaining glycosidase. Knowledge of the mechanism of hydrolysis may have implications for future design of inhibitors for this important drug target.

  13. Reaction mechanism study of 7Li(7Li, 6He) reaction at above Coulomb barrier energies

    Indian Academy of Sciences (India)

    V V Parkar; V Jha; S Santra; B J Roy; K Ramachandran; A Shrivastava; K Mahata; A Chatterjee; S Kailas

    2009-02-01

    The elastic scattering and the 6He angular distributions were measured in 7Li + 7Li reaction at two energies, lab = 20 and 25 MeV. FRDWBA calculations have been performed to explain the measured 6He data. The calculations were very sensitive to the choice of the optical model potentials in entrance and exit channels. The one-step proton transfer was found to be the dominant reaction mechanism in 6He production.

  14. {sup 13}C NMR and EPR spectroscopic evaluation of oil shale mined soil recuperation

    Energy Technology Data Exchange (ETDEWEB)

    Santos, J.V. dos, E-mail: mangrich@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil); Mangrich, A.S. [Instituto Nacional de Ciencia e Tecnologia: Energia e Ambiente, Salvador, BA (Brazil); Pereira, B.F. [EMBRAPA Clima Temperado, Pelotas, RS (Brazil); Pillon, C.N. [EMBRAPA Clima Temperado, Pelotas, RS (Brazil). Estacao Experimental Cascata; Novotny, E.H. [EMBRAPA Solos, Rio de Janeiro, RJ (Brazil); Bonagamba, T.J. [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Instituto de Fisica; Abbt-Braun, G.; Frimmel, F.H. [Engler-Bunte-Institut, Universitaet Karlsruhe, TH (Germany)

    2013-02-15

    In this work, native forest soil (NFS) organic matter (SOM) sample and SOM samples from a neighboring forest soil area of an oil shale mine which is being rehabilitated for thirty years (RFS) were analyzed. X-band electron paramagnetic resonance (EPR) and solid-state {sup 13}C nuclear magnetic resonance (NMR) spectroscopies were used to evaluate the soil reclamation of the Brazilian oil shale mining process. Two-dimensional heterospectral correlation studies of the results obtained from EPRand {sup 13}C NMR were used to obtain information about SOM structures and their interactions with residual paramagnetic metal ion. The signal of the residual metallic oxycation, VO{sup 2+} correlated positively with uronic acid-type hydrophilic organic structures, determined from the {sup 13}C NMR spectra, and correlated negatively with the organic free radical (OFR) signal associated with oxygen atoms (g = 2.0042). The hydrophobic aromatic structures correlate positively with the EPR OFR signal associated with carbon atoms (g = 2.0022). The data from the two spectroscopic magnetic techniques show that the used recuperation process is effective. (author)

  15. Structural Modifications of Deoxycholic Acid to Obtain Three Known Brassinosteroid Analogues and Full NMR Spectroscopic Characterization.

    Science.gov (United States)

    Herrera, Heidy; Carvajal, Rodrigo; Olea, Andrés F; Espinoza, Luis

    2016-08-27

    An improved synthesis route for obtaining known brassinosteroid analogues, i.e., methyl 2α,3α-dihydroxy-6-oxo-5α-cholan-24-oate (11), methyl 3α-hydroxy-6-oxo-7-oxa-5α-cholan-24-oate (15) and methyl 3α-hydroxy-6-oxa-7-oxo-5α-cholan-24-oate (16), from hyodeoxycholic acid (4) maintaining the native side chain is described. In the alternative procedure, the di-oxidized product 6, obtained in the oxidation of methyl hyodeoxycholate 5, was converted almost quantitatively into the target monoketone 7 by stereoselective reduction with NaBH₄, increasing the overall yield of this synthetic route to 96.8%. The complete ¹H- and (13)C-NMR assignments for all compounds synthesized in this work have been made by 1D and 2D heteronuclear correlation gs-HSQC and gs-HMBC techniques. Thus, it was possible to update the spectroscopic information of ¹H-NMR and to accomplish a complete assignment of all (13)C-NMR signals for analogues 5-16, which were previously reported only in partial form.

  16. UV-visible and (1)H-(15)N NMR spectroscopic studies of colorimetric thiosemicarbazide anion sensors.

    Science.gov (United States)

    Farrugia, Kristina N; Makuc, Damjan; Podborska, Agnieszka; Szaciłowski, Konrad; Plavec, Janez; Magri, David C

    2015-02-14

    Four model thiosemicarbazide anion chemosensors containing three N-H bonds, substituted with phenyl and/or 4-nitrophenyl units, were synthesised and studied for their anion binding abilities with hydroxide, fluoride, acetate, dihydrogen phosphate and chloride. The anion binding properties were studied in DMSO and 9 : 1 DMSO-H2O by UV-visible absorption and (1)H/(13)C/(15)N NMR spectroscopic techniques and corroborated with DFT studies. Significant changes were observed in the UV-visible absorption spectra with all anions, except for chloride, accompanied by dramatic colour changes visible to the naked eye. These changes were determined to be due to the deprotonation of the central N-H proton and not due to hydrogen bonding based on (1)H/(15)N NMR titration studies with acetate in DMSO-d6-0.5% water. Direct evidence for deprotonation was confirmed by the disappearance of the central thiourea proton and the formation of acetic acid. DFT and charge distribution calculations suggest that for all four compounds the central N-H proton is the most acidic. Hence, the anion chemosensors operate by a deprotonation mechanism of the central N-H proton rather than by hydrogen bonding as is often reported.

  17. NMR spectroscopic and analytical ultracentrifuge analysis of membrane protein detergent complexes

    Directory of Open Access Journals (Sweden)

    Choe Senyon

    2007-11-01

    Full Text Available Abstract Background Structural studies of integral membrane proteins (IMPs are hampered by inherent difficulties in their heterologous expression and in the purification of solubilized protein-detergent complexes (PDCs. The choice and concentrations of detergents used in an IMP preparation play a critical role in protein homogeneity and are thus important for successful crystallization. Results Seeking an effective and standardized means applicable to genomic approaches for the characterization of PDCs, we chose 1D-NMR spectroscopic analysis to monitor the detergent content throughout their purification: protein extraction, detergent exchange, and sample concentration. We demonstrate that a single NMR measurement combined with a SDS-PAGE of a detergent extracted sample provides a useful gauge of the detergent's extraction potential for a given protein. Furthermore, careful monitoring of the detergent content during the process of IMP production allows for a high level of reproducibility. We also show that in many cases a simple sedimentation velocity measurement provides sufficient data to estimate both the oligomeric state and the detergent-to-protein ratio in PDCs, as well as to evaluate the homogeneity of the samples prior to crystallization screening. Conclusion The techniques presented here facilitate the screening and selection of the extraction detergent, as well as help to maintain reproducibility in the detergent exchange and PDC concentration procedures. Such reproducibility is particularly important for the optimization of initial crystallization conditions, for which multiple purifications are routinely required.

  18. GC-FID and NMR Spectroscopic Studies on Gamma Irradiated Walnut Lipids

    Directory of Open Access Journals (Sweden)

    Vassilia J. Sinanoglou

    2015-01-01

    Full Text Available Walnuts have an excellent fatty acid profile, beneficial for coronary heart diseases. A diet rich in walnuts has shown to decrease the total and LDL cholesterol levels as well as lipoprotein levels. In this study, the effects of different doses of γ-irradiation and different packaging conditions on proximate composition and fatty acid profile of walnuts (Juglans regia L. were investigated merging data from different spectroscopic techniques. Walnuts moisture, ash, fat, and protein content as well as fatty acid profile were evaluated immediately after irradiation. GC-FID results showed that SFA increased and MUFA and PUFA decreased with the increase of irradiation dose. Moreover, MUFA/SFA and PUFA/SFA ratios decreased P<0.05 compared to control samples. Furthermore, NMR spectroscopy was implemented to examine possible discrimination patterns based on irradiation dose and packaging. This approach revealed the role of PUFA decrease with the parallel increase of irradiation dose while indicating the protective role of vacuum and MAP compared to air packaging. In conclusion, at irradiation doses of up to 5 kGy, the walnuts retained the nutritional benefits of its fatty acids, in particular MUFA and PUFA. Concerning the different types of packaging, greater stability in the nuts was observed using MAP packaging.

  19. NMR spectroscopic search module for Spektraris, an online resource for plant natural product identification--Taxane diterpenoids from Taxus × media cell suspension cultures as a case study.

    Science.gov (United States)

    Fischedick, Justin T; Johnson, Sean R; Ketchum, Raymond E B; Croteau, Rodney B; Lange, B Markus

    2015-05-01

    Development and testing of Spektraris-NMR, an online spectral resource, is reported for the NMR-based structural identification of plant natural products (PNPs). Spektraris-NMR allows users to search with multiple spectra at once and returns a table with a list of hits arranged according to the goodness of fit between query data and database entries. For each hit, a link to a tabulated alignment of (1)H NMR and (13)C NMR spectroscopic peaks (query versus database entry) is provided. Furthermore, full spectroscopic records and experimental meta information about each database entry can be accessed online. To test the utility of Spektraris-NMR for PNP identification, the database was populated with NMR data (total of 466 spectra) for ∼ 250 taxanes, which are structurally complex diterpenoids (including the anticancer drug taxol) commonly found in the genus Taxus. NMR data generated with metabolites purified from Taxus cell suspension cultures were then used to search Spektraris-NMR, and enabled the identification of eight taxanes with high confidence. A ninth isolated metabolite could be assigned, based on spectral searches, to a taxane skeletal class, but no high confidence hit was produced. Using various spectroscopic methods, this metabolite was characterized as 2-deacetylbaccatin IV, a novel taxane. These results indicate that Spektraris-NMR is a valuable resource for rapid and reliable identification of known metabolites and has the potential to contribute to de-replication efforts in novel PNP discovery.

  20. {sup 6}Li({sup 18}O, {sup 17}O){sup 7}Li reaction and comparison of {sup 6, 7}Li + {sup 16, 17, 18}O potentials

    Energy Technology Data Exchange (ETDEWEB)

    Rudchik, A.T., E-mail: rudchik@kinr.kiev.ua [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Chercas, K.A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kemper, K.W. [Physics Department, Florida State University, Tallahassee, FL 32306-4350 (United States); Rudchik, A.A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kliczewski, S. [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Koshchy, E.I. [Kharkiv National University, pl. Svobody 4, 61077 Kharkiv (Ukraine); Rusek, K. [National Center for Nuclear Reseaches, ul. Hoża 69, PL-00-681 Warsaw (Poland); Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Mezhevych, S.Yu.; Ponkratenko, O.A.; Pirnak, Val.M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Plujko, V.A. [Taras Shevchenko National University, ul. Volodymyrska 64, 01033 Kyiv (Ukraine); Choiński, J. [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Czech, B.; Siudak, R.; Szczurek, A. [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland)

    2014-07-15

    Angular distributions of the {sup 6}Li({sup 18}O, {sup 17}O){sup 7}Li reaction were measured at E{sub lab}({sup 18}O)=114 MeV for ground and excited states of the exit channel nuclei for the first time. The data were analyzed within the coupled-reaction-channels method (CRC). The {sup 6}Li + {sup 18}O elastic and inelastic scattering channels as well as simplest one- and two-step reactions were included in the coupled-reaction-channels scheme. The {sup 7}Li + {sup 17}O potential was deduced by fitting CRC calculations to the reaction data. The spectroscopic amplitudes for single nucleon and nuclear cluster configurations were calculated within the translationally invariant shell model. Isotopic differences of the {sup 7}Li + {sup 16, 17, 18}O and {sup 7, 8}Li + {sup 17}O potentials and the reaction mechanisms were studied.

  1. Fusion around the barrier for 7Li + 12C

    Indian Academy of Sciences (India)

    A Mukherjee; M Dasgupta; D J Hinde; C R Morton; A C Berriman; R D Butt; J O Newton; H Timmers

    2001-07-01

    Fusion cross-sections for the 7Li + 12C reaction have been measured at energies above the Coulomb barrier by the direct detection of evaporation residues. The heavy evaporation residues with energies below 3 MeV could not be separated out from the -particles in the spectrum and hence their contribution was estimated using statistical model calculations. The present work indicates that suppression of fusion cross-sections due to the breakup of 7Li may not be significant for 7Li + 12C reaction at energies around the barrier.

  2. Spectroscopic approaches to resolving ambiguities of hyper-polarized NMR signals from different reaction cascades

    DEFF Research Database (Denmark)

    Jensen, Pernille Rose; Meier, Sebastian

    2016-01-01

    The influx of exogenous substrates into cellular reaction cascades on the seconds time scale is directly observable by NMR spectroscopy when using nuclear spin polarization enhancement. Conventional NMR assignment spectra for the identification of reaction intermediates are not applicable in thes...

  3. Purification and H-1 NMR spectroscopic characterization of phase II metabolites of tolfenamic acid

    DEFF Research Database (Denmark)

    Sidelmann, U. G.; Christiansen, E.; Krogh, L.;

    1997-01-01

    acid; the study shows the applicability of H-1 NMR for the identification of drug metabolites in biological fluids. In addition to NMR analysis, two metabolites were also identified by mass spectrometry (MS), The glucuronides of the following parent compounds, N-(2-methyl-3-chlorophenyl...

  4. Application of phosphorus-31 and aluminum-27 NMR spectroscopic techniques to study aqueous and methanolic solutions of tetraphenylammonium aluminophosphate

    Science.gov (United States)

    Goudarzi, Nasser; Amin, Amir H.

    2017-01-01

    In this work, aluminum-27 and phosphorus-31 NMR spectroscopic techniques were used to investigate and characterize the distribution of aluminophosphate (AlPO) species soluble in the aqueous and methanolic solutions of tetraphenylammonium (TPhA) chloride. The reaction between hexaaquaaluminum cations, [A1(H2O)6]3+, and different phosphate ligands such as H3PO4, H2PO4-, and the acidic dimers H6P2O8 and H5P2O8- resulted in the formation of the soluble AlPO cations. The effective aluminum-27 and phosphorous-31 NMR spectroscopies can be employed to characterize the species present in a solution. Assignment of the peaks present in the aluminum-27 NMR spectra to the aluminate species or aluminate connectivities was done to acquire information about different AlPO complexes. Some resonance lines were observed in the phosphorus-31 {1H} NMR spectra, indicating the existence of different complexes in the AlPO solutions. Some peaks were observed in the methanolic solutions of AlPO at the chemical shifts of -0.41, -6.4, -7.5, -7.9, -13.1, -13.9, -16.6, -18.1, and -20.6 ppm. Four additional peaks were also observed in the phosphorus-31 {1H} NMR spectra of the methanolic solutions of AlPO, whose intensities changed with changes in the methanol:water volume ratio; they were observed in methanol but not in aqueous AlPO.

  5. Solid-state NMR spectroscopic trends for supramolecular assemblies and protein aggregates.

    Science.gov (United States)

    Linser, Rasmus

    2017-08-24

    Solid-state NMR is able to generate structural data on sample preparations that are explicitly non-crystalline. In particular, for amyloid fibril samples, which can comprise significant degrees of sample disorder, solid-state NMR has been used very successfully. But also solid-state NMR studies of other supramolecular assemblies that have resisted assessment by more standard methods are being performed with increasing ease and biological impact, many of which are briefly reviewed here. New technical trends with respect to structure calculation, protein dynamics and smaller sample amounts have reshaped the field of solid-state NMR recently. In particular, proton-detected approaches based on fast Magic-Angle Spinning (MAS) were demonstrated for crystalline systems initially. Currently, such approaches are being expanded to the above-mentioned non-crystalline targets, the characterization of which can now be pursued with sample amounts on the order of a milligram. In this Trends article, I am giving a brief overview about achievements of the last years as well as the directions that the field has been heading into and delineate some satisfactory perspectives for solid-state NMR's future striving. Copyright © 2017 Elsevier Inc. All rights reserved.

  6. A novel Bayesian approach to quantify clinical variables and to determine their spectroscopic counterparts in 1H NMR metabonomic data

    Directory of Open Access Journals (Sweden)

    Kaski Kimmo

    2007-05-01

    Full Text Available Abstract Background A key challenge in metabonomics is to uncover quantitative associations between multidimensional spectroscopic data and biochemical measures used for disease risk assessment and diagnostics. Here we focus on clinically relevant estimation of lipoprotein lipids by 1H NMR spectroscopy of serum. Results A Bayesian methodology, with a biochemical motivation, is presented for a real 1H NMR metabonomics data set of 75 serum samples. Lipoprotein lipid concentrations were independently obtained for these samples via ultracentrifugation and specific biochemical assays. The Bayesian models were constructed by Markov chain Monte Carlo (MCMC and they showed remarkably good quantitative performance, the predictive R-values being 0.985 for the very low density lipoprotein triglycerides (VLDL-TG, 0.787 for the intermediate, 0.943 for the low, and 0.933 for the high density lipoprotein cholesterol (IDL-C, LDL-C and HDL-C, respectively. The modelling produced a kernel-based reformulation of the data, the parameters of which coincided with the well-known biochemical characteristics of the 1H NMR spectra; particularly for VLDL-TG and HDL-C the Bayesian methodology was able to clearly identify the most characteristic resonances within the heavily overlapping information in the spectra. For IDL-C and LDL-C the resulting model kernels were more complex than those for VLDL-TG and HDL-C, probably reflecting the severe overlap of the IDL and LDL resonances in the 1H NMR spectra. Conclusion The systematic use of Bayesian MCMC analysis is computationally demanding. Nevertheless, the combination of high-quality quantification and the biochemical rationale of the resulting models is expected to be useful in the field of metabonomics.

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

    Science.gov (United States)

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

    2007-04-01

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

  8. {sup 11}B-NMR spectroscopic study on the interaction of epinephrine and p-BPA

    Energy Technology Data Exchange (ETDEWEB)

    Ichihara, K.; Yoshino, K. [Shinshu Univ., Department of Chemistry, Matsumoto, Nagano (Japan)

    2000-10-01

    It is studied that p-BPA (p-bronophenylalanine) which formed complex with catechol functional group has interaction with epinephrine by {sup 11}B-NMR. Two {sup 11}B-NMR resonance signals were observed at pH 7.0. The signal at 29.6 ppm is assigned to p-BPA and at 10.8 ppm is assigned to that of complex. We can determine complex formation constants (logK') in various pH. (author)

  9. THE P-31-NMR SPECTROSCOPIC DETERMINATION OF THE ENANTIOMERIC EXCESS OF UNPROTECTED AMINO-ACIDS

    NARCIS (Netherlands)

    HULST, R; DEVRIES, NK; FERINGA, BL

    1992-01-01

    No separation is needed! The enantiomeric excess of unprotected amino acids can be determined very reliable by P-31 NMR spectroscopy after derivatization as phosphonic amides 1. This rapid and simple analytical procedure, suitable for aqueous solutions. is also applicable for amino acid derivatives,

  10. Sol-gel chemistry synthesis and DTA-TGA, XRPD, SIC and {sup 7}Li, {sup 31}P, {sup 29}Si MAS-NMR studies on the Li-NASICON Li{sub 3}Zr{sub 2-y}Si{sub 2-4y}P{sub 1+4y}O{sub 12} (0 Less-Than-Or-Slanted-Equal-To y Less-Than-Or-Slanted-Equal-To 0.5) system

    Energy Technology Data Exchange (ETDEWEB)

    Belam, W., E-mail: WahidBelam@yahoo.fr [Chemistry Department, Bizerta Science Faculty, 7021 Jarzouna, Bizerta (Tunisia)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer The samples of Li-NASICON were elaborated by sol-gel chemistry. Black-Right-Pointing-Pointer The calcined temperatures of the studied samples were deduced from their thermograms. Black-Right-Pointing-Pointer The recorded X-ray powder diffractograms were indexed in the rhombohedral system. Black-Right-Pointing-Pointer The synthesized Li-NASICON materials are excellent lithium fast cation conductors. - Abstract: Five selected compounds of Li-NASICON, Li{sub 3}Zr{sub 2-y}Si{sub 2-4y}P{sub 1+4y}O{sub 12} (0 Less-Than-Or-Slanted-Equal-To y Less-Than-Or-Slanted-Equal-To 0.5), were synthesized by sol-gel chemistry in order to obtain pure polycrystalline powder and then analyzed by different physicochemical characterizations such as coupled DTA (differential thermal analysis)-TGA (thermogravimetric analysis), XRPD (X-ray powder diffraction), CIS (complex impedance spectroscopy) and MAS (magic angle spinning)-NMR (nuclear magnetic resonance). So the calcined temperature of each sample has been deduced from its corresponding DTA-TGA thermogram. However, the recorded X-ray powder diffractograms were indexed in the rhombohedral system with R3{sup Macron }c space group which corresponds to the ideal structure of NASICON. Whereas, the complex impedance spectroscopy study showed that these Li-NASICON materials are excellent lithium fast cation conductors with total electric conductivity maximal value 1.97 Multiplication-Sign 10{sup -3} S cm{sup -1} at 293 K in the case of Li{sub 3}Zr{sub 1.5}P{sub 3}O{sub 12}. Furthermore, {sup 7}Li, {sup 31}P and {sup 29}Si MAS-NMR spectroscopy study and DFT/B3LYP theoretical calculations of chemical shifts were performed to discuss the ambiguousness that exists between the resonance peak number in the experimental spectrum and the crystallographic site number relative to Li{sub 3}Zr{sub 2}Si{sub 2}PO{sub 12}.

  11. UV/vis, 1H, and 13C NMR spectroscopic studies to determine mangiferin p Ka values

    Science.gov (United States)

    Gómez-Zaleta, Berenice; Ramírez-Silva, María Teresa; Gutiérrez, Atilano; González-Vergara, Enrique; Güizado-Rodríguez, Marisol; Rojas-Hernández, Alberto

    2006-07-01

    The acid constants of mangiferin (a natural xanthonoid) in aqueous solution were determined through an UV/vis spectroscopic study employing the SQUAD program as a computational tool. A NMR study complements the p Ka values assignment and evidences a H-bridge presence on 1-C. The chemical model used was consistent with the experimental data obtained. The p Ka values determined with this procedure were as follows: H 4(MGF) = H 3(MGF) - + H +, pK(6-H) = 6.52 ± 0.06; H 3(MGF) - = H 2(MGF) 2- + H +, pK(3-H) = 7.97 ± 0.06; H 2(MGF) 2- = H(MGF) 3- + H +, pK(7-H) = 9.44 ± 0.04; H(MGF) 3- = (MGF) 4- + H +, pK(1-H) = 12.10 ± 0.01; where it has been considered mangiferin C 19H 18O 11 as H 4(MGF). Mangiferin UV/vis spectral behavior, stability study in aqueous solution as well as NMR spectroscopy studies: one-dimensional 1H, 13C, 2D correlated 1H/ 13C performed by (g)-HSQC and (g)-HMBC methods; are also presented. p Ka values determination of H 4(MGF) in aqueous solution is a necessary contribution to subsequent pharmacokinetic study, and a step towards the understanding of its biological effects.

  12. Infrared and MAS NMR Spectroscopic Studies of Al18B4O33

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The IR spectrum and 11B and 27Al MAS NMR spectra of Al18B4O33 are presented and discussed in relation to the possible existence of boron atoms substituting for aluminum atoms. TheIR spectrum shows that the strong vibrations of the BO3 groups are present in the 1 500~1 200em-1 region, and very weak bands of BO4 units are present in the region from 1 000 to 1 100cm-1. 11B MAS NMR spectrum indicates that the strong signal for BO3 units appears in the region from δ +5 to δ +20, and the very weak signal for BO4 units is at about δ-1, while 27AlMAS NMR spectrum shows five peaks at about δ +62, +42. 1, +14,-4.7 and-6.4, originating from AlO4, AlO4, A1O5, AlO6 and AlO6, respectively. These results reveal that there areminor BO4 units in Al18B4O33, indicating that a small amount of B atoms substitute for Al atomsin the 4-fold coordination.

  13. NMR-spectroscopic characterization of phosphodiester bond cleavage catalyzed by the minimal hammerhead ribozyme.

    Science.gov (United States)

    Fürtig, Boris; Richter, Christian; Schell, Peter; Wenter, Philipp; Pitsch, Stefan; Schwalbe, Harald

    2008-01-01

    In order to relate the conformational dynamics of the hammerhead ribozyme to its biological function the cleavage reaction catalyzed by the hammerhead ribozyme was monitored by time-resolved nuclear magnetic resonance (NMR) spectroscopy. For this purpose, the two nucleosides around the scissile phosphodiester bond were selectively (13)C labelled in multi-step organic syntheses starting from uniformly (13)C-labelled glucose. The phosphoamidites were incorporated using phosphoamidite chemistry in the hammerhead substrate strand. In addition, the 2'-OH group on the 5'-side of the hammerhead substrate strand was labelled with a photolabile protecting group. This labelling strategy enabled a detailed characterisation of the nucleotides around the scissile phosphodiester bond in the ground state conformation of the hammerhead ribozyme in the absence and presence of Mg(2+) ions as well as of the product state. Photochemical induction of the reaction in situ was further characterized by time-resolved NMR spectroscopy. The detailed structural and dynamic investigations revealed that the conformation of the hammerhead ribozyme is significantly affected by addition of Mg(2+) leading to an ensemble of conformations where dynamic transitions between energetically similar conformations occur on the ms-timescale in the presence of Mg(2+). The dynamic transitions are localized around the catalytic core. Cleavage from this ensemble cannot be described by mono-exponential kinetics but follows bi-exponential kinetics. A model is described to take into account these experimental data.

  14. Evaluation of transformer insulating oil quality using NIR, fluorescence, and NMR spectroscopic data fusion.

    Science.gov (United States)

    Godinho, Mariana S; Blanco, Marcos R; Gambarra Neto, Francisco F; Lião, Luciano M; Sena, Marcelo M; Tauler, Romà; de Oliveira, Anselmo E

    2014-11-01

    Power transformers are essential components in electrical energy distribution. One of their most important parts is the insulation system, consisting of Kraft paper immersed in insulating oil. Interfacial tension and color are major parameters used for assessing oil quality and the system׳s degradation. This work proposes the use of near infrared (NIR), molecular fluorescence, and (1)H nuclear magnetic resonance (NMR) spectroscopy methods combined with chemometric multivariate calibration methods (Partial Least Squares - PLS) to predict interfacial tension and color in insulating mineral oil samples. Interfacial tension and color were also determined using tensiometry and colorimetry as standard reference methods, respectively. The best PLS model was obtained when NIR, fluorescence, and NMR data were combined (data fusion), demonstrating synergy among them. An optimal PLS model was calculated using the selected group of variables according to their importance on PLS projections (VIP). The root mean square errors of prediction (RMSEP) values of 2.9 mN m(-1) and 0.3 were estimated for interfacial tension and color, respectively. Mean relative standard deviations of 1.5% for interfacial tension and 6% for color were registered, meeting quality control requirements set by electrical energy companies. The methods proposed in this work are rapid and simple, showing great advantages over traditional approaches, which are slow and environmentally unfriendly due to chemical waste generation.

  15. Spectroscopic (vibrational, NMR and UV-vis.) and quantum chemical investigations on 4-hexyloxy-3-methoxybenzaldehyde

    Science.gov (United States)

    Abbas, Ashgar; Gökce, Halil; Bahçeli, Semiha

    2016-01-01

    In this study, the 4-hexyloxy-3-methoxybenzaldehyde compound as one of the derivatives of vanillin which is a well known flavoring agent, C14H20O3, has been investigated by experimentally and extensively utilizing density functional theory (DFT) at the B3LYP/6-311++G(d,p) level. In this context, the optimized geometry, vibrational frequencies, 1H and 13C NMR chemical shifts, UV-vis. (in gas phase and in methanol solvent) spectra, HOMO-LUMO analysis, molecular electrostatic potential (MEP), thermodynamic parameters and atomic charges of 4-hexyloxy-3-methoxybenzaldehyde have been calculated. In addition, theoretically predicted IR, Raman and UV-vis. (in gas phase and in methanol solvent) spectra of the mentioned molecule have been constructed. The results calculated were compared with the experimental data.

  16. NMR spectroscopic characterization of β-cyclodextrin inclusion complex with vanillin

    Science.gov (United States)

    Pîrnau, Adrian; Bogdan, Mircea; Floare, Calin G.

    2009-08-01

    The inclusion of vanillin by β-cyclodextrin was investigated by 1H NMR. The continuous variation technique was used to evidence the formation of soluble 1:1 complex in aqueous solution. The association constant of vanillin with β-cyclodextrin has been obtained at 298 K by fitting the experimental chemical shifts differences, Δδobs = δfree - δobs of the observed guest and host protons, with a non-linear regression method. Besides the effective association constant, the fitting procedure allows a precise determination of all chemical shift parameters characterizing the pure complex. They can by used for an analysis of the geometry of the molecular complex in solution.

  17. NMR spectroscopic characterization of {beta}-cyclodextrin inclusion complex with vanillin

    Energy Technology Data Exchange (ETDEWEB)

    Pirnau, Adrian; Bogdan, Mircea; Floare, Calin G, E-mail: adrian.pirnau@itim-cj.r [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania)

    2009-08-01

    The inclusion of vanillin by {beta}-cyclodextrin was investigated by {sup 1}H NMR. The continuous variation technique was used to evidence the formation of soluble 1:1 complex in aqueous solution. The association constant of vanillin with {beta}-cyclodextrin has been obtained at 298 K by fitting the experimental chemical shifts differences, {Delta}{delta}{sub obs} {delta}{sub free} - {delta}{sub obs} of the observed guest and host protons, with a non-linear regression method. Besides the effective association constant, the fitting procedure allows a precise determination of all chemical shift parameters characterizing the pure complex. They can by used for an analysis of the geometry of the molecular complex in solution.

  18. 15N NMR Spectroscopic Study on Nitrogen Formsin1mmHumic Substances of Soils

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Nitrogen forms of humic substances from a subalpine meadow soil, alateritic red soil and a weathered coal and the effect of acidhydrolysis on N structures of soil humic substances were studied byusing {15N cross-polarization magic angle spinning nuclearmagnetic resonance (CPMAS NMR) spectroscopy. Of the detectable15N-signal intensity in the spectra of soil humic substances71%79% may be attributed to amide groups, 10%18%to aromatic/aliphatic amines and 6%11% to indole- andpyrrole-like N. Whereas in the spectrum of the fulvic acid fromweathered coal 46%, at least, of the total 15N-signalintensity might be assigned to pyrrole-like N, 14% toaromatic/aliphatic amines, and the remaining intensities could not beassigned with certainty. Data on nonhydrolyzable residue ofprotein-sugar mixture and a 15N-labelled soil fulvic acidconfirm the formation of nonhydrolyzable heterocyclic N during acidhydrolysis.

  19. Spectroscopic (vibrational, NMR and UV-vis.) and quantum chemical investigations on 4-hexyloxy-3-methoxybenzaldehyde.

    Science.gov (United States)

    Abbas, Ashgar; Gökce, Halil; Bahçeli, Semiha

    2016-01-05

    In this study, the 4-hexyloxy-3-methoxybenzaldehyde compound as one of the derivatives of vanillin which is a well known flavoring agent, C14H20O3, has been investigated by experimentally and extensively utilizing density functional theory (DFT) at the B3LYP/6-311++G(d,p) level. In this context, the optimized geometry, vibrational frequencies, (1)H and (13)C NMR chemical shifts, UV-vis. (in gas phase and in methanol solvent) spectra, HOMO-LUMO analysis, molecular electrostatic potential (MEP), thermodynamic parameters and atomic charges of 4-hexyloxy-3-methoxybenzaldehyde have been calculated. In addition, theoretically predicted IR, Raman and UV-vis. (in gas phase and in methanol solvent) spectra of the mentioned molecule have been constructed. The results calculated were compared with the experimental data.

  20. 15N NMR Spectroscopic Study on Nitrogen Forms in Humic Substances of Soils

    Institute of Scientific and Technical Information of China (English)

    WENQIXAIO; ZHUOSUNENG; 等

    2001-01-01

    Nitrogen forms of humic substances from a subalpine meadow soil,a lateritic red soil and a weathered cola and the effect of acid hydrolysis on N structures of soil humic substances were studied by using 15N cross-polarization magic angle spinning nuclear magnetic resonance(CPMAS NMR) spectroscopy,Of the detectable 15N-signal intensity in the spectra of soil humic substances 71%-79% may be attributed to amide groups ,10%-18% to aromatic/aliphatic amines and 6%-11% to indole-and pyrrole-like N.Whereas in the spectrum of the fulvic acid from weathered coal 46%,at least,of the total 15N-signal intensity might be assigned to pyrrole-like N,14% to aromatic/aliphatic amines,and the reamining intensities could not be assigned with certainty,Data on nonhydrolyzable reside of protein-sugar mixture and a 15N-labelled soil fulvic acid confirm the formation of nonhydrolyzable heterocyclic N during acid hydrolysis.

  1. Computational Chemistry Meets Experiments for Explaining the Behavior of Bibenzyl: A Thermochemical and Spectroscopic (Infrared, Raman, and NMR) Investigation.

    Science.gov (United States)

    Latouche, Camille; Barone, Vincenzo

    2014-12-09

    The structure, conformational behavior, and spectroscopic parameters of bibenzyl have been investigated by a computational protocol including proper treatment of anharmonic and hindered rotor contributions. Conventional hybrid functionals overstabilize the anti conformer while low-order post-Hartree-Fock (MP2) approaches strongly favor the gauche conformer. However, inclusion of semiempirical dispersion effects in density functionals or coupled cluster post-Hartree-Fock models agree in forecasting the simultaneous presence of both conformers in the gas phase with a slightly larger stability (0.7 kcal·mol(-1)) of the gauche conformer. Addition of thermal and entropic effects finally leads to very close Gibbs free energies for both conformers and, thus, to a slight preference for the gauche form due to statistical factors (2 vs 1). The situation remains essentially the same in solution. On these grounds, perturbative vibrational computations including both electrical and mechanical anharmonicities lead to IR and Raman spectra in remarkable agreement with experiment. Full assignment of the IR spectra explains the presence of peaks from gauche or anti conformers. Comparison between computed and experimental Raman spectra confirms that both conformers are present in liquid phase, whereas the anti conformer seems to be preponderant in the solid state. Also computed NMR parameters are in good agreement with experiment.

  2. Investigation on Acute Biochemical Effects of Ce(NO3)3 on Liver and Kidney Tissues by MAS 1H NMR Spectroscopic-Based Metabonomic Approach

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    High resolution magic angle spinning (MAS)-1 H nuclear magnetic resonance (NMR) spectroscopic-based metabonomic approach was applied to the investigation on the acute biochemical effects of Ce(NO3)3. Male Wistar rats were liver and kidney tissues were analyzed using principal component analysis to extract toxicity information. The biochemical effects of Ce(NO3)3 were characterized by the increase of triglycerides and lactate and the decrease of glycogen in rat liver tissue, together with an elevation of the triglyceride level and a depletion of glycerophosphocholine and betaine in kidney tissues. The target lesions of Ce(NO3)3 on liver and kidney were found by MAS NMR-based metabonomic method. This study demonstrates that the combination of MAS 1H NMR and pattern recognition analysis can be an effective method for studies of biochemical effects of rare earths.

  3. Charge transfer in Li/CFx-silver vanadium oxide hybrid cathode batteries revealed by solid state 7Li and 19F nuclear magnetic resonance spectroscopy

    Science.gov (United States)

    Sideris, Paul J.; Yew, Rowena; Nieves, Ian; Chen, Kaimin; Jain, Gaurav; Schmidt, Craig L.; Greenbaum, Steve G.

    2014-05-01

    Solid state 7Li and 19F magic angle spinning nuclear magnetic resonance (MAS NMR) experiments are conducted on several cathodes containing CFx-Silver vanadium oxide (CFx-Ag2V4O11) hybrid cathodes discharged to 50% depth of discharge (DoD) and stored at their open-circuit voltage for a period of one and three months. Three carbonaceous sources for the CFx phase are investigated: petroleum coke-based, fibrous, and mixed fibrous. For each hybrid cathode, a measurable increase in the relative amount of lithium fluoride is observed after a three month resting period in both the 7Li and 19F NMR spectra. These changes are attributed to lithium ion migration from the silver vanadium oxide to the CFx phase during the resting period, and help clarify the mechanism behind high power handling capability of this cathode.

  4. Thin target sup 7 Li(p, p'gamma) sup 7 Li inelastic gamma-ray yield measurements

    CERN Document Server

    Aslam; McNeill, F E

    2002-01-01

    Thin target angular distributions of inelastic gamma-ray yields resulting from sup 7 Li(p, p'gamma) sup 7 Li interaction have been measured for incident proton energies between 1.0 and 1.8 MeV. McMaster 3 MV KN Van de Graaff accelerator facility primarily dedicated to in-vivo neutron activation measurements has been used to perform experiments using a thin lithium metal target and 7.62 cm x 7.62 cm, 12.7 cm x 12.7 cm NaI(Tl) scintillation detectors and HPGe detectors. The uncertainty in the relative yield determination is based on the statistics of the data, uncertainty in the 478 keV peak area determination due to other interfering reactions, and the uncertainty in the recording of the proton charge. The results for the angular distribution provide an evidence for anisotropic nature of the radiation as compared to the presumed isotropic nature. The total relative yield was determined from the angular distributions and then compared with the published total cross sections for the reaction. Thick target yields...

  5. Exploring contributions from incomplete fusion in $^{6,7}$Li+$^{209}$Bi and $^{6,7}$Li+$^{198}$Pt reactions

    CERN Document Server

    Parkar, V V; Kailas, S

    2016-01-01

    We use the breakup absorption model to simultaneously describe the measured cross-sections of the Complete fusion (CF), Incomplete fusion (ICF), and Total fusion (TF) in nuclear reactions induced by weakly bound nuclei $^{6,7}$Li on $^{209}$Bi and $^{198}$Pt targets. The absorption cross-sections are calculated using the Continuum Discretized Coupled Channels (CDCC) method with different choices of short range imaginary potentials to get the ICF, CF and TF cross-sections. It is observed that the cross-sections for deuteron-ICF/deuteron-capture are of similar magnitude as the $\\alpha$-ICF/$\\alpha$-capture, in case of $^{6}$Li projectile, while the cross-sections for triton-ICF/triton-capture is more dominant than $\\alpha$-ICF/$\\alpha$-capture in case of $^{7}$Li projectile. Both these observations are also corroborated by the experimental data. The ratio of ICF to TF cross-sections, which defines the value of fusion suppression factor is found to be in agreement with the data available from the literature. The...

  6. Quantum Chemical Study of the Solvent Effect on the Anticancer Active Molecule of Iproplatin: Structural, Electronic, and Spectroscopic Properties (IR, 1H NMR, UV)

    Science.gov (United States)

    Sadeghi, N.; Ghiasi, R.; Fazaeli, R.; Jamehbozorgi, S.

    2017-01-01

    The structural, electronic, and spectroscopic properties of the anticancer active molecule of iproplatin were investigated in the gas and liquid phases. Based on the polarizable continuum model (PCM), the solvent effect on the structural parameters, frontier orbitals, and spectroscopic parameters of the complex was investigated. The results indicate that the polarity of solvents plays a significant role in the structure and pro perties of the complex. 1H and 13C NMR chemical shifts were calculated using the Gauge-invariant atomic orbital (GIAO) method. Pt-Cl and Pt-OH bonds were investigated through a vibrational analysis. Moreover, time dependent density functional theory (TD-DFT) was used to calculate the energy, oscillatory strength, and wavelength absorption maximum (λmax) of electronic transitions and its nature within the complex.

  7. Structure analysis and spectroscopic characterization of 2-Fluoro-3-Methylpyridine-5-Boronic Acid with experimental (FT-IR, Raman, NMR and XRD) techniques and quantum chemical calculations

    Science.gov (United States)

    Alver, Özgür; Dikmen, Gökhan

    2016-03-01

    Possible stable conformers, geometrical molecular structures, vibrational properties as well as band assignments, nuclear magnetic shielding tensors of 2-Fluoro-3-Methylpyridine-5-Boronic Acid (2F3MP5BA) were studied experimentally and theoretically using FT-IR, Raman, (CP/MAS) NMR and XRD spectroscopic methods. FT-IR and Raman spectra were evaluated in the region of 3500-400 cm-1, and 3200-400 cm-1, respectively. The optimized geometric structures, vibrational wavenumbers and nuclear magnetic shielding tensors were examined using Becke-3-Lee-Yang-Parr (B3LYP) hybrid density functional theory method with 6-311++G(d, p) basis set. 1H, 13C NMR chemical shifts were calculated using the gauge invariant atomic orbital (GIAO) method. 1H, 13C, APT and HETCOR NMR experiments of title molecule were carried out in DMSO solution. 13C CP/MAS NMR measurement was done with 4 mm zirconium rotor and glycine was used as an external standard. Single crystal of 2F3MP5BA was also prepared for XRD measurements. Assignments of vibrational wavenumbers were also strengthened by calculating the total energy distribution (TED) values using scaled quantum mechanical (SQM) method.

  8. Theory of laser enhancement and suppression of cold reactions: the fermion-boson 6Li+7Li2(variant Planck's over 2pi omega0) 6Li7Li+7Li radiative collision.

    Science.gov (United States)

    Li, Xuan; Parker, Gregory A; Brumer, Paul; Thanopulos, Ioannis; Shapiro, Moshe

    2008-03-28

    We present a nonperturbative time-dependent quantum mechanical theory of the laser catalysis and control of a bifurcating A+BC(variant Planck's over 2pi omega(0))ABC*(v)(variant Planck's over 2pi omega(0) )AB+C reaction, with ABC*(v) denoting an intermediate, electronically excited, complex of ABC in the vth vibrational state. We apply this theory to the low collision energy fermion-boson light-induced exchange reaction, (6)Li((2)S)+(7)Li(2)((3)Sigma(u)(+))(variant Planck's over 2pi omega(0))((6)Li(7)Li(7)Li)*(variant Planck's over 2pi omega(0))(6)Li(7)Li((3)Sigma(+))+(7)Li((2)S). We show that at very low collision energies and energetically narrow (approximately 0.01 cm(-1)) initial reactant wave packets, it is possible to tune the yield of the exchange reaction from 0 to near-unity (yield >or=99%) values. Controllability is somewhat reduced at collisions involving energetically wider (approximately 1 cm(-1)) initial reactant wave packets. At these energetic bandwidths, the radiative reactive control, although still impressive, is limited to the 0%-76% reactive-probabilities range.

  9. Studies of the Efimov Effect in 7 Li

    Science.gov (United States)

    Luo, D.; Nguyen, J. H. V.; Hulet, R. G.

    2016-05-01

    Ultracold atomic gases provide an ideal environment to study few body physics in the universal regime. Passive techniques, such as monitoring loss of the atomic sample while varying the hold time allows us to explore properties such as the scaling behavior of Efimov trimers. In our experiment, we explore how the Efimov states are affected by non-zero temperature. We measure the three-body loss rate for a 7 Li atom gas at different scattering lengths and extract the location and width of an Efimov recombination minimum for various temperatures. Alternatively, we may perform more active experiments such as creating dimers using RF-field modulation as a probe of molecular binding energies. We use RF-association to form Feshbach dimers and Efimov trimers, and find a strong enhancement of the dimer formation rate at the atom-dimer resonance, which could be explained by an avalanche mechanism. In the past the enhancement in the three-body recombination rate at the same location had also been observed, and attributed to the avalanche. We explore the link between these findings with a side-by-side comparison of the dimer-formation rate and the three-body loss rate. Work supported by the NSF, an ARO MURI Grant, and the Welch Foundation.

  10. Non-Gaussian error distribution of 7Li abundance measurements

    Science.gov (United States)

    Crandall, Sara; Houston, Stephen; Ratra, Bharat

    2015-07-01

    We construct the error distribution of 7Li abundance measurements for 66 observations (with error bars) used by Spite et al. (2012) that give A(Li) = 2.21 ± 0.065 (median and 1σ symmetrized error). This error distribution is somewhat non-Gaussian, with larger probability in the tails than is predicted by a Gaussian distribution. The 95.4% confidence limits are 3.0σ in terms of the quoted errors. We fit the data to four commonly used distributions: Gaussian, Cauchy, Student’s t and double exponential with the center of the distribution found with both weighted mean and median statistics. It is reasonably well described by a widened n = 8 Student’s t distribution. Assuming Gaussianity, the observed A(Li) is 6.5σ away from that expected from standard Big Bang Nucleosynthesis (BBN) given the Planck observations. Accounting for the non-Gaussianity of the observed A(Li) error distribution reduces the discrepancy to 4.9σ, which is still significant.

  11. 6Li/7Li estimates for metal-poor stars

    CERN Document Server

    Perez, A E Garcia; Inoue, S; Ryan, S G; Suzuki, T K; Chiba, M

    2009-01-01

    The presence of the lithium-6 isotope in some metal-poor stars is a matter of surprise because of the high values observed. Non-standard models of Big Bang nucleosynthesis and pre-Galactic cosmic ray fusion and spallation have been proposed to explain these values. However, the observations of this light isotope are challenging which may make some detections disputable. The goal was to determine 6Li/7Li for a sample of metal-poor stars; three of them have been previously studied and the remaining two are new for this type of study. The purpose was to increase, if possible, the number of lithium-6 detections and to confirm previously published results. Spectra of the resonance doublet line of neutral lithium Li I 670.78nm were taken with the High Dispersion Spectrograph at the Subaru 8.2m-telescope for a sample of five metal-poor stars (-3.12 < [Fe/H] < -2.19). The contribution of lithium-6 to the total observed line profile was estimated from the 1D-LTE analysis of the line asymmetry. Observed asymmetri...

  12. Solid-state NMR spectroscopic investigation at thermal waste products from embedded flame retardants and polymers; Festkoerper-NMR-Untersuchungen an thermischen Abbauprodukten von flammgeschuetzten Polymeren

    Energy Technology Data Exchange (ETDEWEB)

    Fichera, M.A.

    2008-07-01

    The author of the contribution under consideration describes the structural characterisation of embedded flame retardants and polymers. Analysis includes determination of the phase contents as well as description of their mutual interactions as a function of their thermal history in different atmospheres (air and nitrogen). Solid-state NMR spectroscopy enables structural information about the amorphous state of the decomposed products, determination of the thermal and thermo-oxidative conversion in different amorphous and crystalline structures, and predictions about the short-range order of the observed nuclei. In this context measurements of single pulse, rotor-synchronised spin echo (SP) and cross polarisation (CP) experiments, as well as REDOR (rotational echo double resonance) and TRAPDOR- (transfer of population in double resonance) have been conducted. Additionally, {sup 1}B SP and {sup 31}P RSE experiments have been used to study quantitatively the borate and both phosphorus and phosphate contents in the solid residues. Particular emphasis was put on quantifying crystalline and non-crystalline phosphate phases. The first system consists o a combination of the flame retardants red phosphorus and magnesium hydroxide in high impact polystyrene (HIPS). From the results of extensive NMR experiments it was deduced that most of inserted red phosphorus remains in amorphous phosphates phases (ortho, pyro, and chain/ring phosphates) besides some crystalline phosphate phases. Decomposition characteristics such as temperature and the availability of oxygen (N{sub 2} atmosphere/air) show a significant influence on the decomposition process and the formation of phosphate phases (crystalline/amorphous). By comparing the results of the annealing processes to the results of the cone calorimeter measurements an anaerobic decomposition way was confirmed. In a second system, thermal reactions between the two flame retardants bisphenol A bis diphenyl phosphate and zinc borate

  13. NMR, FT-IR, FT-Raman, UV spectroscopic, HOMO-LUMO and NBO analysis of cumene by quantum computational methods

    Science.gov (United States)

    Sivaranjani, T.; Xavier, S.; Periandy, S.

    2015-03-01

    This work presents the investigation of cumene using the FT-IR, FT-Raman, NMR and UV spectra obtained through various spectroscopic techniques. The theoretical vibrational frequencies and optimized geometric parameters have been calculated by using HF and density functional theory with the hybrid methods B3LYP, B3PW91 and 6-311+G(d,p)/6-311++G(d,p) basis sets. The theoretical vibrational frequencies have been scaled and compared with the corresponding experimental data. 1H and 13C NMR spectra were recorded and chemical shifts of the molecule were compared to TMS by using the Gauge-Independent Atomic Orbital (GIAO) method. A study on the electronic and optical properties, absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, and potential energy surface (PES) is performed using HF and DFT methods. The thermodynamic properties (heat capacity, entropy and enthalpy) at different temperatures are also calculated. NBO analysis is carried out to picture the charge transfer between the localized bonds and lone pairs. NLO properties related to polarizability and hyperpolarizability are also discussed.

  14. Development of a low resolution (1)H NMR spectroscopic technique for the study of matrix mobility in fresh and freeze-thawed hen egg yolk.

    Science.gov (United States)

    Au, Carmen; Wang, Tong; Acevedo, Nuria C

    2016-08-01

    Three experiments were conducted in developing a low resolution proton nuclear magnetic resonance ((1)H NMR) spectroscopic technique to study matrix mobility in fresh and freeze-thawed gelled yolk. The Carr-Purcell-Meiboom-Gill (CPMG) sequence was used to measure spin-spin relaxation times of proton pools representing major yolk constituents. A component identification test distinguished 3-4 pools. The least mobile pool was assigned to proteins, protein-lipid and protein-water interactions, and the most mobile to unbound water. The remaining pools were assigned to lipids, lipid-protein and lipid-water interactions. A stability test indicated that yolk had varied matrix mobility within the same sample across five days of refrigeration storage. A reproducibility test demonstrated high repeatability of fresh yolk measurements, but significant differences (p<0.05) were found within gelled yolk samples. This research determined that (1)H NMR spectroscopy, a non-destructive technique, can identify yolk components and detect changes in the matrix.

  15. Iodine-water-alkanol and potassium iodide-water-alkanol systems: Phase diagrams and regularities of association according to IR and NMR spectroscopic data

    Science.gov (United States)

    Monakhova, Yu. B.; Varlamova, T. M.; Rubtsova, E. M.; Mushtakova, S. P.

    2015-04-01

    The variation of the iodine and potassium iodide solubilities in water-monoatomic alcohol (ethanol, propanol, isopropanol) solvents is considered from the standpoint of IR spectroscopic and chemometric data on association in water-alkanol binary mixtures. The iodine and potassium iodide solubilities in the mixed solvents vary nonlinearly with solvent composition because of the formation of 1 : 1 and 1 : 3 water-alcohol heteroassociates and alcohol homoassociates. Different kinds of phase diagram are observed for the iodine-water-alcohol systems: the I2-H2O-1-C3H7OH and the I2-H2O-2-C3H7OH diagrams have a phase separation region, while the I2-H2O-C2H5OH diagram does not. This fact is explained in terms of the interaction between the components of the systems. The variation of the potassium iodide solubility in the mixed solvent is discussed: a decrease in the KI solubility is symbatic to an increase in the relative concentration of 1 : 1 associates in the water-alcohol solution. The run of the iodine and potassium iodide solubility curves at low alcohol concentrations is explained on the basis of NMR spectroscopic data on association in aqueous solutions of the monoatomic alcohols.

  16. 1H NMR spectroscopic analysis detects metabolic disturbances in rat urine on acute exposure to heavy metal tungsten alloy based metals salt.

    Science.gov (United States)

    Tyagi, Ritu; Rana, Poonam; Gupta, Mamta; Bhatnagar, Deepak; Srivastava, Shatakshi; Roy, Raja; Khushu, Subash

    2014-03-25

    Heavy metal tungsten alloys (HMTAs) have been found to be safer alternatives for making military munitions. Recently, some studies demonstrating the toxic potential of HMTAs have raised concern over the safety issues, and further propose that HMTAs exposure may lead to physiological disturbances as well. To look for the systemic effect of acute toxicity of HMTA based metals salt, (1)H nuclear magnetic resonance ((1)H NMR) spectroscopic profiling of rat urine was carried out. Male Sprague Dawley rats were administered (intraperitoneal) low and high dose of mixture of HMTA based metals salt and NMR spectroscopy was carried out in urine samples collected at 8, 24, 72 and 120 h post dosing (p.d.). Serum biochemical parameters and liver histopathology were also conducted. The (1)H NMR spectra were analysed using multivariate analysis techniques to show the time- and dose-dependent biochemical variations in post HMTA based metals salt exposure. Urine metabolomic analysis showed changes associated with energy metabolism, amino acids, N-methyl nicotinamide, membrane and gut flora metabolites. Multivariate analysis showed maximum variation with best classification of control and treated groups at 24h p.d. At the end of the study, for the low dose group most of the changes at metabolite level reverted to control except for the energy metabolites; whereas, in the high dose group some of the changes still persisted. The observations were well correlated with histopathological and serum biochemical parameters. Further, metabolic pathway analysis clarified that amongst all the metabolic pathways analysed, tricarboxylic acid cycle was most affected at all the time points indicating a switchover in energy metabolism from aerobic to anaerobic. These results suggest that exposure of rats to acute doses of HMTA based metals salt disrupts physiological metabolism with moderate injury to the liver, which might indirectly result from heavy metals induced oxidative stress.

  17. UV-Raman and NMR spectroscopic studies on the crystallization of zeolite A and a new synthetic route.

    Science.gov (United States)

    Ren, Limin; Li, Caijin; Fan, Fengtao; Guo, Qiang; Liang, Desheng; Feng, Zhaochi; Li, Can; Li, Shougui; Xiao, Feng-Shou

    2011-05-23

    UV-Raman and NMR spectroscopy, combined with other techniques, have been used to characterize crystallization of zeolite A. In situ UV-Raman spectroscopy shows that the starting gel for crystallization of zeolite A contains a lot of four-ring (4R) building units and the appearance of six-ring (6R) building blocks is the signal for crystal formation. (29)Si NMR spectroscopy results suggest that the starting gel is double four-ring (D4R) rich and during crystallization of zeolite A both α and β cages appear. (27)Al NMR spectroscopy results indicate the absence of Al (2Si) species in the starting gel, suggesting the absence of single 4R building units in the starting gel. Furthermore, composition analysis of both solid and liquid samples shows that the solid rather than liquid phase predominates for the crystallization of zeolite A. Therefore, it is proposed that the crystallization of zeolite A mainly occurs in the solid phase by self-assembly or rearrangement starting from the zeolite building units mainly consisting of D4R. The essential role of D4R is directly confirmed by successful conversion from a solution of D4R to zeolite A in the presence of NaCl, and the importance of solid phase is reasonably demonstrated by the successful synthesis of zeolite A from a dry aluminosilicate gel. By considering that the solid phase has a major contribution to crystallization, a novel route was designed to synthesizing zeolite A from the raw materials water glass (Na(2)SiO(3) in aqueous solution) and NaAlO(2), without additional water and NaOH; this route not only simplifies synthetic procedures, but reduces water consumption. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Application of spectroscopic methods (FT-IR, Raman, ECD and NMR) in studies of identification and optical purity of radezolid

    Science.gov (United States)

    Michalska, Katarzyna; Gruba, Ewa; Mizera, Mikołaj; Lewandowska, Kornelia; Bednarek, Elżbieta; Bocian, Wojciech; Cielecka-Piontek, Judyta

    2017-08-01

    In the presented study, N-{[(5S)-3-(2-fluoro-4‧-{[(1H-1,2,3-triazol-5-ylmethyl)amino]methyl}biphenyl-4-yl)-2-oxo-1,3-oxazolidin-5-yl]methyl}acetamide (radezolid) was synthesized and characterized using FT-IR, Raman, ECD and NMR. The aim of this work was to assess the possibility of applying classical spectral methods such as FT-IR, Raman, ECD and NMR spectroscopy for studies on the identification and optical purity of radezolid. The experimental interpretation of FT-IR and Raman spectra of radezolid was conducted in combination with theoretical studies. Density functional theory (DFT) with the B3LYP hybrid functional was used for obtaining radezolid spectra. Full identification was carried out by COSY, 1H {13C} HSQC and 1H {13C} HMBC experiments. The experimental NMR chemical shifts and spin-spin coupling constants were compared with theoretical calculations using the DFT method and B3LYP functional employing the 6-311 ++G(d,p) basis set and the solvent polarizable continuum model (PCM). The experimental ECD spectra of synthesized radezolid were compared with experimental spectra of the reference standard of radezolid. Theoretical calculations enabled us to conduct HOMO and LUMO analysis and molecular electrostatic potential maps were used to determine the active sites of microbiologically active form of radezolid enantiomer. The relationship between results of ab initio calculations and knowledge about chemical-biological properties of S-radezolid and other oxazolidinone derivatives are also discussed.

  19. Structural, vibrational and NMR spectroscopic investigations of newly synthesized 3-((ethylthio)(4-nitrophenyl)methyl)-1H-indole

    Science.gov (United States)

    Bhat, Sheeraz Ahmad; Dar, Ajaz A.; Ahmad, Shabbir; Khan, Abu T.

    2017-10-01

    The compound 3-((ethylthio)(4-nitrophenyl)methyl)-1H-indole was synthesized at room temperature through one-pot three-component reaction from 1H-indole, 4-nitrobenzaldehyde, and ethanethiol using hydrated ferric sulfate as a Lewis acid catalyst. The structure was characterised by single crystal XRD, FTIR (4000-400 cm-1), FT-Raman (4000-50 cm-1) and 1H and 13C NMR analysis. The compound crystallizes in the monoclinic with volume 3238.3(9) Å3. The experimental vibrational data find the theoretical support through anharmonic frequency calculations using DFT/B3LYP level of theory in combination with 6-31G(d,p) basis set. It is observed that the predicted geometry well reproduces the XRD structural parameters. The experimental 1H and 13C NMR spectra in CDCl3 solvent and the simulated spectra predicted using gauge independent atomic orbital (GIAO) approach are also found in agreement with each other. HOMO-LUMO, MEP, atomic charges and various other thermodynamic and NLO properties of the title molecule are also reported in this paper.

  20. NMR spectroscopic and bioinformatic analyses of the LTBP1 C-terminus reveal a highly dynamic domain organisation.

    Directory of Open Access Journals (Sweden)

    Ian B Robertson

    Full Text Available Proteins from the LTBP/fibrillin family perform key structural and functional roles in connective tissues. LTBP1 forms the large latent complex with TGFβ and its propeptide LAP, and sequesters the latent growth factor to the extracellular matrix. Bioinformatics studies suggest the main structural features of the LTBP1 C-terminus are conserved through evolution. NMR studies were carried out on three overlapping C-terminal fragments of LTBP1, comprising four domains with characterised homologues, cbEGF14, TB3, EGF3 and cbEGF15, and three regions with no homology to known structures. The NMR data reveal that the four domains adopt canonical folds, but largely lack the interdomain interactions observed with homologous fibrillin domains; the exception is the EGF3-cbEGF15 domain pair which has a well-defined interdomain interface. (15N relaxation studies further demonstrate that the three interdomain regions act as flexible linkers, allowing a wide range of motion between the well-structured domains. This work is consistent with the LTBP1 C-terminus adopting a flexible "knotted rope" structure, which may facilitate cell matrix interactions, and the accessibility to proteases or other factors that could contribute to TGFβ activation.

  1. Crystal structure, magnetism, {sup 89}Y solid state NMR, and {sup 121}Sb Moessbauer spectroscopic investigations of YIrSb

    Energy Technology Data Exchange (ETDEWEB)

    Benndorf, Christopher [Institut fuer Physikalische Chemie, Universitaet Muenster (Germany); Institut fuer Anorganische und Analytische Chemie, Universitaet Muenster (Germany); Heletta, Lukas; Block, Theresa; Poettgen, Rainer [Institut fuer Anorganische und Analytische Chemie, Universitaet Muenster (Germany); Eckert, Hellmut [Institut fuer Physikalische Chemie, Universitaet Muenster (Germany); Institute of Physics in Sao Carlos, University of Sao Paulo, Sao Carlos (Brazil)

    2017-02-15

    The ternary antimonide YIrSb was synthesized from the binary precursor YIr and elemental antimony by a diffusion controlled solid-state reaction. Single crystals were obtained by a flux technique with elemental bismuth as an inert solvent. The YIrSb structure (TiNiSi type, space group Pnma) was refined from single-crystal X-ray diffractometer data: a = 711.06(9), b = 447.74(5), c = 784.20(8) pm, wR{sub 2} = 0.0455, 535 F{sup 2} values, 20 variables. {sup 89}Y solid state MAS NMR and {sup 121}Sb Moessbauer spectra show single resonance lines in agreement with single-crystal X-ray data. YIrSb is a Pauli paramagnet. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. Syntheses, structures, and comprehensive NMR spectroscopic investigations of hetero-chalcogenidometallates: the right mix toward multinary complexes.

    Science.gov (United States)

    Ruzin, Eugen; Zent, Eldar; Matern, Eberhard; Massa, Werner; Dehnen, Stefanie

    2009-01-01

    Aqueous solutions of ternary ortho-chalcogenidostannate anions [SnE(1)(4-x)E(2)(x)](4-) (E(1), E(2) = S, Se, Te) have been generated following different routes that all lead to equilibria of all possible permutations of binary and ternary anions. This has been rationalized by means of NMR studies that can be explained by calculations using density functional theory (DFT) methods. Thus, if one reacts such solutions with transition-metal ions, quaternary M/Sn/E(1)/E(2) anions are obtained, which exhibit coordination by different ternary chalcogenidostannate ligands. The electronic excitation energies of the corresponding alkali metal salts lie between the E(g) values of compounds containing either M/Sn/E(1) or M/Sn/E(2) anions. In this way, we provide a simple approach toward a library of semiconductor compounds with finely-tuned optoelectronic properties.

  3. Structural, NMR Spectroscopic, and Computational Investigation of Hemin Loading in the Hemophore HasAp from Pseudomonas aeruginosa

    Energy Technology Data Exchange (ETDEWEB)

    Jepkorir, Grace; Rodrguez, Juan Carlos; Rui, Huan; Im, Wonpil; Lovell, Scott; Battaile, Kevin P.; Alontaga, Aileen Y.; Yukl, Erik T.; Monne-Loccoz, Pierre; Rivera, Mario (Oregon State U.); (Kansas); (Hauptman)

    2010-08-16

    When challenged by low-iron conditions several Gram-negative pathogens secrete a hemophore (HasA) to scavenge hemin from its host and deliver it to a receptor (HasR) on their outer membrane for internalization. Here we report results from studies aimed at probing the structural and dynamic processes at play in the loading of the apo-hemophore secreted by P. aeruginosa (apo-HasAp) with hemin. The structure of apo-HasAp shows a large conformational change in the loop harboring axial ligand His32 relative to the structure of holo-HasAp, whereas the loop bearing the other axial ligand, Tyr75, remains intact. To investigate the role played by the axial ligand-bearing loops in the process of hemin capture we investigated the H32A mutant, which was found to exist as a monomer in its apo-form and as a mixture of monomers and dimers in its holo-form. We obtained an X-ray structure of dimeric H32A holo-HasAp, which revealed that the two subunits are linked by cofacial interactions of two hemin molecules and that the conformation of the Ala32 loop in the dimer is identical to that exhibited by the His32 loop in wild type apo-HasAp. Additional data suggest that the conformation of the Ala32 loop in the dimer is mainly a consequence of dimerization. Hence, to investigate the effect of hemin loading on the topology of the His32 loop we also obtained the crystal structure of monomeric H32A holo-HasAp coordinated by imidazole (H32A-imidazole) and investigated the monomeric H32A HasAp and H32A-imidazole species in solution by NMR spectroscopy. The structure of H32A-imidazole revealed that the Ala32 loop attains a 'closed' conformation nearly identical to that observed in wild type holo-HasAp, and the NMR investigations indicated that this conformation is maintained in solution. The NMR studies also highlighted conformational heterogeneity at the H32 loop hinges and in other key sections of the structure. Targeted molecular dynamics simulations allowed us to propose a

  4. Further NMR-spectroscopic studies of interaction of phospholipid liposomes with methacryloyloxydecyl dihydrogen phosphate (MDP) in dental adhesives.

    Science.gov (United States)

    Fujisawa, S; Komoda, Y

    1993-06-01

    To determine how MDP interacts with liposomes, the chemical shifts of dipalmitoylphosphatidylcholine (DPPC)/MDP and dilauroylphosphatidylethanolamine (DLEA)/cholesterol (CS)/MDP liposomes were studied by NMR spectroscopy using a D2O buffer solution at pH 7.0 as a model for biological membranes. Proton chemical shifts of MDP enhanced shielding in DPPC liposomes together with an increase in the mobility of DPPC. However, MDP signals were not observed in DLEA/CS liposomes due to saturation. It is known that an ionized chemical does not lead to increased permeability of cell membranes composed of a lipid bilayer. However, MDP, which is ionized at pH 7.0, had a large interaction with the liposome systems. This appeared to arise from hydrophobic interaction between deca methylene groups of MDP and acyl chains of phospholipid.

  5. Spectroscopic (infrared, Raman, UV and NMR) analysis, Gaussian hybrid computational investigation (MEP maps/HOMO and LUMO) on cyclohexanone oxime

    Science.gov (United States)

    Ramalingam, S.; Karabacak, M.; Periandy, S.; Puviarasan, N.; Tanuja, D.

    2012-10-01

    In the present analysis, FT-IR/FT-Raman spectra of the cyclohexanone oxime (CHO, C6H11NO) are recorded. The observed vibrational frequencies are assigned and the computational calculations are carried out by HF and DFT (B3LYP and B3PW91) methods with 6-311++G(d,p) basis set and the corresponding results are tabulated. In order to yield good coherence with observed values, the calculated frequencies are scaled by appropriate scale factors. The complete assignments are performed on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method. The alternation of structure of cyclohexanone due to the substitution of NOH is investigated. The vibrational sequence pattern of the molecule related to the substitutions is analyzed. Comparison of the observed fundamental vibrational frequencies of CHO and calculated results by density functional (B3LYP and B3PW91) and HF methods indicates that B3LYP is superior to the scaled HF and B3PW91 approach for molecular vibrational problems. Moreover, 13C NMR and 1H NMR chemical shifts are calculated by using the gauge independent atomic orbital (GIAO) method with HF/B3LYP/B3PW91 methods and the same basis set. A study on the electronic properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, are performed by HF and DFT methods. The calculated HOMO and LUMO energies show that charge transfer occurs within the molecule. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. NLO properties and Mulliken charges of the CHO was also calculated and interpreted. The thermodynamic properties (heat capacity, entropy, and enthalpy) of the title compound at different temperatures are calculated in gas phase.

  6. Solution 1H, 15N NMR spectroscopic characterization of substrate-bound, cyanide-inhibited human heme oxygenase: water occupation of the distal cavity.

    Science.gov (United States)

    Li, Yiming; Syvitski, Ray T; Auclair, Karine; Ortiz de Montellano, Paul; La Mar, Gerd N

    2003-11-05

    A solution NMR spectroscopic study of the cyanide-inhibited, substrate-bound complex of uniformly (15)N-labeled human heme oxygenase, hHO, has led to characterization of the active site with respect to the nature and identity of strong hydrogen bonds and the occupation of ordered water molecules within both the hydrogen bonding network and an aromatic cluster on the distal side. [(1)H-(15)N]-HSQC spectra confirm the functionalities of several key donors in particularly robust H-bonds, and [(1)H-(15)N]HSQC-NOESY spectra lead to the identification of three additional robust H-bonds, as well as the detection of two more relatively strong H-bonds whose identities could not be established. The 3D NMR experiments provided only a modest, but important, extension of assignments because of the loss of key TOCSY cross-peaks due to the line broadening from a dynamic heterogeneity in the active site. Steady-state NOEs upon saturating the water signal locate nine ordered water molecules in the immediate vicinity of the H-bond donors, six of which are readily identified in the crystal structure. The additional three are positioned in available spaces to account for the observed NOEs. (15)N-filtered steady-state NOEs upon saturating the water resonances and (15)N-filtered NOESY spectra demonstrate significant negative NOEs between water molecules and the protons of five aromatic rings. Many of the NOEs can be rationalized by water molecules located in the crystal structure, but strong water NOEs, particularly to the rings of Phe47 and Trp96, demand the presence of at least an additional two immobilized water molecules near these rings. The H-bond network appears to function to order water molecules to provide stabilization for the hydroperoxy intermediate and to serve as a conduit to the active site for the nine protons required per HO turnover.

  7. Spectroscopic (FT-IR, FT-Raman, UV, NMR, NBO) investigation and molecular docking study of (R)-2-Amino-1-PhenylEthanol

    Science.gov (United States)

    Subashini, K.; Periandy, S.

    2016-08-01

    A systematic spectroscopic study of (R)-2-Amino-1-Phenylethanol was carried out using FT-IR, FT-Raman, NMR and UV analysis. FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectrum of the title molecule were recorded in solid phase, the 1H and 13C NMR spectra were recorded in CDCl3 (deuterated chloroform) solution phase and the UV-Vis (200-800 nm) spectrum was recorded in gas phase and ethanol solution phase. Potential energy surface (PES) scan was performed using B3LYP functional with 6-311++G (d, p) basis set. The geometrical parameters (such as bond length, bond angle, dihedral angles) and theoretical frequencies of the title compound were studied from density functional theory (DFT) using B3LYP and B3PW91 functionals with 6-311++G (d, p) basis sets. The computed frequencies were scaled and compared with the experimental values and potential energy distribution (PED) has been tabulated. A comparative study of atomic charges was made by calculating Mulliken, Natural Population Analysis (NPA) and Electrostatic Potential (ESP) simultaneously, with B3LYP/6-311++G (d, p) basis set. 1H and 13C NMR spectra were recorded and chemical shifts were compared to TMS by Gauge-Independent Atomic Orbital (GIAO) method. Electronic properties such as excitation energy, energy gap between HOMO and LUMO was calculated using time dependent DFT technique. NBO analysis, which predicts the different possibilities of electronic transition in the molecule, was computed using B3PW91 functional with 6-311++G (d, p) basis set. The thermodynamic properties such as heat capacity, entropy and enthalpy at different temperatures were computed and analyzed. Molecular docking study shows that the secondary hydroxyl group and the primary amino group in the aliphatic chain attached to the benzene ring are crucial for binding and the title compound might exhibit inhibitory activity against Bacteroides fragilis (3P24) and may act as anti-bacterial agent.

  8. In situ7Li and 133Cs nuclear magnetic resonance investigations on the role of Cs+ additive in lithium-metal deposition process

    Science.gov (United States)

    Hu, Jian Zhi; Zhao, Zhenchao; Hu, Mary Y.; Feng, Ju; Deng, Xuchu; Chen, Xilin; Xu, Wu; Liu, Jun; Zhang, Ji-Guang

    2016-02-01

    Cesium ion (Cs+) has been reported to be an effective electrolyte additive to suppress Li dendrite growth which prevents the application of lithium (Li) metal as an anode for rechargeable Li batteries. In this work, we investigated the effect of Cs+ additive on Li depositions using quantitative in situ7Li and 133Cs nuclear magnetic resonance (NMR) with planar symmetric Li cells. It's found that the addition of Cs+ can significantly enhance both the formation of well aligned Li nanorods and reversibility of the Li electrode. In situ133Cs NMR directly confirms that Cs+ migrates to Li electrode to form a positively charged electrostatic shield during the charging process. Much more electrochemical "active" Li was found in Li films deposited with Cs+ additive, while more electrochemical "dead" and thicker Li rods were identified in Li films deposited without Cs+. Combining the in situ and the previous ex-situ results, a Li deposition model has been proposed to explain these observations.

  9. Breakup mechanisms for 7Li + 197Au, 204Pb systems at sub-barrier energies

    Directory of Open Access Journals (Sweden)

    Luong D.H.

    2013-12-01

    Full Text Available Coincidence measurements of breakup fragments were carried out for the 7Li + 197Au and 204Pb systems at sub-barrier energies. The mechanisms triggering breakup, and time-scales of each process, were identified through the reaction Q-values and the relative energy of the breakup fragments. Binary breakup of 7Li were found to be predominantly triggered by nucleon transfer, with p-pickup leading to 8Be → α + α decay being the preferred breakup mode. From the time-scales of each process, the coincidence yields were separated into prompt and delayed components, allowing the identification of breakup process important in the suppression of complete fusion of 7Li at above-barrier energies.

  10. Spectroscopic quantification of soil phosphorus forms by {sup 31}P-NMR after nine years of organic or mineral fertilization

    Energy Technology Data Exchange (ETDEWEB)

    Gatiboni, Luciano Colpo, E-mail: gatiboni@cav.udesc.br [Universidade Estadual de Santa Catarina (UDESC), Lages, SC (Brazil); Brunetto, Gustavo; Rheinheimer, Danilo dos Santos; Kaminski, Joao; Flores, Alex Fabiani Claro; Lima, Maria Angelica Silveira; Girotto, Eduardo; Copetti, Andre Carlos Cruz, E-mail: danilo.rheinheimer@pq.cnpq.br, E-mail: joao.kaminski@gmail.com, E-mail: acflores@quimica.ufsm.br, E-mail: masl32003@gmail.com, E-mail: girottosolos@gmail.com, E-mail: andrecopetti@yahoo.com.br [Universidade Federal de Santa Maria (UFSM), RS (Brazil); Pandolfo, Carla Maria; Veiga, Milton, E-mail: pandolfo@epagri.sc.gov.br, E-mail: milveiga@epagri.sc.gov.br [Empresa de Pesquisa Agropecuaria e Extensao Rural de Santa Catarina (EPAGRI), Campos Novos, SC (Brazil)

    2013-05-15

    Long-standing applications of mineral fertilizers or types of organic wastes such as manure can cause phosphorus (P) accumulation and changes in the accumulated P forms in the soil. The objective of this research was to evaluate the forms of P accumulated in soils treated with mineral fertilizer or different types of manure in a long-term experiment. Soil was sampled from the 0-5 cm layer of plots fertilized with five different nutrient sources for nine years: 1) control without fertilizer; 2) mineral fertilizer at recommended rates for local conditions; 3) 5 t ha{sup -1} year{sup -1} of moist poultry litter; 4) 60 m{sup 3} ha{sup -1} year{sup -1} of liquid cattle manure and 5) 40 m{sup 3} ha{sup -1} year{sup -1} of liquid swine manure. The {sup 31}P-NMR spectra of soil extracts detected the following P compounds: orthophosphate, pyrophosphate, inositol phosphate, glycerophosphate, and DNA. The use of organic or mineral fertilizer over nine years did not change the soil P forms but influenced their concentration. Fertilization with mineral or organic fertilizers stimulated P accumulation in inorganic forms. Highest inositol phosphate levels were observed after fertilization with any kind of manure and highest organic P concentration in glycerophosphate form in after mineral or no fertilization. (author)

  11. Spectroscopic quantification of soil phosphorus forms by 31p-nmr after nine years of organic or mineral fertilization

    Directory of Open Access Journals (Sweden)

    Luciano Colpo Gatiboni

    2013-06-01

    Full Text Available Long-standing applications of mineral fertilizers or types of organic wastes such as manure can cause phosphorus (P accumulation and changes in the accumulated P forms in the soil. The objective of this research was to evaluate the forms of P accumulated in soils treated with mineral fertilizer or different types of manure in a long-term experiment. Soil was sampled from the 0-5 cm layer of plots fertilized with five different nutrient sources for nine years: 1 control without fertilizer; 2 mineral fertilizer at recommended rates for local conditions; 3 5 t ha-1 year-1 of moist poultry litter; 4 60 m³ ha-1 year-1 of liquid cattle manure and 5 40 m³ ha-1 year-1 of liquid swine manure. The 31P-NMR spectra of soil extracts detected the following P compounds: orthophosphate, pyrophosphate, inositol phosphate, glycerophosphate, and DNA. The use of organic or mineral fertilizer over nine years did not change the soil P forms but influenced their concentration. Fertilization with mineral or organic fertilizers stimulated P accumulation in inorganic forms. Highest inositol phosphate levels were observed after fertilization with any kind of manure and highest organic P concentration in glycerophosphate form in after mineral or no fertilization.

  12. Vibrational, NMR and UV-visible spectroscopic investigation and NLO studies on benzaldehyde thiosemicarbazone using computational calculations

    Science.gov (United States)

    Moorthy, N.; Prabakar, P. C. Jobe; Ramalingam, S.; Pandian, G. V.; Anbusrinivasan, P.

    2016-04-01

    In order to investigate the vibrational, electronic and NLO characteristics of the compound; benzaldehyde thiosemicarbazone (BTSC), the XRD, FT-IR, FT-Raman, NMR and UV-visible spectra were recorded and were analysed with the calculated spectra by using HF and B3LYP methods with 6-311++G(d,p) basis set. The XRD results revealed that the stabilized molecular systems were confined in orthorhombic unit cell system. The cause for the change of chemical and physical properties behind the compound has been discussed makes use of Mulliken charge levels and NBO in detail. The shift of molecular vibrational pattern by the fusing of ligand; thiosemicarbazone group with benzaldehyde has been keenly observed. The occurrence of in phase and out of phase molecular interaction over the frontier molecular orbitals was determined to evaluate the degeneracy of the electronic energy levels. The thermodynamical studies of the temperature region 100-1000 K to detect the thermal stabilization of the crystal phase of the compound were investigated. The NLO properties were evaluated by the determination of the polarizability and hyperpolarizability of the compound in crystal phase. The physical stabilization of the geometry of the compound has been explained by geometry deformation analysis.

  13. Design of ET(B) receptor agonists: NMR spectroscopic and conformational studies of ET7-21[Leu7, Aib11, Cys(Acm)15].

    Science.gov (United States)

    Hewage, Chandralal M; Jiang, Lu; Parkinson, John A; Ramage, Robert; Sadler, Ian H

    2002-03-01

    In a previous report we have shown that the endothelin-B receptor-selective linear endothelin peptide, ET-1[Cys (Acm)1,15, Ala3, Leu7, Aib11], folds into an alpha-helical conformation in a methanol-d3/water co-solvent [Hewage et al. (1998) FEBS Lett., 425, 234-238]. To study the requirements for the structure-activity relationships, truncated analogues of this peptide were subjected to further studies. Here we report the solution conformation of ET7-21[Leu7, Aib11, Cys(Acm)15], in a methanol-d3/water co-solvent at pH 3.6, by NMR spectroscopic and molecular modelling studies. Further truncation of this short peptide results in it displaying poor agonist activity. The modelled structure shows that the peptide folds into an alpha-helical conformation between residues Lys9-His16, whereas the C-terminus prefers no fixed conformation. This truncated linear endothelin analogue is pivotal for designing endothelin-B receptor agonists.

  14. The spectroscopic properties of anticancer drug Apigenin investigated by using DFT calculations, FT-IR, FT-Raman and NMR analysis

    Science.gov (United States)

    Mariappan, G.; Sundaraganesan, N.; Manoharan, S.

    2012-09-01

    The FT-Raman and FT-Infrared spectra of solid Apigenin sample were measured in order to elucidate the spectroscopic properties of title molecule in the spectral range of 3500-50 cm-1 and 4000-400 cm-1, respectively. The recorded FT-IR and FT-Raman spectral measurements favor the calculated (by B3LYP/6-31G(d,p) method) structural parameters which are further supported by spectral simulation. Additional support is given by the collected 1H and 13C NMR spectra recorded with the sample dissolved in DMSO. The predicted chemical shifts at the B3LYP/6-31G(d) level obtained using the Gauge-Invariant Atomic Orbitals (GIAO) method with and without inclusion of solvent using the Polarizable Continuum Model (PCM). By using TD-DFT method, electronic absorption spectra of the title compound have been predicted and a good agreement with the TD-DFT method and the experimental one is determined. The UV-visible absorption spectra of the compound that dissolved in Ethanol, Methanol and DMSO were recorded in the range of 800-200 nm. The formation of hydrogen bond and the most possible interaction are explained using natural bond orbital (NBO) analysis. In addition, the molecular electrostatic potential (MEP), frontier molecular orbitals (FMO) analysis and atomic charges of the title compound were investigated using theoretical calculations. The results are discussed herein and compared with similar molecules whenever appropriate.

  15. Divergent Urinary Metabolic Phenotypes between Major Depressive Disorder and Bipolar Disorder Identified by a Combined GC-MS and NMR Spectroscopic Metabonomic Approach.

    Science.gov (United States)

    Chen, Jian-Jun; Zhou, Chan-Juan; Liu, Zhao; Fu, Yu-Ying; Zheng, Peng; Yang, De-Yu; Li, Qi; Mu, Jun; Wei, You-Dong; Zhou, Jing-Jing; Huang, Hua; Xie, Peng

    2015-08-07

    Bipolar disorder (BD) is a complex debilitating mental disorder that is often misdiagnosed as major depressive disorder (MDD). Therefore, a large percentage of BD subjects are incorrectly treated with antidepressants in clinical practice. To address this challenge, objective laboratory-based tests are needed to discriminate BD from MDD patients. Here, a combined gas chromatography-mass spectrometry (GC-MS)-based and nuclear magnetic resonance (NMR) spectroscopic-based metabonomic approach was performed to profile urine samples from 76 MDD and 43 BD subjects (training set) to identify the differential metabolites. Samples from 126 healthy controls were included as metabolic controls. A candidate biomarker panel was identified by further analyzing these differential metabolites. A testing set of, 50 MDD and 28 BD subjects was then used to independently validate the diagnostic efficacy of the identified panel using an area under the receiver operating characteristic curve (AUC). A total of 20 differential metabolites responsible for the discrimination between MDD and BD subjects were identified. A panel consisting of six candidate urinary metabolite biomarkers (propionate, formate, (R*,S*)2,3-dihydroxybutanoic acid, 2,4-dihydroxypyrimidine, phenylalanine, and β-alanine) was identified. This panel could distinguish BD from MDD subjects with an AUC of 0.913 and 0.896 in the training and testing sets, respectively. These results reveal divergent urinary metabolic phenotypes between MDD and BD. The identified urinary biomarkers can aid in the future development of an objective laboratory-based diagnostic test for distinguishing BD from MDD patients.

  16. Binding modes of environmental endocrine disruptors to human serum albumin: insights from STD-NMR, ITC, spectroscopic and molecular docking studies.

    Science.gov (United States)

    Yang, Hongqin; Huang, Yanmei; Liu, Jiuyang; Tang, Peixiao; Sun, Qiaomei; Xiong, Xinnuo; Tang, Bin; He, Jiawei; Li, Hui

    2017-09-11

    Given that bisphenols have an endocrine-disrupting effect on human bodies, thoroughly exposing their potential effects at the molecular level is important. Saturation transfer difference (STD) NMR-based binding studies were performed to investigate the binding potential of two bisphenol representatives, namely, bisphenol B (BPB) and bisphenol E (BPE), toward human serum albumin (HSA). The relative STD (%) suggested that BPB and BPE show similar binding modes and orientations, in which the phenolic rings were spatially close to HSA binding site. ITC analysis results showed that BPB and BPE were bound to HSA with moderately strong binding affinity through electrostatic interactions and hydrogen bonds. The order of binding affinity of HSA for two test bisphenols is as follows: BPE > BPB. The results of fluorescence competitive experiments using 5-dimethylaminonaphthalene-1-sulfonamide and dansylsarcosine as competitors, combined with molecular docking indicated that both bisphenols are prone to attach to the binding site II in HSA. Spectroscopic results (FT-IR, CD, synchronous and 3D fluorescence spectra) showed that BPB/BPE induces different degrees of microenvironmental and conformational changes to HSA.

  17. Spectroscopic characteristic (FT-IR, FT-Raman, UV, 1H and 13C NMR), theoretical calculations and biological activity of alkali metal homovanillates

    Science.gov (United States)

    Samsonowicz, M.; Kowczyk-Sadowy, M.; Piekut, J.; Regulska, E.; Lewandowski, W.

    2016-04-01

    The structural and vibrational properties of lithium, sodium, potassium, rubidium and cesium homovanillates were investigated in this paper. Supplementary molecular spectroscopic methods such as: FT-IR, FT-Raman in the solid phase, UV and NMR were applied. The geometrical parameters and energies were obtained from density functional theory (DFT) B3LYP method with 6-311++G** basis set calculations. The geometry of the molecule was fully optimized, vibrational spectra were calculated and fundamental vibrations were assigned. Geometric and magnetic aromaticity indices, atomic charges, dipole moments, HOMO and LUMO energies were also calculated. The microbial activity of investigated compounds was tested against Bacillus subtilis (BS), Pseudomonas aeruginosa (PA), Escherichia coli (EC), Staphylococcus aureus (SA) and Candida albicans (CA). The relationship between the molecular structure of tested compounds and their antimicrobial activity was studied. The principal component analysis (PCA) was applied in order to attempt to distinguish the biological activities of these compounds according to selected band wavenumbers. Obtained data show that the FT-IR spectra can be a rapid and reliable analytical tool and a good source of information for the quantitative analysis of the relationship between the molecular structure of the compound and its biological activity.

  18. Nuclear structure constrains on resonant energies: A solution of the cosmological {sup 7}Li problem?

    Energy Technology Data Exchange (ETDEWEB)

    Civitarese, O., E-mail: osvaldo.civitarese@fisica.unlp.edu.ar [Department of Physics, University of La Plata c.c. 67, 1900 La Plata (Argentina); Mosquera, M.E., E-mail: mmosquera@fcaglp.unlp.edu.ar [Department of Physics, University of La Plata c.c. 67, 1900 La Plata (Argentina); Facultad de Ciencias Astronómicas y Geofísicas, Universidad Nacional de La Plata, Paseo del Bosque, 1900 La Plata (Argentina)

    2013-01-17

    In this work, we study the cosmological {sup 7}Li problem from a nuclear structure point of view, by including resonances in the reactions which populate beryllium. The calculation of primordial abundances is performed by solving the balance equations semi-analytically. It is found that the primordial abundance of lithium is indeed reduced, as a consequence of the presence of resonant channels in the relevant cross sections. We set limits on the resonant energy for each reaction relevant for the chain leading to {sup 7}Li, by performing a statistical analysis of the available observational data.

  19. Radioactive contamination of {sup 7}LiI(Eu) crystal scintillators

    Energy Technology Data Exchange (ETDEWEB)

    Belli, P. [INFN sezione Roma “Tor Vergata”, I-00133 Rome (Italy); Dipartimento di Fisica, Università di Roma “Tor Vergata”, I-00133 Rome (Italy); Bernabei, R., E-mail: rita.bernabei@roma2.infn.it [INFN sezione Roma “Tor Vergata”, I-00133 Rome (Italy); Dipartimento di Fisica, Università di Roma “Tor Vergata”, I-00133 Rome (Italy); Budakovsky, S.V. [Institute for Scintillation Materials, 61001 Kharkiv (Ukraine); Cappella, F. [INFN sezione Roma “La Sapienza”, I-00185 Rome (Italy); Dipartimento di Fisica, Università di Roma “La Sapienza”, I-00185 Rome (Italy); Cerulli, R. [INFN, Laboratori Nazionali del Gran Sasso, I-67100 Assergi (AQ) (Italy); Danevich, F.A. [Institute for Nuclear Research, MSP 03680 Kyiv (Ukraine); D' Angelo, S. [INFN sezione Roma “Tor Vergata”, I-00133 Rome (Italy); Dipartimento di Fisica, Università di Roma “Tor Vergata”, I-00133 Rome (Italy); Incicchitti, A. [INFN sezione Roma “La Sapienza”, I-00185 Rome (Italy); Dipartimento di Fisica, Università di Roma “La Sapienza”, I-00185 Rome (Italy); Laubenstein, M. [INFN, Laboratori Nazionali del Gran Sasso, I-67100 Assergi (AQ) (Italy); Poda, D.V. [Institute for Nuclear Research, MSP 03680 Kyiv (Ukraine); and others

    2013-03-11

    The radioactive contamination of two 26 g samples of low background lithium iodide crystal scintillators doped by europium and enriched in {sup 7}Li to 99.9% ({sup 7}LiI(Eu)) has been investigated by scintillation method at the sea level, and by ultra-low background HPGe γ spectrometry deep underground. No radioactive contamination was detected. In particular, the contamination of the crystal scintillators by {sup 226}Ra and {sup 228}Th does not exceed 1 mBq/kg, and the activity of {sup 40}K is less than 0.5 Bq/kg.

  20. Search for higher excited states of $^{8}$Be* to study the cosmological $^{7}$Li problem

    CERN Multimedia

    We would like to study the unresolved $^{7}$Li abundance anomaly by carrying out experiments that destroy the rare isotope $^{7}$Be, the main source of $^{7}$Li. Utilizing a 35 MeV $^{7}$Be beam from HIE-ISOLDE, we would like to measure the (d,p) and (d,d) reactions with T-REX. The higher beam energy, for the first time, would allow us to measure higher excitation energies in $^{8}$Be up to about 20 MeV. With a wider angular coverage, we can make improved average cross-section measurement without assuming isotropy done in earlier works.

  1. Hyperfine structure in photoassociative spectra of 6Li2 and 7Li2

    NARCIS (Netherlands)

    Abraham, E.R.I.; McAlexander, W.I.; Stoof, H.T.C.; Hulet, R.G.

    1996-01-01

    We present spectra of hyperfine resolved vibrational levels of the A1Σu+and 1 3Σg+ states of 6Li2 and 7Li2 obtained via photoassociation of colliding ultracold atoms in a magneto-optical trap. A simple first-order perturbation theory analysis accurately accounts for the frequency splittings and rela

  2. NMR, FT-IR, Raman and UV-Vis spectroscopic investigation and DFT study of 6-Bromo-3-Pyridinyl Boronic Acid

    Science.gov (United States)

    Dikmen, Gökhan; Alver, Özgür

    2015-11-01

    Possible stable conformers and geometrical molecular structures of 6-Bromo-3-Pyridinyl Boronic acid (6B3PBA; C5H5BBrNO2) were studied experimentally and theoretically using FT-IR and Raman spectroscopic methods. FT-IR and Raman spectra were recorded in the region of 4000-400 cm-1 and 3700-400 cm-1, respectively. The structural properties were investigated further, using 1H, 13C, 1H coupled 13C, HETCOR, COSY and APT NMR techniques. The optimized geometric structures were searched by Becke-3-Lee-Yang-Parr (B3LYP) hybrid density functional theory method with 6-311++G(d, p) basis set. Vibrational wavenumbers of 6B3PBA were calculated whereby B3LYP density functional methods including 6-311++G(d, p), 6-311G(d, p), 6-311G(d), 6-31G(d, p) and 6-31G(d) basis sets. The comparison of the experimentally and theoretically obtained results using mean absolute error and experimental versus calculated correlation coefficients for the vibrational wavenumbers indicates that B3LYP method with 6-311++G(d, p) gives more satisfactory results for predicting vibrational wavenumbers when compared to the 6-311G(d, p), 6-311G(d), 6-31G(d, p) and 6-31G(d) basis sets. However, this method and none of the mentioned methods here seem suitable for the calculations of OH stretching modes, most likely because increasing unharmonicity in the high wave number region and possible intra and inter molecular interactions at OH edges lead some deviations between experimental and theoretical results. Moreover, reliable vibrational assignments were made on the basis of total energy distribution (TED) calculated using scaled quantum mechanical (SQM) method.

  3. Formation of ultracold 7Li85Rb molecules in the lowest triplet electronic state by photoassociation and their detection by ionization spectroscopy

    Science.gov (United States)

    Altaf, Adeel; Dutta, Sourav; Lorenz, John; Pérez-Ríos, Jesús; Chen, Yong P.; Elliott, D. S.

    2015-03-01

    We report the formation of ultracold 7Li85Rb molecules in the a3Σ+ electronic state by photoassociation (PA) and their detection via resonantly enhanced multiphoton ionization (REMPI). With our dual-species Li and Rb magneto-optical trap apparatus, we detect PA resonances with binding energies up to ˜62 cm-1 below the 7Li 2s 2S1/2 + 85Rb 5p 2P1/2 asymptote. In addition, we use REMPI spectroscopy to probe the a3Σ+ state and excited electronic 33Π and 43Σ+ states and identify a3Σ+ (v″ = 7-13), 33Π (vΠ' = 0-10), and 43Σ+ (vΣ' = 0-5) vibrational levels. Our line assignments agree well with ab initio calculations. These preliminary spectroscopic studies on previously unobserved electronic states are crucial to discovering transition pathways for transferring ultracold LiRb molecules created via PA to deeply bound rovibrational levels of the electronic ground state.

  4. Push-through Direction Injectin NMR Automation

    Science.gov (United States)

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

  5. Push-through Direction Injectin NMR Automation

    Science.gov (United States)

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

  6. Probing transfer to unbound states of the ejectile with weakly bound 7Li on 93Nb

    CERN Document Server

    Pandit, S K; Mahata, K; Keeley, N; Parkar, V V; Rout, P C; Martel, I; Palshetkar, C S; Kumar, A; Ramachandran, K; Patale, P; Chatterjee, A; Kailas, S

    2016-01-01

    The two-step process of transfer followed by breakup is explored by measuring a rather complete set of exclusive data for reaction channels populating states in the ejectile continua of the $^7$Li+$^{93}$Nb system at energies close to the Coulomb barrier. The cross sections for $\\alpha+\\alpha$ events from one proton pickup were found to be smaller than those for $\\alpha+d$ events from one neutron stripping and $\\alpha+t$ events from direct breakup of $^7$Li. Coupled channels Born approximation and continuum discretized coupled channels calculations describe the data well and support the conclusion that the $\\alpha+d$ and $\\alpha+\\alpha$ events are produced by direct transfer to unbound states of the ejectile.

  7. Role of the cluster structure of $^7$Li in the dynamics of fragment capture

    CERN Document Server

    Shrivastava, A; Diaz-Torres, A; Nanal, V; Ramachandran, K; Rejmund, M; Bhattacharyya, S; Chatterjee, A; Kailas, S; Lemasson, A; Palit, R; Parkar, V V; Pillay, R G; Rout, P C; Sawant, Y

    2012-01-01

    Exclusive measurements of prompt $\\gamma$-rays from the heavy-residues with various light charged particles in the $^7$Li + $^{198}$Pt system, at an energy near the Coulomb barrier (E/$V_b$ $\\sim$ 1.6) are reported. Recent dynamic classical trajectory calculations, constrained by the measured fusion, $\\alpha$ and $t$ capture cross-sections have been used to explain the excitation energy dependence of the residue cross-sections. These calculations distinctly illustrate a two step process, breakup followed by fusion in case of the capture of $t$ and $\\alpha$ clusters; whereas for $^{6}$He + $p$ and $^{5}$He + $d$ configurations, massive transfer is inferred to be the dominant mechanism. The present work clearly demonstrates the role played by the cluster structures of $^7$Li in understanding the reaction dynamics at energies around the Coulomb barrier.

  8. Role of the cluster structure of {sup 7}Li in the dynamics of fragment capture

    Energy Technology Data Exchange (ETDEWEB)

    Shrivastava, A., E-mail: aradhana@barc.gov.in [Nuclear Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Navin, A. [GANIL, CEA/DSM - CNRS/IN2P3, Bd Henri Becquerel, BP 55027, F-14076 Caen Cedex 5 (France); Diaz-Torres, A. [ECT, Villa Tambosi, I-38123 Villazzano, Trento (Italy); Nanal, V. [DNAP, Tata Institute of Fundamental Research, Mumbai 400005 (India); Ramachandran, K. [Nuclear Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Rejmund, M. [GANIL, CEA/DSM - CNRS/IN2P3, Bd Henri Becquerel, BP 55027, F-14076 Caen Cedex 5 (France); Bhattacharyya, S. [Variable Energy Cyclotron Centre, 1/AF Bidhan Nagar, Kolkata 700064 (India); Chatterjee, A.; Kailas, S. [Nuclear Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Lemasson, A. [GANIL, CEA/DSM - CNRS/IN2P3, Bd Henri Becquerel, BP 55027, F-14076 Caen Cedex 5 (France); Palit, R. [DNAP, Tata Institute of Fundamental Research, Mumbai 400005 (India); Parkar, V.V. [Nuclear Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Pillay, R.G. [DNAP, Tata Institute of Fundamental Research, Mumbai 400005 (India); Rout, P.C. [Nuclear Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Sawant, Y. [DNAP, Tata Institute of Fundamental Research, Mumbai 400005 (India)

    2013-01-08

    Exclusive measurements of prompt {gamma}-rays from the heavy-residues with various light charged particles in the {sup 7}Li + {sup 198}Pt system, at an energy near the Coulomb barrier (E/V{sub b}{approx}1.6) are reported. Recent dynamic classical trajectory calculations, constrained by the measured fusion, {alpha}- and t-capture cross-sections have been used to explain the excitation energy dependence of the residue cross-sections. These calculations distinctly illustrate a two-step process, breakup followed by fusion, in case of the capture of t and {alpha} clusters; whereas for {sup 6}He+p and {sup 5}He+d configurations, massive transfer is inferred to be the dominant mechanism. The present work clearly demonstrates the role played by the cluster structures of {sup 7}Li in understanding the reaction dynamics at energies around the Coulomb barrier.

  9. New measurement of the 10B(n,α)7 Li through the Trojan Horse Method

    Science.gov (United States)

    Spartá, Roberta

    2016-04-01

    B(n,α) Li reaction cross section has been measured using the Trojan Horse method, with the specific aim to separate the α1 contribution (coming from the first Li excited level) by the αo (related to the Li ground state), using a very thin target. Preliminary results are shown of the three-body B(d,α7 Li)H cross section.

  10. In-beam PET measurement of $^{7}Li^{3+}$ irradiation induced $\\beta^+}$-activity

    CERN Document Server

    Priegnitz, M; Parodi, K; Sommerer, F; Fiedler, F; Enghardt, W

    2008-01-01

    At present positron emission tomography (PET) is the only feasible method of an in situ and non-invasive monitoring of patient irradiation with ions. At the experimental carbon ion treatment facility of the Gesellschaft für Schwerionenforschung (GSI) Darmstadt an in-beam PET scanner has been integrated into the treatment site and lead to a considerable quality improvement of the therapy. Since ions other than carbon are expected to come into operation in future patient treatment facilities, it is highly desirable to extend in-beam PET also to other therapeutic relevant ions, e.g. 7Li. Therefore, by means of the in-beam PET scanner at GSI the β+-activity induced by 7Li3+ ions has been investigated for the first time. Targets of PMMA, water, graphite and polyethylene were irradiated with monoenergetic, pencil-like beams of 7Li3+ with energies between 129.1 A MeV and 205.3 A MeV and intensities ranging from 3.0 × 107 to 1.9 × 108 ions s−1. This paper presents the measured β+-activity profiles as well as d...

  11. Line shift, line asymmetry, and the 6Li/7Li isotopic ratio determination

    CERN Document Server

    Cayrel, Roger; Chand, Hum; Bonifacio, Piercarlo; Spite, Monique; Spite, François; Petitjean, Patrick; Ludwig, Hans-Günter; Caffau, Elisabetta

    2007-01-01

    Context: Line asymmetries are generated by convective Doppler shifts in stellar atmospheres, especially in metal-poor stars, where convective motions penetrate to higher atmospheric levels. Such asymmetries are usually neglected in abundance analyses. The determination of the 6Li/7Li isotopic ratio is prone to suffering from such asymmetries, as the contribution of 6Li is a slight blending reinforcement of the red wing of each component of the corresponding 7Li line, with respect to its blue wing. Aims: The present paper studies the halo star HD 74000 and estimates the impact of convection-related asymmetries on the Li isotopic ratio determination. Method: Two methods are used to meet this aim. The first, which is purely empirical, consists in deriving a template profile from another element that can be assumed to originate in the same stellar atmospheric layers as Li I, producing absorption lines of approximately the same equivalent width as individual components of the 7Li I resonance line. The second metho...

  12. In situ 7Li and 133Cs nuclear magnetic resonance investigations on the role of Cs+ additive in lithium-metal deposition process

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Zhao, Zhenchao; Hu, Mary Y.; Feng, Ju; Deng, Xuchu; Chen, Xilin; Xu, Wu; Liu, Jun; Zhang, Ji-Guang

    2016-02-01

    Application of Li metal electrode in rechargeable lithium battery is hindered by safety concerns due to dendritic growth on the electrode over several charge-discharge cycles. We have found previously that adding low concentration Cs+ in electrolytes can promote smooth deposition of lithium onto metal electrode during repeated charge-discharge cycling using idea Li|Cu battery without the using of a separator. In this work, quantitative in situ 7Li and 133Cs NMR investigations using real planar symmetric lithium battery cells with and without Cs+ additives were carried out. It is found that the deposited lithium atoms on electrodes are highly porous. Detailed analysis of the data were carried out by separating the 7Li signal from deposited lithium that was oriented parallel to the electrode surface with the signal from the Li-metal nanorodes oriented perpendicular or nearly perpendicular to the electrode surface. The results demonstrate that addition of Cs+ can significantly enhance both the formation of uniform Li nanorods, and the reversibility of electrode. In situ 133Cs NMR directly confirms that Cs+ migrates to the electrode to form a positively charged electrostatic shield during cycling process. Combining the quantitative analysis of the orientation dependent signals of deposited metal Li and previous ex-situ results, different Li deposition models are proposed. During cycling process, more “active” lithium participates in the Li transfer between the electrode and nanorods for the battery with Cs+, while for the battery without Cs+ more dead and thinker lithium rods are formed and Li transfer between dendrites from different electrodes dominates.

  13. Synergistic effect of the simultaneous chemometric analysis of {sup 1}H NMR spectroscopic and stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data: Application to wine analysis

    Energy Technology Data Exchange (ETDEWEB)

    Monakhova, Yulia B., E-mail: yul-monakhova@mail.ru [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, Saratov 410012 (Russian Federation); Godelmann, Rolf [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Hermann, Armin [Landesuntersuchungsamt -Institut für Lebensmittelchemie und Arzneimittelprüfung, Emy-Roeder-Straße 1, Mainz 55129 (Germany); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, Karlsruhe 76187 (Germany); Cannet, Claire; Schäfer, Hartmut; Spraul, Manfred [Bruker Biospin GmbH, Silberstreifen, Rheinstetten 76287 (Germany); Rutledge, Douglas N. [AgroParisTech, UMR 1145, Ingénierie Procédés Aliments, 16 rue Claude Bernard, Paris F-75005 (France)

    2014-06-23

    Highlights: • {sup 1}H NMR profilings of 718 wines were fused with stable isotope analysis data (SNIF-NMR, {sup 18}O, {sup 13}C). • The best improvement was obtained for prediction of the geographical origin of wine. • Certain enhancement was also obtained for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data). • Independent component analysis was used as an alternative chemometric tool for classification. - Abstract: It is known that {sup 1}H NMR spectroscopy represents a good tool for predicting the grape variety, the geographical origin, and the year of vintage of wine. In the present study we have shown that classification models can be improved when {sup 1}H NMR profiles are fused with stable isotope (SNIF-NMR, {sup 18}O, {sup 13}C) data. Variable selection based on clustering of latent variables was performed on {sup 1}H NMR data. Afterwards, the combined data of 718 wine samples from Germany were analyzed using linear discriminant analysis (LDA), partial least squares-discriminant analysis (PLS-DA), factorial discriminant analysis (FDA) and independent components analysis (ICA). Moreover, several specialized multiblock methods (common components and specific weights analysis (ComDim), consensus PCA and consensus PLS-DA) were applied to the data. The best improvement in comparison with {sup 1}H NMR data was obtained for prediction of the geographical origin (up to 100% for the fused data, whereas stable isotope data resulted only in 60–70% correct prediction and {sup 1}H NMR data alone in 82–89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for {sup 1}H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of {sup 1}H NMR data with stable isotope data improves efficiency of classification models for geographical origin and vintage of wine and can be potentially used for other food products as well.

  14. Molecular structure, spectroscopic (FT-IR, FT Raman, UV, NMR and THz) investigation and hyperpolarizability studies of 3-(2-Chloro-6-fluorophenyl)-1-(2-thienyl) prop-2-en-1-one

    Science.gov (United States)

    Kumar, Rajesh; Kumar, Amit; Deval, Vipin; Gupta, Archana; Tandon, Poonam; Patil, P. S.; Deshmukh, Prathmesh; Chaturvedi, Deepika; Watve, J. G.

    2017-02-01

    In the present work, a combined experimental and theoretical study on ground state molecular structure, spectroscopic and nonlinear optical properties of the chalcone derivative 3-(2-Chloro-6-fluorophenyl)-1-(2-thienyl) prop-2-en-1-one (2C6F2SC) is reported. Initial geometry generated from single crystal X-ray diffraction parameters was minimized at DFT level employing B3LYP/6-311++G (d,p) without any constraint to the potential energy surface. The molecule has been characterized using various experimental techniques FT-IR, FT-Raman, UV-Vis, 1H NMR, TD-THz and the spectroscopic data have been analyzed theoretically by Density Functional Theory (DFT) method. Harmonic vibrational frequencies were calculated theoretically using the optimized ground state geometry and the spectra were interpreted by means of potential energy distribution. Time Dependent Density Functional Theory (TD-DFT) has been used to calculate energies, absorption wavelengths, oscillator strengths of electronic singlet-singlet transitions. The calculated energy and oscillator strength complement with the experimental findings. The HOMO-LUMO energy gap explains the charge interaction taking place within the molecule. Good correlations between the experimental 1H NMR chemical shifts and calculated GIAO shielding tensors were found. Stability of the molecule, hyperconjugative interactions and charge delocalization has been analyzed by natural bond orbital (NBO) analysis. The first order hyperpolarizability (β) of this molecular system and related properties (μ, and Δα) have been calculated using the finite-field approach.

  15. Trials for the cosmological 7Li problem with 7Be beams at CRIB and collaborating studies

    Science.gov (United States)

    Hayakawa, S.

    2017-09-01

    For many years, the cosmological ^7 Li problem has been tackled from various aspects. The nuclear reaction data have also been improved, but still there remains some ambiguities. We review our experimental plans to measure the cross sections of three key reactions which act to destroy ^7 Be during the Big-Bang Nucleosynthesis (BBN). These experiments are all based on ^7 Be beams produced at Center-for-Nuclear-Study Radioactive Ion Beam separator (CRIB) in collaborations mainly with research groups from INFN-LNS and RCNP. The preliminary result of the previous experiment and the future plan are discussed.

  16. Angular Distribution of the 12C(6He, 7Li)11B Reaction

    Institute of Scientific and Technical Information of China (English)

    LI Er-Tao; LI Zhi-Hong; LI Yun-Ju; YAN Sheng-Quan; BAI Xi-Xiang; GUO Bing; SU Jun; WANG You-Bao; WANG Bao-Xiang; LIAN Gang; ZENG Sheng; FANG Xiao; ZHAO Wei-Juan; LIU Wei-Ping

    2009-01-01

    Angular distribution of the 12C(6He, 7Li)11B transfer reaction is measured with a secondary 6He beam of 36.4 Me V for the first time. The experimental angular distribution is well reproduced by the distorted-wave Born approxima-tion (DWBA) calculation. The success of the present experiment shows that it is feasible to measure one-nucleon transfer reaction on a light nucleus target with the secondary beam facility of the HI-13 tandem accelerator at China Institute of Atomic Energy (CIAE), Beifing.

  17. Corrosion barriers processed by Al electroplating and their resistance against flowing Pb–15.7Li

    Energy Technology Data Exchange (ETDEWEB)

    Krauss, Wolfgang, E-mail: wolfgang.krauss@kit.edu; Konys, Jürgen; Wulf, Sven-Erik

    2014-12-15

    In the HCLL blanket design, ferritic–martensitic steels are in direct contact with the flowing liquid breeder Pb–15.7Li and have to withstand severe corrosion attack. Beyond corrosion, T-permeation from the breeder into the RAFM-steels is also an important issue and has to be reduced significantly. Earlier work showed that Al-based coatings can act as barriers for both, however, applied processes e.g. HDA or VPS exhibited strong drawbacks in the past. Meanwhile new industrial relevant coating processes, using electroplating technology are under development and called ECA (electrochemical aluminization) and ECX (electrochemical deposition from ionic liquids) process. In this study electrochemically Al-coated and heat-treated Eurofer samples were tested in PICOLO loop for exposure times up to 12,000 h (ECA) and 2000 h (first results ECX) respectively to determine corrosion properties in flowing Pb–15.7Li (550 °C, 0.1 m/s). Cross section analysis afterward corrosion testing proved the ability of thin Al-based barriers made by electrochemical techniques to protect the bare Eurofer from corrosion attack even at exposure times of 12,000 h. Determined radial corrosion rates lay between 10 and 20 μm/a. First results for ECX coated samples (2000 h) revealed more homogeneous corrosion behavior of the barrier layer itself compared to ECA.

  18. Quality of sour cherry juice of different clones and cultivars (Prunus cerasus L.) determined by a combined sensory and NMR spectroscopic approach

    DEFF Research Database (Denmark)

    Clausen, Morten Rahr; Pedersen, Bjarne Hjelmsted; Bertram, Hanne Christine S.

    2011-01-01

    Juice was manufactured from seven different sour cherry clones/cultivars and evaluated by quantitative descriptive sensory analysis and 1H NMR spectroscopy. The sensory evaluation showed a large variation in several sensory attributes between the sour cherry clones/cultivars, which could be divid...

  19. Spectroscopic (FT-IR, FT-Raman, 1H, 13C NMR, UV/VIS), thermogravimetric and antimicrobial studies of Ca(II), Mn(II), Cu(II), Zn(II) and Cd(II) complexes of ferulic acid

    Science.gov (United States)

    Kalinowska, M.; Piekut, J.; Bruss, A.; Follet, C.; Sienkiewicz-Gromiuk, J.; Świsłocka, R.; Rzączyńska, Z.; Lewandowski, W.

    2014-03-01

    The molecular structure of Mn(II), Cu(II), Zn(II), Cd(II) and Ca(II) ferulates (4-hydroxy-3-methoxycinnamates) was studied. The selected metal ferulates were synthesized. Their composition was established by means of elementary and thermogravimetric analysis. The following spectroscopic methods were used: infrared (FT-IR), Raman (FT-Raman), nuclear magnetic resonance (13C, 1H NMR) and ultraviolet-visible (UV/VIS). On the basis of obtained results the electronic charge distribution in studied metal complexes in comparison with ferulic acid molecule was discussed. The microbiological study of ferulic acid and ferulates toward Escherichia coli, Bacillus subtilis, Candida albicans, Pseudomonas aeruginosa, Staphylococcus aureus and Proteus vulgaris was done.

  20. Microscale Syntheses, Reactions, and 1H NMR Spectroscopic Investigations of Square Planar Macrocyclic Tetraamido-N Cu(III) Complexes Relevant to Green Chemistry

    Science.gov (United States)

    Uffelman, Erich S.; Doherty, Jonathan R.; Schulze, Carl; Burke, Amy L.; Bonnema, Kristen R.; Watson, Tanya T.; Lee, Daniel W., III

    2004-01-01

    Microscale fusions, description, and spectroscopic analysis of the reactivity of a square planar Cu(III) complex significant to green chemistry, are presented. The experiment also includes nine focal points on which pre-lab and post-lab questions are based, and the final exams reflect the students' comprehension of these and other features of…

  1. Lanthanide paramagnetic probes for NMR spectroscopic studies of fast molecular conformational dynamics and temperature control. Effective six-site proton exchange in 18-crown-6 by exchange spectroscopy.

    Science.gov (United States)

    Babailov, Sergey P

    2012-02-06

    (1)H and (13)C NMR measurements are reported for the CDCl(3) and CD(2)Cl(2) solutions of [La(18-crown-6)(NO(3))(3)] (I), [Pr(18-crown-6) (NO(3))(3)] (II), [Ce(18-crown-6)(NO(3))(3)] (III), and [Nd(18-crown-6)(NO(3))(3)] (IV) complexes. Temperature dependencies of the (1)H NMR spectra of paramagnetic II-IV have been analyzed using the dynamic NMR (DNMR) methods for six-site exchange. Two types of conformational dynamic processes were identified (the first one is conditioned by interconversion of complex enantiomeric forms and pseudorotation of a macrocycle molecule upon the C(2) symmetry axis; the second one is conditioned by macrocycle molecule inversion). Application of exchange spectroscopy (2D-EXSY) of DNMR for investigation of this dynamic system (II-IV) simplifies the assignment of the NMR signals and represents the first experimental study of multisite exchange. In the present work, the methodology of paramagnetic 4f (Ce, Pr, and Nd) probe applications for the study of free-energy, enthalpy, and entropy changes in chemical exchange processes, as well as the advantages of this method in a comparison with DNMR studies of diamagnetic substances, is discussed. In particular, as a result of paramagnetic chemical shifts in 4f complexes, the range of measurable rate constants expands considerably compared to the analogous range in diamagnetic compounds. Coordination compounds investigated in the paper represent new types of thermometric NMR sensors and lanthanide paramagnetic probes for in situ temperature control in solution.

  2. Dynamics of fragment capture for cluster structures of weakly bound 7Li

    Directory of Open Access Journals (Sweden)

    Shrivastava A.

    2013-12-01

    Full Text Available Role of cluster structures of 7Li on reaction dynamics have been studied by performing exclusive measurements of prompt-γ rays from residues with scattered particles at energy, E/Vb = 1.6, with 198Pt target. Yields of the residues resulting after capture of t and 4,5,6He, corresponding to different excitation energies of the composite system were estimated. The results were compared with three body classical-dynamical model for breakup fusion, constrained by the measured fusion, α and t capture cross-sections. The cross-section of residues from capture of α and t agreed well with the prediction of the model showing dominance of the two step process - breakup fusion, while those from tightly bound 6He showed massive transfer to be the dominant mechanism.

  3. Fast neutron measurements with 7Li and 6Li enriched CLYC scintillators

    Science.gov (United States)

    Giaz, A.; Blasi, N.; Boiano, C.; Brambilla, S.; Camera, F.; Cattadori, C.; Ceruti, S.; Gramegna, F.; Marchi, T.; Mattei, I.; Mentana, A.; Million, B.; Pellegri, L.; Rebai, M.; Riboldi, S.; Salamida, F.; Tardocchi, M.

    2016-07-01

    The recently developed Cs2LiYCl6:Ce (CLYC) crystals are interesting scintillation detectors not only for their gamma energy resolution (<5% at 662 keV) but also for their capability to identify and measure the energy of both gamma rays and fast/thermal neutrons. The thermal neutrons were detected by the 6Li(n,α)t reaction while for the fast neutrons the 35Cl(n,p)35S and 35Cl(n,α)32P neutron-capture reactions were exploited. The energy of the outgoing proton or α particle scales linearly with the incident neutron energy. The kinetic energy of the fast neutrons can be measured using both the Time Of Flight (TOF) technique and using the CLYC energy signal. In this work, the response to monochromatic fast neutrons (1.9-3.8 MeV) of two CLYC 1″×1″ crystals was measured using both the TOF and the energy signal. The observables were combined to identify fast neutrons, to subtract the thermal neutron background and to identify different fast neutron-capture reactions on 35Cl, in other words to understand if the detected particle is an α or a proton. We performed a dedicated measurement at the CN accelerator facility of the INFN Legnaro National Laboratories (Italy), where the fast neutrons were produced by impinging a proton beam (4.5, 5.0 and 5.5 MeV) on a 7LiF target. We tested a CLYC detector 6Li-enriched at about 95%, which is ideal for thermal neutron measurements, in parallel with another CLYC detector 7Li-enriched at more than 99%, which is suitable for fast neutron measurements.

  4. Fast neutron measurements with {sup 7}Li and {sup 6}Li enriched CLYC scintillators

    Energy Technology Data Exchange (ETDEWEB)

    Giaz, A., E-mail: agnese.giaz@mi.infn.it [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Blasi, N.; Boiano, C.; Brambilla, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Camera, F. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Cattadori, C. [INFN sezione di Milano Bicocca, Piazza della Scienza 3, 20125 Milano (Italy); Ceruti, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Gramegna, F.; Marchi, T. [INFN Laboratori Nazionali di Legnaro, Viale dell’Università, 2, 35020 Legnaro, PD (Italy); Mattei, I. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Mentana, A. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Million, B.; Pellegri, L. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Rebai, M. [Università degli Studi di Milano Bicocca, Physics Department, Piazza della Scienza 3, 20126 Milano (Italy); Riboldi, S. [INFN Milano, Via Celoria 16, 20133 Milano (Italy); Università degli Studi di Milano, Physics Department, Via Celoria 16, 20133 Milano (Italy); Salamida, F. [INFN sezione di Milano Bicocca, Piazza della Scienza 3, 20125 Milano (Italy); Tardocchi, M. [Istituto di Fisica del Plasma, Associazione EURATOM-ENEA-CNR, Via R. Cozzi 53, 2015 Milano (Italy)

    2016-07-21

    The recently developed Cs{sub 2}LiYCl{sub 6}:Ce (CLYC) crystals are interesting scintillation detectors not only for their gamma energy resolution (<5% at 662 keV) but also for their capability to identify and measure the energy of both gamma rays and fast/thermal neutrons. The thermal neutrons were detected by the {sup 6}Li(n,α)t reaction while for the fast neutrons the {sup 35}Cl(n,p){sup 35}S and {sup 35}Cl(n,α){sup 32}P neutron-capture reactions were exploited. The energy of the outgoing proton or α particle scales linearly with the incident neutron energy. The kinetic energy of the fast neutrons can be measured using both the Time Of Flight (TOF) technique and using the CLYC energy signal. In this work, the response to monochromatic fast neutrons (1.9–3.8 MeV) of two CLYC 1″×1″ crystals was measured using both the TOF and the energy signal. The observables were combined to identify fast neutrons, to subtract the thermal neutron background and to identify different fast neutron-capture reactions on {sup 35}Cl, in other words to understand if the detected particle is an α or a proton. We performed a dedicated measurement at the CN accelerator facility of the INFN Legnaro National Laboratories (Italy), where the fast neutrons were produced by impinging a proton beam (4.5, 5.0 and 5.5 MeV) on a {sup 7}LiF target. We tested a CLYC detector {sup 6}Li-enriched at about 95%, which is ideal for thermal neutron measurements, in parallel with another CLYC detector {sup 7}Li-enriched at more than 99%, which is suitable for fast neutron measurements.

  5. Ab initio calculations on the a3∑+u state properties of dimer 7Li2

    Institute of Scientific and Technical Information of China (English)

    Shi De-Heng; Sun Jin-Feng; Zhu Zun-Lue; Liu Yu-Fang

    2007-01-01

    The comparison between single-point energy scanning (SPES) and geometry optimization (OPT) in determining the equilibrium geometry of the a3∑u+ state for 7Li2 is made at numerous basis sets such as 6-311++G(2df), cc-PVTZ,6-311++G(2df, p), 6-311G(3df,3pd), 6-311++G(2df,2pd), D95(3df, 3pd), 6-311++G, DGDZVP, 6-311++G(3df,2pd),6-311G(2df,2pd), D95V++, CEP-121G, 6-311++G(d,p), 6-311++G(2df, pd) and 6-311++G(3df,3pd) in full active space using a symmetry-adapted-cluster/ symmetry-adapted-cluster configuration-interaction (SAC/SAC-CI) method presented in Gaussian03 program package. The difference of the equilibrium geometries obtained by SPES and by OPT is reported. Analyses show that the results obtained by SPES are more reasonable than those obtained by OPT. We have calculated the complete potential energy curves at these sets over a wide internuclear distance range from about 3.0a0to 37.0a0, and the conclusion is that the basis set cc-PVTZ is the most suitable one. With the potential obtained at cc-PVTZ, the spectroscopic data (Te, De, Do, ωe, ωeχe, αe and Be) are computed and they are 1.006 eV, 338.71 cm-1,307.12 cm-1, 64.88 cm-1, 3.41 cm-1, 0.0187 cm-1 and 0.279 cm-1, respectively, which are in good agreement with recent measurements. The total 11 vibrational states are found at J=0. Their corresponding vibrational levels and classical turning points are computed and compared with available RKR data, and good agreement is found. One inertial rotation constant (By) and six centrifugal distortion constants (Dy Hv, Lv, My, Nv and Ov) are calculated.The scattering length is calculated to be -27.138a0, which is in good accord with the experimental data.

  6. An atomic beam of 6Li — 7Li for high resolution spectroscopy from matrix isolation sublimation

    Science.gov (United States)

    Oliveira, A. N.; Sacramento, R. L.; Silva, B. A.; Uhlmann, F. O.; Wolff, W.; Cesar, C. L.

    2016-07-01

    We propose the Matrix Isolation Sublimation (MlSu) technique for generating cold lithium atoms for the measurement of the 6Li - 7Li isotope shift in D1 and D2 transitions. The technique is capable of generating cold 6Li and 7Li beams at 4 K with forward velocity of 125 m/s. Using this beam we offer a distinguished source of lithium atoms for transitions measurements, adding a new possibility to make high resolution spectroscopy towards improving the experimental checks of the theory.

  7. Study of H/D exchange rates to derive the strength of intramolecular hydrogen bonds in halo substituted organic building blocks: An NMR spectroscopic investigation

    Science.gov (United States)

    Mishra, Sandeep Kumar; Suryaprakash, N.

    2015-10-01

    Rates of hydrogen/deuterium (H/D) exchange determined by 1H NMR spectroscopy are utilized to derive the strength of hydrogen bonds and to monitor the electronic effects in the site-specific halogen substituted benzamides and anilines. The theoretical fitting of the time dependent variation of the integral areas of 1H NMR resonances to the first order decay function permitted the determination of H/D exchange rate constants (k) and their precise half-lives (t1/2) with high degree of reproducibility. The comparative study also permitted the unambiguous determination of relative strength of hydrogen bonds and the contribution from electronic effects on the H/D exchange rate.

  8. Vibrational spectroscopic, 1H NMR and quantum chemical computational study of 4-hydroxy-2-oxo-1,2-dihydroquinoline-8-carboxylic acid.

    Science.gov (United States)

    Ulahannan, Rajeev T; Panicker, C Yohannan; Varghese, Hema Tresa; Van Alsenoy, C; Musiol, Robert; Jampilek, Josef; Anto, P L

    2014-01-01

    FT-IR, FT-Raman and (1)H NMR spectra of 4-hydroxy-2-oxo-1,2-dihydroquinoline-8-carboxylic acid were recorded and obtained data were confronted with the computed using Gaussian09 software package. DFT/B3LYP, B3PW91 calculations have been done using 6-31G* and SDD basis sets, to investigate the vibrational frequencies and geometrical parameters. The assignments of the normal modes are done by potential energy distribution (PED) calculations. The calculated first hyperpolarizability is comparable with the reported values of similar quinoline derivatives and is an attractive object for future studies of non-linear optics. The stability of the molecule arising from hyperconjugative interaction and charge delocalization has been analyzed using NBO analysis. MEP predicts the most reactive part in the molecule. The calculated (1)H NMR results are in good agreement with experimental data.

  9. Synthesis, spectroscopic investigations (X-ray, NMR and TD-DFT), antimicrobial activity and molecular docking of 2,6-bis(hydroxy(phenyl)methyl)cyclohexanone.

    Science.gov (United States)

    Barakat, Assem; Ghabbour, Hazem A; Al-Majid, Abdullah Mohammed; Soliman, Saied M; Ali, M; Mabkhot, Yahia Nasser; Shaik, Mohammed Rafi; Fun, Hoong-Kun

    2015-07-21

    The synthesis of 2,6-bis(hydroxy(phenyl)methyl)cyclohexanone 1 is described. The molecular structure of the title compound 1 was confirmed by NMR, FT-IR, MS, CHN microanalysis, and X-ray crystallography. The molecular structure was also investigated by a set of computational studies and found to be in good agreement with the experimental data obtained from the various spectrophotometric techniques. The antimicrobial activity and molecular docking of the synthesized compound was investigated.

  10. Crystallographic, spectroscopic (FTIR and NMR) and quantum computational calculation studies on bis(2-methoxy-4-((E)-prop-1-enyl)phenyl)oxalate

    Science.gov (United States)

    Ersanli, Cem Cüneyt; Kaya Kantar, Günay; Şaşmaz, Selami

    2017-09-01

    In this paper, we report first, a new synthesis of bis(2-methoxy-4-((E)-prop-1-enyl)phenyl)oxalate, namely, C22H22O6, (I). Then, we present detailed FTIR, 1H NMR, 13C NMR spectroscopies and single-crystal X-ray diffraction techniques, Hartree-Fock (HF) and Density Functional Theory (DFT) molecular orbital calculation study of the title compound. Compound (I) crystallizes in the monoclinic space group P21/c, with Z = 2 in cells with a = 6.3440(5)Å, b = 10.1098(9)Å, c = 16.1899(15)Å, V = 1035.65(16)Å3 and displays weak C-H⋯O intermolecular interaction which contributes to crystal packing. The molecular geometry was also calculated using the Gaussian03W software, and structure was optimized using the HF and DFT/B3LYP methods with the 6-31G(d,p) basis set at the ground state. The harmonic vibrational frequencies, 1H and 13C NMR chemical shifts of I were calculated using the same method with the 6-31G(d,p) basis set. The calculated results show that the predicted geometry can well reproduce structural parameters. The energetic behaviors of the title compound in solvent media were examined using the DFT/B3LYP method with the 6-31G(d,p) basis set applying the Polarizable Continuum Model (PCM). Besides, the frontier molecular orbitals (FMOs), Mulliken population method, natural population analysis (NPA), molecular electrostatic potential (MEP) map of the title compound were investigated by theoretical calculations. Based on vibrational analyses, the thermodynamic properties of I at different temperatures have been calculated, and corresponding relations between the properties and temperature have also been obtained.

  11. Spectroscopic [FT-IR and FT-Raman] and theoretical [UV-Visible and NMR] analysis on α-Methylstyrene by DFT calculations.

    Science.gov (United States)

    Karthikeyan, N; Joseph Prince, J; Ramalingam, S; Periandy, S

    2015-05-15

    In the present research work, the FT-IR, FT-Raman and (13)C and (1)H NMR spectra of the α-Methylstyrene were recorded. The observed fundamental frequencies in finger print as well as functional group regions were assigned according to their uniqueness region. The Gaussian computational calculations are carried out by HF and DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The impact of the presence of vinyl group in phenyl structure of the compound is investigated. The modified vibrational pattern of the molecule associated vinyl group was analyzed. Moreover, (13)C NMR and (1)H NMR were calculated by using the gauge independent atomic orbital (GIAO) method with B3LYP methods and the 6-311++G(d,p) basis set and their spectra were simulated and the chemical shifts linked to TMS were compared. A study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies were carried out. The kubo gap of the present compound was calculated related to HOMO and LUMO energies which confirm the occurring of charge transformation between the base and ligand. Besides frontier molecular orbitals (FMO), molecular electrostatic potential (MEP) was performed. The NLO properties related to Polarizability and hyperpolarizability based on the finite-field approach were also discussed. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

  12. Chromatographic, NMR and vibrational spectroscopic investigations of astaxanthin esters: application to "Astaxanthin-rich shrimp oil" obtained from processing of Nordic shrimps.

    Science.gov (United States)

    Subramanian, B; Thibault, M-H; Djaoued, Y; Pelletier, C; Touaibia, M; Tchoukanova, N

    2015-11-01

    Astaxanthin (ASTX) is a keto carotenoid, which possesses a non-polar linear central conjugated chain and polar β-ionone rings with ketone and hydroxyl groups at the extreme ends. It is well known as a super anti-oxidant, and recent clinical studies have established its nutritional benefits. Although it occurs in several forms, including free molecule, crystalline, aggregates and various geometrical isomers, in nature it exists primarily in the form of esters. Marine animals accumulate ASTX from primary sources such as algae. Nordic shrimps (P. borealis), which are harvested widely in the Atlantic Ocean, form a major source of astaxanthin esters. "Astaxanthin-rich shrimp oil" was developed as a novel product in a shrimp processing plant in Eastern Canada. A compositional analysis of the shrimp oil was performed, with a view to possibly use it as a nutraceutical product for humans and animals. Astaxanthin-rich shrimp oil contains 50% MUFAs and 22% PUFAs, of which 20% are omega-3. In addition, the shrimp oil contains interesting amounts of EPA and DHA, with 10%/w and 8%/w, respectively. Astaxanthin concentrations varied between 400 and 1000 ppm, depending on the harvesting season of the shrimp. Astaxanthin and its esters were isolated from the oil and analysed by NMR, FTIR and Micro-Raman spectroscopy. Astaxanthin mono- and diesters were synthesized and used as standards for the analysis of astaxanthin-rich shrimp oil. NMR and vibrational spectroscopy techniques were successfully used for the rapid characterization of monoesters and diesters of astaxanthin. Raman spectroscopy provided important intermolecular interactions present in the esterified forms of astaxanthin molecules. Also discussed in this paper is the use of NMR, FTIR and Micro-Raman spectroscopy for the detection of astaxanthin esters in shrimp oil.

  13. (1)H NMR spectroscopic elucidation in solution of the kinetics and thermodynamics of spin crossover for an exceptionally robust Fe(2+) complex.

    Science.gov (United States)

    Petzold, Holm; Djomgoue, Paul; Hörner, Gerald; Speck, J Matthäus; Rüffer, Tobias; Schaarschmidt, Dieter

    2016-09-21

    A series of Fe(2+) spin crossover (SCO) complexes [Fe(5/6)](2+) employing hexadentate ligands (5/6) with cis/trans-1,2-diamino cyclohexanes (4) as central building blocks were synthesised. The ligands were obtained by reductive amination of 4 with 2,2'-bipyridyl-6-carbaldehyde or 1,10-phenanthroline-2-carbaldehyde 3. The chelating effect and the rigid structure of the ligands 5/6 lead to exceptionally robust Fe(2+) and Zn(2+) complexes conserving their structure even in coordinating solvents like dmso at high temperatures. Their solution behavior was investigated using variable temperature (VT) (1)H NMR spectroscopy and VT Vis spectroscopy. SCO behavior was found for all Fe(2+) complexes in this series centred around and far above room temperature. For the first time we have demonstrated that the thermodynamics as well as kinetics for SCO can be deduced by using VT (1)H NMR spectroscopy. An alternative scheme using a linear correction term C(1) to model chemical shifts for Fe(2+) SCO complexes is presented. The rate constant for the SCO of [Fe(rac-trans-5)](2+) obtained by VT (1)H NMR was validated by Laser Flash Photolysis (LFP), with excellent agreement (1/(kHL + kLH) = 33.7/35.8 ns for NMR/LFP). The solvent dependence of the transition temperature T1/2 and the solvatochromism of complex [Fe(rac-trans-5)](2+) were ascribed to hydrogen bond formation of the secondary amine to the solvent. Enantiomerically pure complexes can be prepared starting with R,R- or S,S-1,2-diaminocyclohexane (R,R-trans-4 or S,S-trans-4). The high robustness of the complexes reduces a possible ligand scrambling and allows preparation of quasiracemic crystals of [Zn(R,R-5)][Fe(S,S-5)](ClO4)4·(CH3CN) composed of a 1 : 1 mixture of the Zn and Fe complexes with inverse chirality.

  14. Metal Carbonation of Forsterite in Supercritical CO2 and H2O Using Solid State 29Si, 13C NMR Spectroscop

    Energy Technology Data Exchange (ETDEWEB)

    Kwak, Ja Hun; Hu, Jian Z.; Hoyt, David W.; Sears, Jesse A.; Wang, Chong M.; Rosso, Kevin M.; Felmy, Andrew R.

    2010-03-11

    Ex situ solid state NMR was used for the first time to study fundamental mineral carbonation processes and reaction extent relevant to geologic carbon sequestration (GCS) using a model silicate mineral forsterite (Mg2SiO4)+supercriticalCO2 with and without H2O. Run conditions were 80 C and 96 atm. 29Si NMR clearly shows that in the absence of CO2, the role of H2O is to hydrolyze surface Mg-O-Si bonds to produce dissolved Mg2+, and mono- and oligomeric hydroxylated silica species. Surface hydrolysis products contain only Q0 (Si(OH)4) and Q1(Si(OH)3OSi) species. An equilibrium between Q0, Q1 and Mg2+ with a saturated concentration equivalent to less than 3.2% of the Mg2SiO4 conversion is obtained at a reaction time of up to 7 days. Using scCO2 without H2O, no reaction is observed within 7 days. Using both scCO2 and H2O, the surface reaction products for silica are mainly Q3 (SiOH(OSi)3) species accompanied by a lesser amount of Q2 (Si(OH)2(OSi)2) and Q4 (Si(OSi)4). However, no Q0 and Q1 were detected, indicating the carbonic acid formation/deprotonation and magnesite (MgCO3) precipitation reactions are faster than the forsterite hydrolysis process. Thus it can be concluded that the Mg2SiO4 hydrolysis process is the rate limiting step of the overall mineral carbonation process. 29Si NMR combined with XRD, TEM, SAED and EDX further reveal that the reaction is a surface reaction with the Mg2SiO4 crystallite in the core and with condensed Q2-Q4 species forming amorphous surface layers. 13C MAS NMR identified a possible reaction intermediate as (MgCO3)4-Mg(OH)2-5H2O. However, at long reaction times only crystallite magnesite MgCO3 products are observed.

  15. X-ray and 1H-NMR spectroscopic studies of the structures and conformations of the new nootropic agents RU-35929, RU-47010 and RU-35965

    Science.gov (United States)

    Amato, Maria E.; Bandoli, Giuliano; Casellato, Umberto; Pappalardo, Giuseppe C.; Toja, Emilio

    1990-10-01

    The crystal and molecular structures of the nootropics (±)1-benzenesulphonyl-2-oxo-5-ethoxypyrrolidine ( 1), (±)1-(3-pyridinylsulphonyl)-2-oxo-5-ethoxypyrrolidine ( 2) and (±)1-benzenesulphonyl-2-oxo-5-isopropyloxypyrrolidine ( 3) have been determined by X-ray analysis. The solution conformation of 1, 2 and 3 has been investigated by 1H NMR spectroscopy. In the solid state, the main feature consists of the similar structural parameters and conformations, with the exception of the conformation adopted by the 5-ethoxy moiety which changes on passing from 1 to 2. The solid state overall enveloped conformation of the 2-pyrrolidinone ring for the three nootropics is found to be retained in solution on the basis of NMR evidence. Comparison between calculated and experimental coupling constant values shows that one of the two possible puckered opposite conformational isomers (half-chair shapes) occurs in solution. The relative pharmacological potencies of 1, 2 and 3 cannot therefore be interpreted in terms of the different conformation features presently detectable by available experimental methods.

  16. Combined experimental and quantum chemical studies on spectroscopic (FT-IR, FT-Raman, UV-Vis, and NMR) and structural characteristics of quinoline-5-carboxaldehyde

    Science.gov (United States)

    Kumru, Mustafa; Altun, Ahmet; Kocademir, Mustafa; Küçük, Vesile; Bardakçı, Tayyibe; Şaşmaz, İbrahim

    2016-12-01

    Comparative experimental and theoretical studies have been performed on the structure and spectral (FT-IR, FT-Raman, UV-Vis and NMR) features of quinoline-5-carboxaldehyde. Quantum chemical calculations have been carried out at Hartree-Fock and density functional B3LYP levels with the triple-zeta 6-311++G** basis set. Two stable conformers of quinoline-5-carboxaldehyde arising from the orientation of the carboxaldehyde moiety have been located at the room temperature. The energetic separation of these conformers is as small as 2.5 kcal/mol with a low transition barrier (around 9 kcal/mol). Therefore, these conformers are expected to coexist at the room temperature. Several molecular characteristics of quinoline-5-carboxaldehyde obtained through B3LYP and time-dependent B3LYP calculations, such as conformational stability, key geometry parameters, vibrational frequencies, IR and Raman intensities, UV-Vis vertical excitation energies and the corresponding oscillator strengths have been analyzed. The 1H and 13C NMR chemical shifts of quinoline-5-carboxaldehyde were also investigated.

  17. Domain-specific interactions between MLN8237 and human serum albumin estimated by STD and WaterLOGSY NMR, ITC, spectroscopic, and docking techniques

    Science.gov (United States)

    Yang, Hongqin; Liu, Jiuyang; Huang, Yanmei; Gao, Rui; Tang, Bin; Li, Shanshan; He, Jiawei; Li, Hui

    2017-03-01

    Alisertib (MLN8237) is an orally administered inhibitor of Aurora A kinase. This small-molecule inhibitor is under clinical or pre-clinical phase for the treatment of advanced malignancies. The present study provides a detailed characterization of the interaction of MLN8237 with a drug transport protein called human serum albumin (HSA). STD and WaterLOGSY nuclear magnetic resonance (NMR)-binding studies were conducted first to confirm the binding of MLN8237 to HSA. In the ligand orientation assay, the binding sites of MLN8237 were validated through two site-specific spy molecules (warfarin sodium and ibuprofen, which are two known site-selective probes) by using STD and WaterLOGSY NMR competition techniques. These competition experiments demonstrate that both spy molecules do not compete with MLN8237 for the specific binding site. The AutoDock-based blind docking study recognizes the hydrophobic subdomain IB of the protein as the probable binding site for MLN8237. Thermodynamic investigations by isothermal titration calorimetry (ITC) reveal that the non-covalent interaction between MLN8237 and HSA (binding constant was approximately 105 M-1) is driven mainly by favorable entropy and unfavorable enthalpy. In addition, synchronous fluorescence, circular dichroism (CD), and 3D fluorescence spectroscopy suggest that MLN8237 may induce conformational changes in HSA.

  18. Inelastic neutron scattering cross-section measurements on 7Li and 63,65Cu

    Directory of Open Access Journals (Sweden)

    Nyman Markus

    2017-01-01

    Full Text Available The γ-ray production cross section for the 477.6-keV transition in 7Li following inelastic neutron scattering has been measured from the reaction threshold up to 18 MeV. This cross section is interesting as a possible standard for other inelastic scattering measurements. The experiment was conducted at the Geel Electron LINear Accelerator (GELINA pulsed white neutron source with the Gamma Array for Inelastic Neutron Scattering (GAINS spectrometer. Previous measurements of this cross section are reviewed and compared with our results. Recently, this cross section has also been calculated using the continuum discretized coupled-channels (CDCC method. Experiments for studying neutrinoless double-β decay (2β0ν or other very rare processes require greatly reducing the background radiation level (both intrinsic and external. Copper is a common shielding and structural material, used extensively in experiments such as COBRA, CUORE, EXO, GERDA, and MAJORANA. Understanding the background contribution arising from neutron interactions in Cu is important when searching for very weak experimental signals. Neutron inelastic scattering on natCu was investigated with GAINS. The results are compared with previous experimental data and evaluated nuclear data libraries.

  19. Coherent photoproduction of pi^0- and eta-mesons off 7Li

    CERN Document Server

    Maghrbi, Y; Ahrens, J; Annand, J R M; Arends, H J; Beck, R; Bekrenev, V; Boillat, B; Braghieri, A; Branford, D; Briscoe, W J; Brudvik, J; Cherepnya, S; Codling, R F B; Downie, E J; Drexler, P; Fil'kov, L V; Fix, A; Glazier, D I; Gregor, R; Heid, E; Hornidge, D; Jaegle, I; Jahn, O; Kashevarov, V L; Keshelashvili, I; Knezevic, A; Kondratiev, R; Korolija, M; Krambrich, D; Lang, M; Lisin, V; Livingston, K; Lugert, S; MacGregor, I J D; Manley, D M; Martinez, M; McGeorge, J C; Mekterovic, D; Metag, V; Nefkens, B M K; Nikolaev, A; Novotny, R; Ostrick, M; Pedroni, P; Pheron, F; Polonski, A; Prakhov, S; Price, J W; Rosner, G; Rost, M; Rostomyan, T; Schadmand, S; Schumann, S; Sober, D; Starostin, A; Supek, I; Tarbert, C M; Thomas, A; Unverzagt, M; Watts, D P; Werthmueller, D; Zehr, F

    2013-01-01

    Coherent photoproduction of $\\pi^0$-mesons from threshold ($E_{th} \\approx$ 136 MeV) throughout the $\\Delta$-resonance region and of $\\eta$-mesons close to the production threshold ($E_{th} \\approx$ 570 MeV for $\\eta$) has been measured for $^7$Li nuclei. The experiment was performed using the tagged-photon beam of the Mainz MAMI accelerator with the Crystal Ball and TAPS detectors combined to give an almost 4$\\pi$ solid-angle electromagnetic calorimeter. The reactions were identified by a combined invariant-mass and missing-energy analysis. A comparison of the pion data to plane-wave impulse modelling tests the nuclear mass form factor. So far coherent $\\eta$-production had been only identified for the lightest nuclear systems ($^2$H and $^3$He). For $^3$He a large enhancement of the cross section above plane-wave approximations had been reported, indicating the formation of a quasi-bound state. The present Li-data for $\\eta$-production agree with a plane-wave approximation. Contrary to $^3$He, neither a thr...

  20. Coherent photoproduction of {pi}{sup 0}- and {eta}-mesons off {sup 7}Li

    Energy Technology Data Exchange (ETDEWEB)

    Maghrbi, Y.; Krusche, B.; Boillat, B.; Jaegle, I.; Keshelashvili, I.; Pheron, F.; Werthmueller, D.; Zehr, F. [University of Basel, Department of Physics, Basel (Switzerland); Ahrens, J.; Arends, H.J.; Heid, E.; Jahn, O.; Krambrich, D.; Martinez, M.; Ostrick, M.; Rost, M.; Thomas, A. [University of Mainz, Institut fuer Kernphysik, Mainz (Germany); Annand, J.R.M.; Codling, R.F.B.; Livingston, K.; MacGregor, I.J.D.; McGeorge, J.C.; Rosner, G. [University of Glasgow, School of Physics and Astronomy, Glasgow (United Kingdom); Beck, R.; Lang, M.; Nikolaev, A.; Schumann, S.; Unverzagt, M. [University of Mainz, Institut fuer Kernphysik, Mainz (Germany); University of Bonn, Helmholtz-Institut fuer Strahlen- und Kernphysik, Bonn (Germany); Bekrenev, V. [Petersburg Nuclear Physics Institute, Gatchina (Russian Federation); Braghieri, A.; Pedroni, P.; Rostomyan, T. [INFN, Sezione di Pavia, Pavia (Italy); Branford, D.; Glazier, D.I.; Tarbert, C.M.; Watts, D.P. [University of Edinburgh, School of Physics, Edinburgh (United Kingdom); Briscoe, W.J. [The George Washington University, Center for Nuclear Studies, Washington, DC (United States); Brudvik, J.; Nefkens, B.M.K.; Prakhov, S.; Price, J.W.; Starostin, A. [University of California Los Angeles, Los Angeles, California (United States); Cherepnya, S.; Fil' kov, L.V. [Lebedev Physical Institute, Moscow (Russian Federation); Downie, E.J. [University of Mainz, Institut fuer Kernphysik, Mainz (Germany); University of Glasgow, School of Physics and Astronomy, Glasgow (United Kingdom); The George Washington University, Center for Nuclear Studies, Washington, DC (United States); Drexler, P.; Gregor, R.; Lugert, S.; Metag, V.; Novotny, R.; Schadmand, S. [University of Giessen, II. Physikalisches Institut, Giessen (Germany); Fix, A. [Tomsk Polytechnic University, Laboratory of Mathematical Physics, Tomsk (Russian Federation); Hornidge, D. [Mount Allison University, Sackville (Canada); Kashevarov, V.L. [University of Mainz, Institut fuer Kernphysik, Mainz (Germany); Lebedev Physical Institute, Moscow (Russian Federation); Knezevic, A.; Korolija, M.; Mekterovic, D.; Supek, I. [Rudjer Boskovic Institute, Zagreb (Croatia); Kondratiev, R.; Lisin, V.; Polonski, A. [Institute for Nuclear Research, Moscow (Russian Federation); Manley, D.M. [Kent State University, Kent, Ohio (United States); Sober, D. [The Catholic University of America, Washington, DC (United States); Collaboration: The Crystal Ball at MAMI, TAPS, and A2 Collaborations

    2013-03-15

    Coherent photoproduction of {pi}{sup 0}-mesons from threshold (E{sub th} {approx} 136 MeV) throughout the {Delta}-resonance region and of {eta}-mesons close to the production threshold (E{sub th} {approx} 570 MeV) for {eta} has been measured for {sup 7}Li nuclei. The experiment was performed using the tagged-photon beam of the Mainz MAMI accelerator with the Crystal Ball and TAPS detectors combined to give an almost 4 {pi} solid-angle electromagnetic calorimeter. The reactions were identified by a combined invariant-mass and missing-energy analysis. A comparison of the pion data to plane-wave impulse modelling tests the nuclear mass form factor. So far coherent {eta} production had been only identified for the lightest nuclear systems ({sup 2}H and {sup 3}He). For {sup 3}He a large enhancement of the cross section above plane-wave approximations had been reported, indicating the formation of a quasi-bound state. The present Li data for {eta} production agree with a plane-wave approximation. Contrary to {sup 3}He, neither a threshold enhancement of the total cross section nor a deviation of the angular distributions from the expected form factor dependence were observed. (orig.)

  1. Systematics of the breakup probability function for {sup 6}Li and {sup 7}Li projectiles

    Energy Technology Data Exchange (ETDEWEB)

    Capurro, O.A., E-mail: capurro@tandar.cnea.gov.ar [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); Pacheco, A.J.; Arazi, A. [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Carnelli, P.F.F. [CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Instituto de Investigación e Ingeniería Ambiental, Universidad Nacional de San Martín, 25 de Mayo y Francia, B1650BWA San Martín, Buenos Aires (Argentina); Fernández Niello, J.O. [Laboratorio TANDAR, Comisión Nacional de Energía Atómica, Av. General Paz 1499, B1650KNA San Martín, Buenos Aires (Argentina); CONICET, Av. Rivadavia 1917, C1033AAJ Buenos Aires (Argentina); Instituto de Investigación e Ingeniería Ambiental, Universidad Nacional de San Martín, 25 de Mayo y Francia, B1650BWA San Martín, Buenos Aires (Argentina); and others

    2016-01-15

    Experimental non-capture breakup cross sections can be used to determine the probability of projectile and ejectile fragmentation in nuclear reactions involving weakly bound nuclei. Recently, the probability of both type of dissociations has been analyzed in nuclear reactions involving {sup 9}Be projectiles onto various heavy targets at sub-barrier energies. In the present work we extend this kind of systematic analysis to the case of {sup 6}Li and {sup 7}Li projectiles with the purpose of investigating general features of projectile-like breakup probabilities for reactions induced by stable weakly bound nuclei. For that purpose we have obtained the probabilities of projectile and ejectile breakup for a large number of systems, starting from a compilation of the corresponding reported non-capture breakup cross sections. We parametrize the results in accordance with the previous studies for the case of beryllium projectiles, and we discuss their systematic behavior as a function of the projectile, the target mass and the reaction Q-value.

  2. Elastic scattering and fusion cross-sections in 7Li + 27Al reaction

    Indian Academy of Sciences (India)

    D Patel; S Santra; S Mukherjee; B K Nayak; P K Rath; V V Parkar; R K Choudhury

    2013-10-01

    With an aim to understand the effects of breakup and transfer channels on elastic scattering and fusion cross-sections in the 7Li + 27Al reaction, simultaneous measurement of elastic scattering angular distributions and fusion cross-sections have been carried out at various energies (lab = 8.0–16.0 MeV) around the Coulomb barrier. Optical model (OM) analysis of the elastic scattering data does not show any threshold anomaly or breakup threshold anomaly behaviour in the energy dependence of the real and imaginary parts of the OM potential. Fusion cross-section at each bombarding energy is extracted from the measured -particle evaporation energy spectra at backward angles by comparing with the statistical model prediction. Results on fusion cross-sections from the present measurements along with data from the literature have been compared with the coupled-channels predictions. Detailed coupled-channels calculations have been carried out to study the effect of coupling of breakup, inelastic and transfer, channels on elastic scattering and fusion. The effect of 1-stripping transfer coupling was found to be significant compared to that of the projectile breakup couplings in the present system.

  3. Design of a helix-bundle cross-link: NMR and UV-visible spectroscopic analyses and molecular modeling of ring-oxidized retinals.

    Science.gov (United States)

    Williams, T C; Mani, V

    1991-03-19

    In order to generate potential chemical cross-links for studying the chromophore binding site of bacteriorhodopsin and related helix-bundle proteins, MnO2 was used to oxidize all-trans-retinal's ring moiety. The structures and solution conformations of three ring-oxidized retinal analogues have been determined by using UV-visible absorption and 1H and 13C NMR spectroscopies, primarily with regard to (i) the introduction of a functional group at the ring end of the chromophore, (ii) the retention of the all-trans geometry of the polyenal side chain, and (iii) the torsional angle of the ring-polyenal bond. Analyses of their UV-visible absorption spectral parameters (lambda max, epsilon max, and vibrational fine structure) and NMR spectral parameters (1H-1H coupling constants, 1H and 13C NMR chemical shifts, and 1H homonuclear Overhauser effects) indicated the 4-oxo and the 2,3-dehydro-4-oxo derivatives both possess the twisted 6-s-cis conformation adopted by most six-membered ring analogues of retinal in solution or crystal. However, the alpha-dioxocyclopentenyl analogue exists in solution predominantly (70-80%) as the planar 6-s-trans conformer, similar to violerythrine chromophore analogues. In order to identify the minor solution forms, molecular modeling and geometry optimizations using the semiempirical molecular orbital method AM1 defined two additional symmetry-related minima at +/- 30-40 degrees in its C6-C7 torsional energy profile. Because the chromophores of bacterio- and halorhodopsins and sensory rhodopsins are bound as the 6-s-trans conformer [Harbison, G.S., Smith, S.O., Pardoen, J.A., Courtin, J.M.L., Lugtenburg, J., Herzfeld, J., Mathies, R.A., & Griffin, R.G. (1985) Biochemistry 24, 6955-6962; Baselt, D.R., Fodor, S.P.A., van der Steen, R., Lugtenburg, J., Bogomolni, R.A., & Mathies, R.A. (1989) Biophys. J. 55, 193-196], we suggest that the cyclopentenyl analogue's alpha-diketo function may be favorably positioned within the binding pocket and

  4. 13C-NMR spectroscopic evaluation of the citric acid cycle flux in conditions of high aspartate transaminase activity in glucose-perfused rat hearts.

    Science.gov (United States)

    Tran-Dinh, S; Hoerter, J A; Mateo, P; Gyppaz, F; Herve, M

    1998-12-01

    A new mathematical model, based on the observation of 13C-NMR spectra of two principal metabolites (glutamate and aspartate), was constructed to determine the citric acid cycle flux in the case of high aspartate transaminase activity leading to the formation of large amounts of labeled aspartate and glutamate. In this model, the labeling of glutamate and aspartate carbons by chemical and isotopic exchange with the citric acid cycle are considered to be interdependent. With [U-13C]Glc or [1,2-(13)C]acetate as a substrate, all glutamate and aspartate carbons can be labeled. The isotopic transformations of 32 glutamate isotopomers into 16 aspartate isotopomers or vice versa were studied using matrix operations; the results were compiled in two matrices. We showed how the flux constants of the citric acid cycle and the 13C-enrichment of acetyl-CoA can be deduced from 13C-NMR spectra of glutamate and/or aspartate. The citric acid cycle flux in beating Wistar rat hearts, aerobically perfused with [U-13C]glucose in the absence of insulin, was investigated by 13C-NMR spectroscopy. Surprisingly, aspartate instead of glutamate was found to be the most abundantly-labeled metabolite, indicating that aspartate transaminase (which catalyses the reversible reaction: (glutamate + oxaloacetate 2-oxoglutarate + aspartate) is highly active in the absence of insulin. The amount of aspartate was about two times larger than glutamate. The quantities of glutamate (G0) or aspartate (A0) were approximately the same for all hearts and remained constant during perfusion: G0 = (0.74 +/- 0.03) micromol/g; A0 = (1.49 +/- 0.05) micromol/g. The flux constants, i.e., the fraction of glutamate and aspartate in exchange with the citric acid cycle, were about 1.45 min(-1) and 0.72 min(-1), respectively; the flux of this cycle is about (1.07 +/- 0.02) micromol min(-1) g(-1). Excellent agreement between the computed and experimental data was obtained, showing that: i) in the absence of insulin, only 41

  5. Elastic and inelastic scattering of {sup 14}N ions by {sup 7}Li at 80 MeV (c.m. 26.7 MeV)

    Energy Technology Data Exchange (ETDEWEB)

    Rudchik, A.T.; Herashchenko, O.V.; Rudchik, A.A.; Mezhevych, S.Yu.; Mokhnach, A.V.; Pirnak, V.M.; Ponkratenko, O.A.; Ilyin, A.P.; Uleshchenko, V.V. [Institute for Nuclear Research, Kyiv (Ukraine); Kemper, K.W. [Florida State University, Physics Department, Tallahassee, Florida (United States); Rusek, K. [National Institute for Nuclear Research, Warsaw (Poland); Heavy Ion Laboratory of Warsaw University, Warsaw (Poland); Koshchy, E.I. [Kharkiv National University, Kharkiv (Ukraine); Kliczewski, S.; Siudak, R.; Szczurek, A. [H. Niewodniczanski Institute of Nuclear Physics, Cracow (Poland); Plujko, V.A. [Taras Shevchenko Kyiv National University, Kyiv (Ukraine); Choinski, J. [Heavy Ion Laboratory of Warsaw University, Warsaw (Poland); Stolarz, A. [National Institute for Nuclear Research, Warsaw (Poland)

    2014-10-15

    New angular distribution data for {sup 7}Li + {sup 14}N elastic and inelastic scattering at the energy E{sub lab} ({sup 14}N) = 80 MeV (c.m. 26.7MeV) are presented. The data were analyzed within the optical model and the coupled-reaction-channels method using a channels-coupling scheme that included the {sup 7}Li and {sup 14}N inelastic scattering channels, spin reorientations of {sup 7}Li and {sup 14}N as well as most important transfer reactions. The low-energy excited states of {sup 7}Li and {sup 14}N were assumed to be collective in nature. The {sup 7}Li + {sup 14}N potential parameters as well as deformation parameters of {sup 7}Li and {sup 14}N were deduced. The {sup 7}Li + {sup 14}N potential and the data were compared with those of {sup 6}Li + {sup 14}N to observe isotopic differences. The enhanced large-angle elastic and inelastic scattering data are shown to have a large contribution from the ground-state reorientation of {sup 7}Li. (orig.)

  6. Primidone--an antiepileptic drug--characterisation by quantum chemical and spectroscopic (FTIR, FT-Raman, 1H, 13C NMR and UV-Visible) investigations.

    Science.gov (United States)

    Arjunan, V; Santhanam, R; Subramanian, S; Mohan, S

    2013-05-15

    The solid phase FTIR and FT-Raman spectra of primidone were recorded in the regions 4000-400 cm(-1) and 4000-100 cm(-1), respectively. The vibrational spectra were analysed and the observed fundamentals were assigned and analysed. The experimental wavenumbers were compared with the theoretical scaled vibrational wavenumbers determined by DFT methods. The Raman intensities were also determined with B3LYP/6-31G(d,p) method. The total electron density and molecular electrostatic potential surface of the molecule were constructed by using B3LYP/6-311++G(d,p) method to display electrostatic potential (electron+nuclei) distribution. The HOMO and LUMO energies were measured. Natural bond orbital analysis of primidone has been performed to indicate the presence of intramolecular charge transfer. The (1)H and (13)C NMR spectra were recorded and the chemical shifts of the molecule were calculated. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. New organic single crystal of (benzylthio)acetic acid: Synthesis, crystal structure, spectroscopic (ATR-FTIR, 1H and 13C NMR) and thermal characterization

    Science.gov (United States)

    Sienkiewicz-Gromiuk, Justyna; Tarasiuk, Bogdan; Mazur, Liliana

    2016-04-01

    (Benzylthio)acetic acid (Hbta) was synthesized with 78% yield from benzyl chloride and thiourea as substrates. Well-shaped crystals of Hbta were grown by slow solvent evaporation technique from pure methanol. The compound was investigated by single-crystal X-ray and powder diffraction techniques and was also characterized by other analytical methods, like ATR-FTIR, 1H and 13C NMR and TG/DSC. The acid molecule adopts bent conformation in the solid state. The crystal structure of Hbta is stabilized by numerous intermolecular interactions, including O-H···O, C-H···O, C-H···S and C-H···π contacts. Thermal decomposition of the obtained material takes place above 150 °C.

  8. (1)H and (13)C NMR spectroscopic studies of hexane-extractable lipids from soils under shelterbelts of different age and composition of plants.

    Science.gov (United States)

    Szajdak, Lech Wojciech; Maryganova, Victoria; Skakovskii, Eugene; Tychinskaya, Ludmila

    2015-01-01

    Comparative study of the composition of lipids extracted with n-hexane from soils under shelterbelts of different age and composition of plants and adjoining cultivated fields in agrolandscape has been carried out with the application of (1)Н and (13)С NMR spectroscopy. The lipid content correlates with the organic carbon content in soils and is the highest in the soil under the 200-years old shelterbelt. The data received indicate that hexane-extractable lipids from the soil under the 200-years old shelterbelt have undergone the most significant biochemical and chemical transformations (oxidation, hydrolysis, polymerization) with the accumulation of resistant compounds and destruction of esters of o-phthalic acid as anthropogenic contaminants compared to the lipids from the soil under the 14-years old shelterbelt and soils of adjoining arable fields.

  9. Vibrational spectroscopic (FT-IR, FT-Raman, ¹H NMR and UV) investigations and computational study of 5-nitro-2-(4-nitrobenzyl) benzoxazole.

    Science.gov (United States)

    Bhagyasree, J B; Varghese, Hema Tresa; Panicker, C Yohannan; Samuel, Jadu; Van Alsenoy, Christian; Bolelli, Kayhan; Yildiz, Ilkay; Aki, Esin

    2013-02-01

    The optimized molecular structure, vibrational frequencies, corresponding vibrational assignments of 5-nitro-2-(4-nitrobenzyl) benzoxazole have been investigated experimentally and theoretically using Gaussian09 software package. Potential energy distribution of the normal modes of vibrations was done using GAR2PED program. The energy and oscillator strength calculated by time dependent density functional theory almost compliments with experimental findings. Gauge-including atomic orbital (1)H NMR chemical shifts calculations were carried out by using B3LYP functional with 6-31G basis set. The HOMO and LUMO analysis is used to determine the charge transfer within the molecule. The stability of the molecule arising from hyper-conjugative interaction and charge delocalization have been analyzed using NBO analysis. MEP was performed by the DFT method and the predicted infrared intensities and Raman activities have also been reported. The calculated geometrical parameters are in agreement with that of similar derivatives.

  10. Spectroscopic (FT-IR, FT-Raman, UV, NMR, NBO, NLO) investigation and molecular docking study of (R)-2-Methylamino-1-Phenylethanol (Halostachine)

    Science.gov (United States)

    Subashini, K.; Govindarajan, R.; Surendran, R.; Mukund, K.; Periandy, S.

    2016-12-01

    FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectra of (R)-2-Methylamino-1-Phenylethanol have been recorded in solid phase, 1H and 13C NMR in deuterated chloroform (CDCl3) phase and UV spectrum (200-400 nm) in solid phase and in ethanol solution. The different conformers of the compound and their minimum energies were studied by potential energy surface scan, using semi-empirical method PM6. The computed wavenumbers obtained from B3LYP and B3PW91 functionals along with 6-311++G (d, p) basis sets were scaled so as to agree with the experimental values and the scaling factors have been reported. All the fundamental modes have been assigned based on the potential energy distribution (PED) values and the structure of the molecule was analyzed in parameters like bond length, bond angle and dihedral angles through B3LYP and B3PW91 functionals along with 6-311++G(d,p) basis set. The values of dipole moment (μ), polarizability (α) and hyper polarizability (β) of the molecule were calculated using which, the non-linear optical property of the molecule has been discussed. The observed HOMO-LUMO mappings reveals the different charge transfer possibilities within the molecule. Natural Bond Orbital analysis was computed and possible transitions were correlated with the electronic transitions. Mulliken charges, electrostatic potential charges and natural charges are also predicted. The theoretical 1H and 13C NMR chemical shifts were computed using B3LYP functionals using 6-311++G (2d, p) basis sets. The temperature dependence of the thermodynamic properties; heat capacity, entropy and enthalpy for the title compound were also determined by B3LYP functionals with 6-311++G (d, p) basis set. Molecular docking study shows that the title compound might exhibit inhibitory activity against Bacillus anthracis (3V5O).

  11. FTIR, FTRaman, UV-Visible and NMR spectroscopic studies on 3,3‧,4,4‧-tetrachloroazoxybenzene, an azoxybenzene derivative with toxic effects

    Science.gov (United States)

    Castillo, María V.; Pergomet, Jorgelina L.; Carnavale, Gustavo A.; Davies, Lilian; Zinczuk, Juan; Brandán, Silvia Antonia

    2017-08-01

    We have synthesized 3,3‧,4,4‧ Tetrachloroazoxybenzene (TCAOB) and, later, characterized it by using infrared, Raman, 1H, 13C NMR and UV-visible spectroscopies. The structural, topological and vibrational properties of four Cis and three Trans isomers were theoretically predicted by using the hybrid B3LYP together with the 6-31G* and 6-311++G** basis sets. The 69 normal modes of vibration for all TCAOB isomers were assigned by using the scaled quantum mechanical force field (SQMFF) procedure and their experimental vibrational spectra and normal internal coordinates. The high stabilities of all Cis and Trans isomers are supported by the π→π*, n→σ*, n→π* and π*→π* electronic transitions calculated by NBO studies while the AIM analyses reveal for the Trans forms the existence of intra-molecular Csbnd H⋯O hydrogen bonds, as suggested by the broad IR band observed in the higher wavenumbers region. The low gap energy for the Trans I isomer supports their higher reactivity probably due to the repulsion of the more electronegative Cl and O atoms as a consequence of their proximities. In addition, the force constants for all Cis and Trans isomers were calculated by using both levels of theory. Here, the comparisons of the predicted IR, Raman, NMR and ultraviolet-visible spectra with the corresponding experimental ones demonstrate good concordances. The existence of the Ndbnd O groups in all TCAOB isomers support the differences in their properties, as compared with those reported for TCAB.

  12. Electronic [UV-Visible] and vibrational [FT-IR, FT-Raman] investigation and NMR-mass spectroscopic analysis of terephthalic acid using quantum Gaussian calculations.

    Science.gov (United States)

    Karthikeyan, N; Prince, J Joseph; Ramalingam, S; Periandy, S

    2015-03-15

    In this research work, the vibrational IR, polarization Raman, NMR and mass spectra of terephthalic acid (TA) were recorded. The observed fundamental peaks (IR, Raman) were assigned according to their distinctiveness region. The hybrid computational calculations were carried out for calculating geometrical and vibrational parameters by DFT (B3LYP and B3PW91) methods with 6-31++G(d,p) and 6-311++G(d,p) basis sets and the corresponding results were tabulated. The molecular mass spectral data related to base molecule and substitutional group of the compound was analyzed. The modification of the chemical property by the reaction mechanism of the injection of dicarboxylic group in the base molecule was investigated. The (13)C and (1)H NMR spectra were simulated by using the gauge independent atomic orbital (GIAO) method and the absolute chemical shifts related to TMS were compared with experimental spectra. The study on the electronic and optical properties; absorption wavelengths, excitation energy, dipole moment and frontier molecular orbital energies, were performed by hybrid Gaussian calculation methods. The orbital energies of different levels of HOMO and LUMO were calculated and the molecular orbital lobe overlapping showed the inter charge transformation between the base molecule and ligand group. From the frontier molecular orbitals (FMO), the possibility of electrophilic and nucleophilic hit also analyzed. The NLO activity of the title compound related to Polarizability and hyperpolarizability were also discussed. The present molecule was fragmented with respect to atomic mass and the mass variation depends on the substitutions have also been studied. Crown Copyright © 2014. Published by Elsevier B.V. All rights reserved.

  13. Structural and spectroscopic (UV-Vis, IR, Raman, and NMR) characteristics of anisaldehydes that are flavoring food additives: A density functional study in comparison with experiments

    Science.gov (United States)

    Altun, Ahmet; Swesi, O. A. A.; Alhatab, B. S. S.

    2017-01-01

    The molecular structures, vibrational spectra (IR and Raman), electronic spectra (UV-Vis and DOS), and NMR spectra (13C and 1H) of p-anisaldehyde, m-anisaldehyde, and o-anisaldehyde have been studied by using the B3LYP density functional and the 6-311++G** basis set. While p-anisaldehyde has been found to contain two stable conformers at room temperature, m-anisaldehyde and o-anisaldehyde contain four stable conformers. In agreement with the calculated ground-state energetics and small transition barriers, the comparison of the experimental and calculated spectra of the anisaldehydes indicates equilibrium between all conformers at room temperature. However, the two conformers of o-anisaldehyde, in which the methoxy group lies out of the ring plane, are too rare at the equilibrium. The equilibrium conditions of the conformers of the anisaldehyde isomers have been shown readily accessible through UV-Vis and 13C NMR spectral studies but requiring very detailed vibrational analyses. The effect of the solvent has been found to red-shift the electronic absorption bands and to make the anisaldehydes more reactive and soft. Molecular electrostatic potential maps of the anisaldehydes show that their oxygen atoms are the sites for nucleophilic reactivity. Compared with the most sophisticated NBO method, ESP charges have been found mostly reliable while Mulliken charges fail badly with the present large 6-311++G** basis set. The present calculations reproduce not only the experimental spectral characteristics of the anisaldehydes but also reveal their several structural features.

  14. A spectroscopic study of nicotine analogue 2-phenylpyrrolidine (PPD) using resonant two-photon ionization (R2PI), microwave, and 2D NMR techniques.

    Science.gov (United States)

    Martin, Danielle E; Robertson, Evan G; MacLellan, Jonathan G; Godfrey, Peter D; Thompson, Christopher D; Morrison, Richard J S

    2009-02-25

    Conformational preferences of the nicotine analogue 2-phenylpyrrolidine (PPD) have been studied in both gaseous and solution phases. Theoretical calculations at the MP2 and B3LYP levels point to 5-6 stable conformers which differ in three degrees of conformational freedom; torsion between the two rings, inversion at the pyrrolidine (PY) amine, and PY ring puckering, characterized using the Cremer-Pople definition for pseudorotation. Only one conformer has a trans arrangement between the amino hydrogen and the phenyl substituent. It is 6-8 kJ mol(-1) more stable than the cis conformers, has a perpendicular ring arrangement, and puckers at the nitrogen atom--similar to structures reported for nicotine. Resonant two-photon ionization (R2PI) data, including hole burn spectra, indicate only one conformer is present in the free jet expansion, and band contour analysis suggests assignment to the trans conformer. Confirmation was provided by microwave spectroscopy. Fifty-seven lines measured in the 48-72 GHz region were assigned to 206 b-type transitions and fitted to yield rotational constants within 2 MHz of MP2 values predicted for the trans conformer. The solution-phase conformers of PPD were studied using 1D and 2D (1)H NMR spectroscopy and solvent-based theoretical calculations. In marked contrast to the gas phase, NMR data reveals only cis conformers present in solution. Calculations confirm increased stability for these conformers when placed in simulated chloroform or water environments. Solvent molecules are believed to disrupt a crucial N...H(ortho) stabilizing interaction present within the trans conformer.

  15. Spectroscopic (FT-IR, FT-Raman, UV, NMR, NLO) investigation and molecular docking study of 1-(4-Methylbenzyl) piperazine

    Science.gov (United States)

    Subashini, K.; Periandy, S.

    2017-04-01

    The title compound, 1-(4-Methylbenzyl) piperazine, was analyzed by recording FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectra in solid phase, 1H and 13C NMR in CDCl3 (deuterated chloroform) and UV spectrum (200-400 nm) in solid phase and in ethanol solution. The different conformers of the compound and their minimum energies were studied by potential energy surface scan, using semi-empirical method PM6. Density functional theory (DFT) calculation with 6-311++G (d, p) basis set along with B3LYP and B3PW91 functionals have been used to compute ground state molecular geometries and vibrational frequencies. The assignments of the vibrational spectra have carried out with the help of Potential Energy distribution (PED) analysis. Factor group analysis has also been tabulated. Charge distribution, Frontier Molecular Orbitals, UV-Vis spectra, Molecular Electrostatic Potential (MEP) maps, Non-linear optical (NLO) property and thermodynamic properties of the title compound at different temperatures, were determined using B3LYP functional along with 6-311++G (d, p) basis set. The theoretical 1H and 13C NMR chemical shifts were computed using B3LYP functional with 6-311++G (2d, p) basis sets. Natural Bond orbital analysis were computed and possible transitions were correlated with the electronic transitions. The title compound not only exhibits appreciable dipole moment and hyper polarizability (indicating good NLO properties) but also forms a stable complex with Bacillus cereus, (2HUC), with binding affinity -6.7 kcal/mol through molecular docking, suggesting that, it might exhibit inhibitory activity against Bacillus cereus.

  16. Molecular structure, spectroscopic characterization (FT-IR, FT-Raman, UV and NMR), HOMO and LUMO analysis of 3-ethynylthiophene with DFT quantum chemical calculations

    Science.gov (United States)

    Karabacak, Mehmet; Bilgili, Sibel; Mavis, Tugba; Eskici, Mustafa; Atac, Ahmet

    2013-11-01

    In this work, FT-IR, FT-Raman, UV and NMR spectra of 3-ethynylthiophene (3-ETP, C6H4S) were carried out by using density functional theory DFT/B3LYP method with the 6-311++G(d,p), 6-311+G(d,p), 6-311G(d,p), 6-31++G(d,p), 6-31+G(d,p), 6-31G(d,p) basis sets. FT-IR and FT-Raman spectra were recorded in the regions of 3500-400 cm-1 and 3500-50 cm-1, respectively. The geometrical parameters, energies and wavenumbers were obtained and the complete assignments of fundamental vibrations were performed on the basis of the total energy distribution (TED) of the vibrational modes, calculated with scaled quantum mechanics (SQM) method and PQS program. The 1H, 13C and HMQC (1H-13C correlation) NMR spectra in chloroform (CDCl3) were recorded and calculated. The UV spectrum of investigated compound were recorded in the region of 200-400 nm in ethanol solution. The electronic properties, such as excitation energies, absorption wavelengths, HOMO and LUMO energies were performed by DFT/B3LYP approach and the results were compared with experimental observations. The thermodynamic properties such zero-point vibrational energy, thermal energy, specific heat capacity, rotational constants, entropy, and dipole moment of the studied compound were calculated. As a result, the calculated results were compared with the observed data and found to be in good agreement.

  17. Spectroscopic (FT-IR, FT-Raman, UV, NMR, NLO) investigation, molecular docking and molecular simulation dynamics on 1-Methyl-3-Phenylpiperazine

    Science.gov (United States)

    Subashini, K.; Periandy, S.

    2017-09-01

    The title compound was analyzed, by recording FT-IR (4000-400 cm-1) and FT-Raman (4000-100 cm-1) spectra in solid phase, 1H and 13C NMR in CDCl3 (deuterated chloroform) and UV spectrum (200-400 nm) in solid phase and in ethanol solution. Conformational analysis was done using semi-empirical method PM6. The computed wavenumbers obtained from B3LYP and B3PW91 functionals along with 6-311++G (d, p) basis sets were scaled so as to agree with the experimental values and the scaling factors have been reported. All fundamental modes have been assigned based on the potential energy distribution (PED) values and the structure of the molecule was analyzed in terms of parameters like bond length, bond angle and dihedral angles through B3LYP and B3PW91 functionals along with 6-311++G(d,p) basis set. The observed HOMO-LUMO mappings reveal the different charge transfer possibilities within the molecule. The percentage contribution of a group to each molecular orbital was calculated using Gauss Sum program. Natural bond orbital analysis was computed and possible transition were correlated with the electronic transitions. Mulliken charges, electrostatic potential charges and natural charges are also predicted. The theoretical 1H and 13C NMR chemical shifts were computed using B3LYP functionals using 6-311++G (2d, p) basis sets. The temperature dependence of the thermodynamic properties; heat capacity, entropy and enthalpy for the title compound were also determined by B3LYP functional with 6-311++G (d, p) basis set. Molecular docking study shows that the title compound might exhibit inhibitory activity against Clostridium botulinum (2J3X). The interaction of the ligand (title molecule) with 2J3X for 2 ns duration and radial distribution function have been observed through molecular dynamics simulations.

  18. NMR Studies of Lithium Iodide Based Solid Electrolytes

    DEFF Research Database (Denmark)

    Dupree, R.; Howells, R. J.; Hooper, A.

    1983-01-01

    In mixture of LiI with γAl2O3 the ionic conductivity is found to increase by up to three orders of magnitude over pure LiI. NMR measurements of7Li relaxation times were performed on both anhydrous LiI and a mixture of LiI with 30m/o γAl2O3. The relaxation is found to be purely dipolar in origin f...

  19. Validity test of the Trojan Horse Method applied to the {sup 7}Li+p{yields} {alpha}+{alpha} reaction via the {sup 3}He break-up

    Energy Technology Data Exchange (ETDEWEB)

    Tumino, A.; Spitaleri, C.; Sergi, M.L.; Cherubini, S.; La Cognata, M.; Lamia, L.; Romano, S.; Tudisco, S. [Universita di Catania, Dipartimento di Metodologie Fisiche e Chimiche per l' Ingegneria, Catania (Italy); INFN Laboratori Nazionali del Sud, Catania (Italy); Kroha, V.; Burjan, V.; Novac, J.; Vincour, J. [Nuclear Physics Institute of ASCR, Rez, Prague (Czech Republic); Fueloep, Z.; Somorjai, E. [Institute of Nuclear Research of Hungarian Academy of Sciences (ATOMKI), Debrecen (Hungary); Pizzone, R.G. [INFN Laboratori Nazionali del Sud, Catania (Italy)

    2006-03-15

    The Trojan Horse Method (THM) was applied to the {sup 3}He+{sup 7}Li interaction in order to investigate the quasi-free {sup 7}Li(p,{alpha}){sup 4}He reaction. The three-body experiment was performed at 33 MeV corresponding to a {sup 7}Li-p relative energy ranging from 50 keV to 7 MeV. The extracted {sup 7}Li(p,{alpha}){sup 4}He quasi-free cross-section was compared with the behavior of direct data, as well as with the result of a previous THM investigation on the {sup 7}Li(p,{alpha}){sup 4}He reaction off the neutron in {sup 2}H. A good agreement between data sets shows up throughout the energy range investigated, providing a very important validity test of the pole approximation for the THM. (orig.)

  20. NMR analysis of compositional heterogeneity in polysaccharides

    Science.gov (United States)

    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...

  1. Preparation and characterizations of SnO2 nanopowder and spectroscopic (FT-IR, FT-Raman, UV-Visible and NMR) analysis using HF and DFT calculations.

    Science.gov (United States)

    Ayeshamariam, A; Ramalingam, S; Bououdina, M; Jayachandran, M

    2014-01-24

    In this work, pure and singe phase SnO2 Nano powder is successfully prepared by simple sol-gel combustion route. The photo luminescence and XRD measurements are made and compared the geometrical parameters with calculated values. The FT-IR and FT-Raman spectra are recorded and the fundamental frequencies are assigned. The optimized parameters and the frequencies are calculated using HF and DFT (LSDA, B3LYP and B3PW91) theory in bulk phase of SnO2 and are compared with its Nano phase. The vibrational frequency pattern in nano phase gets realigned and the frequencies are shifted up to higher region of spectra when compared with bulk phase. The NMR and UV-Visible spectra are simulated and analyzed. Transmittance studies showed that the HOMO-LUMO band gap (Kubo gap) is reduced from 3.47 eV to 3.04 eV while it is heated up to 800°C. The Photoluminescence spectra of SnO2 powder showed a peak shift towards lower energy side with the change of Kubo gap from 3.73 eV to 3.229 eV for as-prepared and heated up to 800°C. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.

  2. Comprehensive quantum chemical and spectroscopic (FTIR, FT-Raman, 1H, 13C NMR) investigations of O-desmethyltramadol hydrochloride an active metabolite in tramadol - An analgesic drug

    Science.gov (United States)

    Arjunan, V.; Santhanam, R.; Marchewka, M. K.; Mohan, S.

    2014-03-01

    O-desmethyltramadol is one of the main metabolites of tramadol widely used clinically and has analgesic activity. The FTIR and FT-Raman spectra of O-desmethyl tramadol hydrochloride are recorded in the solid phase in the regions 4000-400 cm-1 and 4000-100 cm-1, respectively. The observed fundamentals are assigned to different normal modes of vibration. Theoretical studies have been performed as its hydrochloride salt. The structure of the compound has been optimised with B3LYP method using 6-31G** and cc-pVDZ basis sets. The optimised bond length and bond angles are correlated with the X-ray data. The experimental wavenumbers were compared with the scaled vibrational frequencies determined by DFT methods. The IR and Raman intensities are determined with B3LYP method using cc-pVDZ and 6-31G(d,p) basic sets. The total electron density and molecular electrostatic potential surfaces of the molecule are constructed by using B3LYP/cc-pVDZ method to display electrostatic potential (electron + nuclei) distribution. The electronic properties HOMO and LUMO energies were measured. Natural bond orbital analysis of O-desmethyltramadol hydrochloride has been performed to indicate the presence of intramolecular charge transfer. The 1H and 13C NMR chemical shifts of the molecule have been anlysed.

  3. Thermal, conductivity, NMR, and Raman spectroscopic measurements and phase diagram of the Cs2S2O7-CsHSO4 system

    DEFF Research Database (Denmark)

    Rasmussen, Søren Birk; Hama, Hind; Lapina, Olga;

    2003-01-01

    The conductivity of the binary system CS2S2O7-CsHSO4 has been measured at 20 different molten compositions in the full composition range and in the temperature range 430-750 K. From the obtained liquidus-solidus phase transition temperatures, the phase diagram has been constructed. It is of the s......The conductivity of the binary system CS2S2O7-CsHSO4 has been measured at 20 different molten compositions in the full composition range and in the temperature range 430-750 K. From the obtained liquidus-solidus phase transition temperatures, the phase diagram has been constructed...... from the NMR measurements on CsHSO4, CS2S2O7, and Cs2S2O7-CsHSO4 mixtures. For 11 selected compositions covering the entire composition range of the CS2S2O7-CsHSO4 binary system, the conductivity of the molten state has been expressed by equations of the form k(X) = A(X) + B(X)(T - T-m) + C(X)(T - T...

  4. Spectroscopic (FTIR, FT-Raman, UV and NMR) investigation and NLO, HOMO-LUMO, NBO analysis of 2-Benzylpyridine based on quantum chemical calculations.

    Science.gov (United States)

    Mathammal, R; Sudha, N; Guru Prasad, L; Ganga, N; Krishnakumar, V

    2015-02-25

    In this work, the vibrational characteristics of 2-Benzylpyridine have been investigated. The structure of the molecule has been optimized and the structural characteristics of the molecule have been determined by density functional theory B3LYP method with 6-31G(d,p) basis set. The infrared and Raman spectra have been simulated from calculated intensities. Both the experimental and theoretical vibrational data confirms the presence of functional groups in the title compound. The (1)H and (13)C NMR spectra were recorded and (1)H and (13)C nuclear magnetic resonance chemical shifts of the molecule were calculated using the gauge independent atomic orbital method. UV-Visible spectrum of the title compound was recorded in the region 190-1100 nm and the electronic properties HOMO and LUMO energies were calculated by CIS approach. Nonlinear optical and thermodynamic properties were interpreted. All the calculated results were compared with the available experimental data of the title molecule. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Hyperpolarized 89Y NMR spectroscopic detection of yttrium ion and DOTA macrocyclic ligand complexation: pH dependence and Y-DOTA intermediates

    Science.gov (United States)

    Ferguson, Sarah; Kiswandhi, Andhika; Niedbalski, Peter; Parish, Christopher; Kovacs, Zoltan; Lumata, Lloyd

    Dissolution dynamic nuclear polarization (DNP) is a rapidly emerging physics technique used to enhance the signal strength in nuclear magnetic resonance (NMR) and imaging (MRI) experiments for nuclear spins such as yttrium-89 by >10,000-fold. One of the most common and stable MRI contrast agents used in the clinic is Gd-DOTA. In this work, we have investigated the binding of the yttrium and DOTA ligand as a model for complexation of Gd ion and DOTA ligand. The macrocyclic ligand DOTA is special because its complexation with lanthanide ions such as Gd3+ or Y3+ is highly pH dependent. Using this physics technology, we have tracked the complexation kinetics of hyperpolarized Y-triflate and DOTA ligand in real-time and detected the Y-DOTA intermediates. Different kinds of buffers were used (lactate, acetate, citrate, oxalate) and the pseudo-first order complexation kinetic calculations will be discussed. The authors would like to acknowledge the support by US Dept of Defense Award No. W81XWH-14-1-0048 and Robert A. Welch Foundation Grant No. AT-1877.

  6. (19) F NMR Spectroscopic Analysis of the Binding Modes in Triple-Helical Peptide Nucleic Acid (PNA)/MicroRNA Complexes.

    Science.gov (United States)

    Tähtinen, Ville; Granqvist, Lotta; Murtola, Merita; Strömberg, Roger; Virta, Pasi

    2017-05-23

    Triplex-forming peptide nucleic acids (TFPNAs) were targeted to double-helical regions of (19) F-labeled RNA hairpin models (a UA-rich duplex with a hexaethylene glycol (heg) loop and a microRNA model, miR-215). In addition to conventional UV- and circular dichroism (CD)-based detection, binding was monitored by (19) F NMR spectroscopy. Detailed information on the stoichiometry and transition between the triple-helical peptide nucleic acid (PNA)/RNA and (PNA)2 /RNA binding modes could be obtained. γ-(R)-Hydroxymethyl-modified thymine-1-yl- and 2-aminopyridin-3-yl-acetyl derivatives of TFPNAs were additionally synthesized, which were targeted to the same RNA models, and the effect of the γ-(R)-hydroxymethyl group on binding was studied. An appropriate pattern of γ-(R)-hydroxymethyl modifications reduced the stability of the ternary complex and preferred stoichiometric binding to the miR-215 model. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Synthesis, spectroscopic and X-ray characterization of a copper(II) complex with the Schiff base derived from pyridoxal and aminoguanidine: NMR spectral studies of the ligand.

    Science.gov (United States)

    Leovac, Vukadin M; Joksović, Milan D; Divjaković, Vladimir; Jovanović, Ljiljana S; Saranović, Zana; Pevec, Andrej

    2007-07-01

    A copper(II) complex with the pyridoxal-aminoguanidine (PL-AG) Schiff base adduct, as an organic compound of the very potent biological activity and promising pharmacological importance in the treatment of diabetic complications, has been prepared and characterized. The X-ray structural analysis of the [CuCl2(PL-AG)] complex showed that it has a distorted pseudo-square-pyramidal (4+1) structure with the tridentate ONN Schiff base in the equatorial plane, with the Cu-O(1), Cu-N(1) and Cu-N(3) bond lengths of 1.917(2)A, 1.930(2)A and 1.984(2)A, respectively. The bond length of the equatorial Cu-Cl(1) is 2.279(1)A, while that of the apical Cu-Cl(2) is 2.792(1)A. Pyridoxal fragment is coordinated in its zwitterionic form. In addition to the X-ray structural analysis, the complex was characterized by IR spectrometric, conductometric and magnetic techniques, and the ligand itself by IR, 1H and 13C NMR spectra.

  8. Synthesis, spectroscopic (FT-IR, FT-Raman, NMR, UV-Visible), first order hyperpolarizability, NBO and molecular docking study of (E)-1-(4-bromobenzylidene)semicarbazide

    Science.gov (United States)

    Raja, M.; Muhamed, R. Raj; Muthu, S.; Suresh, M.

    2017-01-01

    The compound (E)-1-(4-bromobenzylidene)semicarbazide(4BSC) was synthesized and characterized by FT-IR, FT-Raman, UV-Visible, 1HNMR and 13CNMR spectra. The optimized molecular geometry(bond length, bond angle), the complete vibrational frequency, the infrared intensities and the Raman scattering activities were calculated by using density functional theory(DFT) B3LYP method with the help of 6-311++G(d,p) basis set. From the recorded UV-Visible spectrum, the electronic properties such as excitation energies, wavelength, band gap and oscillator strength are evaluated by TD-DFT in DMSO solution and gas phase methods using 6-311++G(d,p) basis set. The calculated HOMO - LUMO band gap energies confirm that charge transfer occurs within the molecule. The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of the molecule are calculated by the gauge-independent atomic orbital (GIAO) method and compared with experimental results. The hyperconjugative interaction energy E(2) and electron densities of donor (i) and acceptor (j) bonds were calculated using NBO analysis. Besides NLO and MEP were also calculated and interpreted. To study the biological activity of the investigation molecule, molecular docking was done to identify the hydrogen bond lengths and binding energy with different antimicrobial protein. Thermodynamic properties of the title compound at different temperatures have been calculated, revealing the correlations the heat capacity (C), entropy (S) and enthalpy changes (H) and temperatures.

  9. Quantum mechanical, spectroscopic studies (FT-IR, FT-Raman, NMR, UV) and normal coordinates analysis on 3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide

    Science.gov (United States)

    Muthu, S.; Uma Maheswari, J.; Sundius, Tom

    2013-05-01

    Famotidine (3-([2-(diaminomethyleneamino) thiazol-4-yl] methylthio)-N'-sulfamoylpropanimidamide) is a histamine H2-receptor antagonist that inhibits stomach acid production, and it is commonly used in the treatment of peptic ulcer disease (PUD) and gastroesophageal reflux disease (GERD/GORD). Quantum chemical calculations of the equilibrium geometry of famotidine in the ground state were carried out using density functional theory (DFT/B3LYP) with the 6-311G(d,p) basis set. In addition, harmonic vibrational frequencies, infrared intensities and Raman activities were calculated at the same level of theory. A detailed interpretation of the infrared and Raman spectrum of the drug is also reported. Theoretical simulations of the FT-IR, and FT-Raman spectra of the title compound have been calculated. Good correlations between the experimental 1H and 13C NMR chemical shifts and calculated GIAO shielding tensors were found. The results of the energy and oscillator strength calculations by time-dependent density functional theory (TD-DFT) supplement the experimental findings. Total and partial density of state (TDOS and PDOS) and also overlap population density of state (COOP or OPDOS) diagrams analysis were presented. The dipole moment, linear polarizability and first order hyperpolarizability values were also computed. The linear polarizability and first order hyperpolarizabilities of the studied molecule indicate that the compound is a good candidate for nonlinear optical materials.

  10. Structural, spectroscopic (FT-IR, NMR, UV-visible), nonlinear optical (NLO), cytotoxic and molecular docking studies of 4-nitro-isonitrosoacetophenone (ninapH) by DFT method

    Science.gov (United States)

    Kucuk, Ilhan; Kaya, Yunus; Kaya, A. Asli

    2017-07-01

    (4-Nitro-phenyl)-oxo-acetaldehyde oxime (ninapH) is a type of oxime, which has a oxime and α-carbonyl groups. This molecule has been synthesized from literature procedure. The structural properties and conformational behaviors were examined using the density functional theory (DFT) with the B3LYP method combined with the 6-311++G(d,p) basis set. As a result of the conformational studies, the most stable conformer was determined, and then this molecule was optimized with the same basis set. Comprehensive theoretical and experimental structural studies on the molecule have been carried out by FT-IR, NMR and UV-vis spectrometry. The calculated HOMO and LUMO energies show that charge transfer within the molecule. The first order hyperpolarizability and molecular electrostatic potential (MEP) were also performed. The thermodynamic properties (heat capacity, entropy, and enthalpy) of the ninapH have been calculated at different temperatures, 100-1000 K. In addition, the molecular docking studies have been performed with DNA and protein structures (downloaded from Protein Data Bank).

  11. Spectroscopic (FT-IR, FT-Raman, 1H- and 13C-NMR, Theoretical and Microbiological Study of trans o-Coumaric Acid and Alkali Metal o-Coumarates

    Directory of Open Access Journals (Sweden)

    Małgorzata Kowczyk-Sadowy

    2015-02-01

    Full Text Available This work is a continuation of research on a correlation between the molecular structure and electronic charge distribution of phenolic compounds and their biological activity. The influence of lithium, sodium, potassium, rubidium and cesium cations on the electronic system of trans o-coumaric (2-hydroxy-cinnamic acid was studied. We investigated the relationship between the molecular structure of the tested compounds and their antimicrobial activity. Complementary molecular spectroscopic techniques such as infrared (FT-IR, Raman (FT-Raman, ultraviolet-visible (UV-VIS and nuclear magnetic resonance (1H- and 13C-NMR were applied. Structures of the molecules were optimized and their structural characteristics were calculated by the density functional theory (DFT using the B3LYP method with 6-311++G** as a basis set. Geometric and magnetic aromaticity indices, atomic charges, dipole moments and energies were also calculated. Theoretical parameters were compared to the experimental characteristics of investigated compounds. Correlations between certain vibrational bands and some metal parameters, such as electronegativity, ionization energy, atomic and ionic radius, were found. The microbial activity of studied compounds was tested against Escherichia coli, Bacillus subtilis, Pseudomonas aeruginosa, Staphylococcus aureus, Proteus vulgaris and Candida albicans.

  12. Measurements of angular distributions for7Li elastically scattered from58Ni at energies around the Coulomb barrier

    Science.gov (United States)

    Amador-Valenzuela, P.; Aguilera, E. F.; Martinez-Quiroz, E.; Lizcano, D.; Morales-Rivera, J. C.

    2017-07-01

    Recently, experimental measurements of elastic scattering angular distributions for the system7Li+58Ni at ten different energies around the Coulomb barrier were made by the Heavy-Ion Group. The measurements were made at the Tandem Van de Graaff Particle Accelerator Laboratory in the National Institute for Nuclear Research (ININ) in Mexico. In this work, preliminary elastic scattering angular distributions for five energies (E lab , = 12.0, 12.5, 13.0, 13.5 and 14.22 MeV) are presented. The preliminary experimental data were analyzed using the São Paulo Optical Model Potential (SPP) which is based on a double-folding potential, reproducing very well these data. A comparison is made with old data reported back in 1973 and in 2012. Further analysis is in progress in order to fully understand this particular system, specially because7Li is known to be a weakly bound nucleus.

  13. $^{7}Li(p,n)$ Nuclear Data Library for Incident Proton Energies to 150 MeV

    CERN Document Server

    Mashnik, S G; Hughes, H G; Little, R C; MacFarlane, R E; Waters, L S; Young, P G

    2000-01-01

    We describe evaluation methods that make use of experimental data, and nuclear model calculations, to develop an ENDF-formatted data library for the reaction p + Li7 for incident protons with energies up to 150 MeV. The important 7-Li(p,n_0) and 7-Li(p,n_1) reactions are evaluated from the experimental data, with their angular distributions represented using Lengendre polynomial expansions. The decay of the remaining reaction flux is estimated from GNASH nuclear model calculations. The evaluated ENDF-data are described in detail, and illustrated in numerous figures. We also illustrate the use of these data in a representative application by a radiation transport simulation with the code MCNPX.

  14. Experimental probe for the production of 97Ru from the 7Li+93Nb reaction: A study of precompound emissions

    Science.gov (United States)

    Kumar, Deepak; Maiti, Moumita; Lahiri, Susanta

    2016-10-01

    Background: Interaction of weakly bound heavy ions with an intermediate or heavy target is not yet understood completely due to the scarcity of experimental data. In order to develop a clear understanding of breakup fusion or preequilibrium emission even in the low energy range, 3-10 MeV/nucleon, more experimental investigations are necessary. Purpose: We aim to study the reaction mechanisms involved in the weakly bound heavy-ion induced reaction 7Li+93Nb at low energies by measuring the production cross sections of the residual radionuclides. Method: Natural niobium (93Nb) foil, backed by an aluminum (Al) catcher, arranged in a stack was bombarded by 7Li ions of 20-45 MeV energy. Activity of the residues produced in each 93Nb target was measured by off line γ -ray spectrometry after the end of bombardment (EOB) and cross sections were calculated. Experimental cross sections were compared with those computed using compound and precompound models. Results: In general, measured excitation functions of all residues produced in the 7Li+93Nb reaction showed good agreement with the model calculations based on the Hauser-Feshbach formalism and the exciton model for compound and precompound processes, respectively. Significant preequilibrium emission of neutrons was observed at the relatively high energy tail of the excitation function of 97Ru. Conclusions: Preequilibrium processes played an important role in the enhancement of the cross section in the x n reaction channel over the compound reaction mechanism at higher energies for the 7Li+93Nb reaction. Additionally, indirect evidence of incomplete or breakup fusion was also perceived.

  15. AB-BNCT beam shaping assembly based on {sup 7}Li(p,n){sup 7}Be reaction optimization

    Energy Technology Data Exchange (ETDEWEB)

    Minsky, D.M., E-mail: minsky@tandar.cnea.gov.ar [Gerencia de Investigacion y Aplicaciones, CNEA, Av. Gral Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina)] [Escuela de Ciencia y Tecnologia, UNSAM, M. de Irigoyen 3100 (1650), San Martin (Argentina)] [CONICET, Av. Rivadavia 1917 (C1033AAJ), Buenos Aires (Argentina); Kreiner, A.J. [Gerencia de Investigacion y Aplicaciones, CNEA, Av. Gral Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina)] [Escuela de Ciencia y Tecnologia, UNSAM, M. de Irigoyen 3100 (1650), San Martin (Argentina)] [CONICET, Av. Rivadavia 1917 (C1033AAJ), Buenos Aires (Argentina); Valda, A.A. [Gerencia de Investigacion y Aplicaciones, CNEA, Av. Gral Paz 1499 (B1650KNA), San Martin, Buenos Aires (Argentina)] [Escuela de Ciencia y Tecnologia, UNSAM, M. de Irigoyen 3100 (1650), San Martin (Argentina)

    2011-12-15

    A numerical optimization of a Beam Shaping Assembly (BSA) for Accelerator Based-Boron Neutron Capture Therapy (AB-BNCT) has been performed. The reaction {sup 7}Li(p,n){sup 7}Be has been considered using a proton beam on a lithium fluoride target. Proton energy and the dimensions of a simple BSA geometry have been varied to obtain a set of different configurations. The optimal configuration of this set is shown.

  16. Preliminary study of the 19F(7Li,7Be)19O reaction at 52 MeV with MAGNEX

    CERN Document Server

    Cavallaro, M; Cappuzzello, F; Carbone, D; Foti, A; Orrigo, S E A; Rodrigues, M R D; Schillaci, M; Borello-Lewin, T; Petrascu, H

    2010-01-01

    The 19F(7Li,7Be)19O charge-exchange reaction at 52 MeV incident energy has been performed at INFN-LNS in Catania using the MAGNEX spectrometer. The use of an algebraic ray-reconstruction technique has allowed to extract the 19O excitation energy spectrum and the experimental angular distributions obtained with a single angular setting of the spectrometer.

  17. Interspecies collision-induced losses in a dual species 7Li-85Rb magneto-optical trap

    Science.gov (United States)

    Dutta, Sourav; Altaf, Adeel; Lorenz, John; Elliott, D. S.; Chen, Yong P.

    2014-05-01

    In this article, we report the measurement of collision-induced loss rate coefficients βLi, Rb and βRb, Li, and also discuss means to significantly suppress such collision-induced losses. We first describe our dual-species magneto-optical trap (MOT) that allows us to simultaneously trap ≥5 × 108 7Li atoms loaded from a Zeeman slower and ≥2 × 108 85Rb atoms loaded from a dispenser. We observe strong interspecies collision-induced losses in the MOTs which dramatically reduce the maximum atom number achievable in the MOTs. We measure the trap loss rate coefficients βLi, Rb and βRb, Li, and, from a study of their dependence on the MOT parameters, determine the cause for the losses observed. Our results provide valuable insights into ultracold collisions between 7Li and 85Rb, guide our efforts to suppress collision-induced losses, and also pave the way for the production of ultracold 7Li85Rb molecules.

  18. Interspecies collision-induced losses in a dual species 7Li-85Rb magneto-optical trap

    CERN Document Server

    Dutta, Sourav; Lorenz, John; Elliott, D S; Chen, Yong P

    2013-01-01

    In this article, we report the measurement of collision-induced loss coefficients \\beta_{Li,Rb} and \\beta_{Rb,Li}, and also discuss means to significantly suppress such collision induced losses. We first describe our dual-species magneto-optical trap (MOT) that allows us to simultaneously trap > 5x10^8 7Li atoms loaded from a Zeeman slower and > 2x10^8 85Rb atoms loaded from a dispenser. We observe strong interspecies collision-induced losses in the MOTs which dramatically reduce the maximum atom number achievable in the MOTs. We measure the trap loss rate coefficients \\beta_{Li,Rb} and \\beta_{Rb,Li}, and, from a study of their dependence on the MOT parameters, determine the cause for the losses observed. Our results provide valuable insights into ultracold collisions between 7Li and 85Rb, guide our efforts to suppress collision induced losses, and also pave the way for the production of ultracold 7Li85Rb molecules.

  19. Prediction of a weakly bound excited state of Efimov character in a 7LiHe42 system

    Science.gov (United States)

    Wu, Meng-Shan; Han, Hui-Li; Li, Cheng-Bin; Shi, Ting-Yun

    2014-12-01

    We carry out calculations on the van der Waals trimer 7LiHe42 using the mapping method within the frame of hyperspherical coordinates, which allows us to give accurate binding energies and wave functions for both the ground and excited state of the system. When the realistic two-body potentials are adopted, the system presents an excited state which shows Efimov character. We study the range of the interaction strength in which the excited state could exist and find that the state persists within the experiment error band for binding energy of LiHe molecule. We also study the three-body parameter (3BP) of 7LiHe42 system and its relationship with the background scattering length aHeHe. Our calculations demonstrate that the 3BP of 7LiHe42 system is dependent on the value of the scattering length aHeHe, independent of the short-range details of the He-He interaction. The results confirm the prediction of Wang et al. [Phys. Rev. Lett. 109, 243201 (2012), 10.1103/PhysRevLett.109.243201] that the 3BP for a heteronuclear atomic system is universally determined from the van der Waals lengths and the homonuclear scattering length.

  20. NMR spectroscopic study of the carbon and nitrogen dynamics of grass-derived pyrogenic organic material during 2.3 years of incubation in soil

    Science.gov (United States)

    Hilscher, André; Knicker, Heike

    2010-05-01

    Incomplete combustion of vegetation results in pyrogenic organic material (PyOM) which occurs ubiquitously in soils and sediments. To understand the C sequestration potential of PyOM in environmental systems knowledge is required about the respective degradation and humification mechanisms and the stability of the different chemical PyOM structures. The present study focuses on the microbial recalcitrance of PyOM on molecular scale. Therefore, microcosms incubation experiments were performed using PyOM produced from highly isotopically enriched 13C and 15N rye grass (Lolium perenne) at 350°C under oxic conditions for one (1M) and four minutes (4M). Solid-state CPMAS 13C and 15N NMR studies were accomplished to obtain insights into the involved humification mechanisms at different stages the PyOM degradation. In total up to 38% of the bulk PyOM C was mineralised during the 28 months of incubation. The O/N-alkyl C and alkyl C residues which survived the charring process were effectively decomposed. At the end of the incubation up to 73% and 57% of the initial O/N-alkyl C and alkyl C amount were mineralised or converted to other C groups, respectively. The total aryl C group recovery of the PyOM decreased significantly during the 28 months of incubation (P ≤ 0.001). After 20 months of incubation between 26% and 40% of the initial aryl C amount was lost. For this group, relative short half time periods in the range of 3.0 and 3.8 years were obtained. The observed loss of aromatic C structures may be attributed to two simultaneous processes, the mineralisation to CO2 and the conversion to other C groups by partial oxidation. The presence of a readily decomposable co-substrate showed no significant changes in the degradation pattern of the different PyOM, possibly because decomposable sources were already available in the starting PyOM. Most of the organic bound N of the fresh PyOM was assignable to heterocyclic aromatic compounds such as pyrrole and indole

  1. The study of 12C(α,γ astrophysical reaction using 12C(6Li,d and 12C(7Li,t reaction at 20 MeV and in the framework of the potential model

    Directory of Open Access Journals (Sweden)

    Adhikari S.

    2015-01-01

    Full Text Available The triton angular distribution in the 12C(7Li,t16O reaction has been measured at 20 MeV incident energy. Comparison of the data with Finite Range DWBA and CDCC-CRC calculations show that breakup coupling effects are prominent in the transfer to the ground state. This observation is similar to that in the 12C(6Li,d reaction at the same incident energy. The alpha spectroscopic factor of the 16O ground state is determined (Sα=0.25 from a comparison of the measured angular distribution with respect to the CDCC-CRC calculations. The E2 S-factor of the 12C(α,γ reaction at 300 keV in the framework of a potential model is determined to be about 118 keV-barn.

  2. Local environments and lithium adsorption on the iron oxyhydroxides lepidocrocite (gamma-FeOOH) and goethite (alpha-FeOOH): A 2H-2 and 7Li solid-state MAS NMR study

    DEFF Research Database (Denmark)

    Nielsen, Ulla Gro; Grey, Clare P.; Paik, Jonkim

    2008-01-01

    2H and 7LiMAS NMR spectroscopy techniques were applied to study the local surface and bulk environments of iron oxyhydroxide lepiclocrocite (gamma-FeOOH). 2H variable-temperature (VT) MAS NMR experiments were performed, showing the presence of short-range, strong antiferromagnetic correlations, e...

  3. Depth profiling Li in electrode materials of lithium ion battery by {sup 7}Li(p,γ){sup 8}Be and {sup 7}Li(p,α){sup 4}He nuclear reactions

    Energy Technology Data Exchange (ETDEWEB)

    Sunitha, Y., E-mail: sunibarc@gmail.com; Kumar, Sanjiv

    2017-06-01

    A proton induced γ-ray emission method based on {sup 7}Li(p,γ){sup 8}Be proton capture reaction and a nuclear reaction analysis method involving {sup 7}Li(p,α){sup 4}He reaction are described for depth profiling Li in the electrode materials, graphite and lithium cobalt oxide for example, of a Li-ion battery. Depth profiling by {sup 7}Li(p,γ){sup 8}Be reaction is accomplished by the resonance at 441 keV and involves the measurement of 14.6 and 17.6 MeV γ-rays, characteristic of the reaction, by a NaI(Tl) detector. The method has a detection sensitivity of ∼0.2 at% and enables profiling up to a depth ≥20 µm with a resolution of ≥150 nm. The profiling to a fairly large depth is facilitated by the absence of any other resonance up to 1800 keV proton energy. The reaction has substantial off-resonance cross-sections. A procedure is outlined for evaluating the off-resonance yields. Interferences from fluorine and aluminium are major limitation of this depth profiling methodology. The depth profile measurement by {sup 7}Li(p,α){sup 4}He reaction, on the other hand, utilises 2–3 MeV protons and entails the detection of α-particles at 90° or 150° angles. The reaction exhibits inverse kinematics at 150°. This method, too, suffers interference from fluorine due to the simultaneous occurrence of {sup 19}F(p,α){sup 16}O reaction. Kinematical considerations show that the interference is minimal at 90° and thus is the recommended angle of detection. The method is endowed with a detection sensitivity of ∼0.1 at%, a depth resolution of ∼100 nm and a probing depth of about 30 µm in the absence and 5–8 µm in the presence of fluorine in the material. Both methods yielded comparable depth profiles of Li in the cathode (lithium cobalt oxide) and the anode (graphite) of a Li-ion battery.

  4. (p,px) reaction on /sup 6/Li and /sup 7/Li nuclei at incident proton energy of 70 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Gorpinich, O.K.; Kadkin, E.P.; Kondrat' ev, S.N.; Lobach, Yu.M.; Pasechnik, M.V.; Saltykov, L.S.; Tokarevskij, V.V. (AN Ukrainskoj SSR, Kiev. Inst. Yadernykh Issledovanij)

    1983-01-01

    Measurements of two-dimensional coincidence spectra of charged particles from the /sup 6/Li(p, 2p)/sup 5/He, /sup 6/Li(p, p..cap alpha..)/sup 2/H, /sup 7/Li(p, pt)/sup 4/He, /sup 7/Li(p, p..cap alpha..)/sup 3/H reactions has been carried out using the equipment for simultaneous investigation of correlation of charged particles of different types. The /sup 6/Li(p, pd) reaction probability reaches the maximum value when the residual nucleus momentum is close to zero. This fact may confirm an existance of strong /sup 6/Li ..cap alpha..d-clusterization. The /sup 7/Li(p, pt) reaction occurs with the minimum probability in a quasi-free region that confirms /sup 7/Li ..cap alpha..t-structure. A direct comparison of particle two-dimensional spectra projections of (p, px) type reactions reveals that a probability of quasi-free scattering of proton on deuteron (triton) /sup 6/Li(/sup 7/Li) cluster is higher than quasi-free scattering on intranuclear protons. This fact is also confirmed by an assumption on ..cap alpha..d(..cap alpha..t)-cluster /sup 6/Li(/sup 7/Li) nucleus structure.

  5. Complete and incomplete fusion dynamics of {sup 6,7}Li + {sup 159}Tb reactions near the Coulomb barrier

    Energy Technology Data Exchange (ETDEWEB)

    Gautam, Manjeet Singh [Thapar University, School of Physics and Materials Science, Patiala (India); Indus Degree College, Department of Physics, Kinana, Jind, Haryana (India); Grover, Neha; Sharma, Manoj K. [Thapar University, School of Physics and Materials Science, Patiala (India)

    2017-01-15

    The complete fusion (CF) and incomplete fusion (ICF) cross-sections are estimated for {sup 6,} {sup 7}Li + {sup 159}Tb reactions using the energy-dependent Woods-Saxon potential model (EDWSP model) and dynamical cluster-decay model (DCM). The CF data of the {sup 6}Li + {sup 159}Tb({sup 7}Li + {sup 159}Tb) reaction at above barrier energies is suppressed with reference to expectations of the EDWSP model by 25% (20%) which is smaller than the reported data by ∝ 9% (6%). This suppression is correlated with the projectile breakup effect. The projectiles {sup 6,7}Li are loosely bound systems, which may break up into charged fragments prior to reaching the fusion barrier and subsequently one of the fragment is captured by the target leading to the suppression of fusion data at above barrier energies. The sum of CF and ICF, which is termed as total fusion cross-section (TF), removes the discrepancies between theoretical predictions and the above barrier complete fusion data and hence is adequately explained via the EDWSP model over a wide range of energy spread across the Coulomb barrier. In addition to fusion, the decay mechanism of {sup 6}Li + {sup 159}Tb reaction is studied within the framework of the dynamical cluster-decay model (DCM). The breakup of the projectile ({sup 6}Li) in the entrance channel indicates the presence of ICF, which is investigated further using the collective clusterization approach of DCM. The present theoretical analysis suggests that a larger barrier modification is needed to address the fusion data of chosen reactions in the below barrier energy region. (orig.)

  6. Measuring the ratio of aqueous diffusion coefficients between 6Li +Cl - and 7Li +Cr - by osmometry

    Science.gov (United States)

    Fritz, Steven J.

    1992-10-01

    Osmotic equilibrium is a singular occurrence in the evolution of an osmotic cell because at this event the net solution flux is zero such that -J w · V¯w = J s · V¯s. At this juncture, the diffusion coefficient of the solute through the membrane (ω) equals the solute flux ( Js) divided by the osmotic pressure (ΔΠ). Because the solute permeability coefficient (ω) is related to the Fickian diffusion coefficient ( D) through the gas constant, temperature, and the membrane's thickness and tortuosity, the ratio of ω values for individual isotopic species equals the ratio of D values for the same isotopic components. A 0.9450 molal LiCl solution was placed within sealed dialysis tubing and osmoted against a kilogram of deionized water at 22°C. Osmotic equilibrium occurred at 164 ± 10 min. The ratio of ω6Li +Cl -/ω7Li +Cl - was measured to be 1.011 ± 0.003 - a value close to the square root of the mass ratio between 7LiCl and 6LiCl (= 1.012) as calculated by Graham's Law. The measured diffusion coefficient ratio was used to predict the degree of hyperfiltration-induced fractionation of Li isotopes as a function of membrane ideality. When a membrane's σ exceeds 0.95 (as is likely for low-porosity shales) the 6Li /7Li ratio on the high-pressure side of the membrane can theoretically vary by more than 0.0017.

  7. Role of neutron transfer processes on the 6Li+120Sn and 7Li+119Sn fusion reactions

    Directory of Open Access Journals (Sweden)

    Fisichella M.

    2015-01-01

    Full Text Available The results concerning the study of 6Li+120Sn and 7Li+119Sn systems are presented. These two sistems are characterised by very similar structures of the interacting nuclei and by different Q-value for one-and two- neutron transfer. Our aim is to disentangle the possible effects due to the different n-transfer Q-values, at sub-barriers energies, by comparing the two fusion excitation function. In these experiments the fusion cross section has been measured by using a stack activation technique. No particular differences in the two fusion excitation functions have been observed.

  8. A TPD and AR based comparison of accelerator neutron irradiation fields between (7)Li and W targets for BNCT.

    Science.gov (United States)

    Tanaka, Kenichi; Endo, Satoru; Yonai, Shunsuke; Baba, Mamoru; Hoshi, Masaharu

    2014-06-01

    The characteristics of moderator assembly dimension was investigated for the usage of (7)Li(p,n) neutrons by 2.3-2.8MeV protons and W(p,n) neutrons by 50MeV protons. The indexes were the treatable protocol depth (TPD) and advantage depth (AD). Consequently, a configuration for W target with the Fe filter, Fluental moderator, Pb reflector showed the TPD of 5.8cm and AD of 9.3cm. Comparable indexes were found for the Li target in a geometry with the MgF2 moderator and Teflon reflector.

  9. Calculation of Double-Differential Cross Sections of n+7Li Reactions Below 20 MeV

    Institute of Scientific and Technical Information of China (English)

    ZHANG Jing-Shang; HAN Ying-Lu

    2002-01-01

    A new reaction model for light nuclei is proposed to analyze the measured data,especially for analysis of the double-differential cross sections of the outgoing particles.Many channels arc opened in the n + 7Li reaction below En< 20 MeV.The reaction mechanism is very complex,beside the sequential emissions there are also three-body breakup processes.Because of a strong recoil effect of light nucleus reactions,the energy balance is strictly taken into account.The comparisons of the calculated results with the double-differential measurements indicate that the model calculations are successful for the total outgoing neutrons.

  10. Elastic forward analysis using sup 7 Li ions A useful tool for H and light elements determination

    CERN Document Server

    Romero, S; Murillo, G; Berdejo, H M

    2002-01-01

    Films of CN sub x /Si, TiN sub x /AISI 304 and AlO sub x /Si were analyzed with sup 7 Li ions from 4.0 to 4.5 MeV and an experimental arrangement that, through detection of scattered projectiles and recoils by a single detector, allows quantification of H, light elements and heavier ones. A discussion is presented of the capabilities of Rutherford backscattering spectrometry (RBS) and conventional elastic recoil detection analysis (ERDA) compared to elastic forward analysis.

  11. Evaluation of chemopreventive response of two cycloxygenase-2 inhibitors, etoricoxib and diclofenac in rat colon cancer using FTIR and NMR spectroscopic techniques Evaluación de la respuesta quimiopreventiva de dos inhibidores de la ciclooxigenasa 2, etoricoxib y diclofenaco en el cáncer de colon murino empleando las técnicas espectroscópicas FTIR Y NMR

    Directory of Open Access Journals (Sweden)

    M. Kaur Saini

    2010-08-01

    Full Text Available Non steroidal anti inflammatory drugs (NSAIDs are efficacious in chemoprevention of colorectal cancer. Therefore, the potential ability of Etoricoxib, a selective cycloxygenase-2(COX-2 inhibitor and Diclofenac, a preferential COX-2 inhibitor are considered in the chemoprevention of 1, 2-dimethylhydrazine (DMH induced colon carcinogenesis in rat model. DMH was injected s.c. for six weeks while Etoricoxib and Diclofenac were fed daily orally alone and also in combination with an weekly subcutaneous injection of 1,2-dimethylhydrazine dihydrochloride (DMH to the rats. After the treatment period of 6 weeks the animals were sacrificed by an overdose of ether anesthesia and the colonic tissues were removed and studied by the FTIR and NMR Spectroscopic techniques to evaluate the changes occurring in the lipid bilayer of colonic membrane lipids. The alterations in wave number of FTIR spectra as well as the chemical shifts of NMR spectra were recorded which signify the modulation of membrane lipids during colon carcinogenesis and possible cancer prevention by the oral administration of NSAIDs in an experimental model of chemical induced colon carcinogenesis.Los fármacos antiinflamatorios no esteroideos (AINE son eficaces en la prevención del cáncer colorrectal. Por lo tanto, la capacidad potencial de Etoricoxib, un inhibidor selectivo de la ciclooxigenasa-2(COX-2, y de Diclofenaco, un inhibidor preferencial de la COX-2, se considera en la quimioprevención de la carcinogénesis de colon inducida por 1, 2-dimetilhidracina (DMH en el modelo murino. Se inyectó s.c. DMH durante 6 semanas a la vez que se administraban diariamente por vía oral Etoricoxib y Diclofenaco solos y en combinación con una inyección s.c. semanal de dihidrocloruro de 1,2-dimetilhidracina (DMH a las ratas. Después del período de tratamiento de 6 semanas, se sacrificó a los animales mediante una sobredosis de anestesia con éter y se extirpó el tejido colónico para estudio con

  12. Elastic scattering and cluster-transfer reactions of 98Rb on 7Li at REX-ISOLDE

    CERN Document Server

    Bouma, Jake

    Exotic nuclei are nuclei with unusual proton to neutron ratios that exist far away from stability. Due to their instability, these nuclei are only available for nuclear reactions as radioactive ion beams. Experiments must therefore be performed in inverse kinematics at advanced radioactive isotope separation and acceleration facilities. REX-ISOLDE at CERN is one such facility, capable of producing post-accelerated radioactive ion beams with energies up to 2.85 MeV/u. Cluster-transfer reactions in inverse kinematics with a $^{7}$Li target are proposed as a tool for the study of exotic nuclei at REX-ISOLDE. In these reactions, either the $\\alpha$ or triton clusters that make up the weakly bound $^{7}$Li nucleus can be transfered to the beam nucleus. The remaining cluster that is not transferred can be detected, and identifies the particular transfer channel. Through this mechanism it is possible to populate states of very high spin, which is useful for $\\gamma$-spectroscopy in poorly known exotic regions. Speci...

  13. The 7Be(d,p)2alpha cross section at Big Bang energies and the primordial 7Li abundance

    CERN Document Server

    Angulo, C; Couder, M; Demaret, P; Leleux, P; Vanderbist, F; Coc, A; Kiener, J; Tatischeff, V; Davinson, T; Murphy, A S; Achouri, N L; Orr, N A; Cortina-Gil, D; Figuera, P; Fulton, B R; Mukha, I; Vangioni, E

    2005-01-01

    The WMAP satellite, devoted to the observations of the anisotropies of the Cosmic Microwave Background (CMB) radiation, has recently provided a determination of the baryonic density of the Universe with unprecedented precision. Using this, Big Bang Nucleosynthesis (BBN) calculations predict a primordial 7Li abundance which is a factor 2-3 higher than that observed in galactic halo dwarf stars. It has been argued that this discrepancy could be resolved if the 7Be(d,p)2alpha reaction rate is around a factor of 100 larger than has previously been considered. We have now studied this reaction, for the first time at energies appropriate to the Big Bang environment, at the CYCLONE radioactive beam facility at Louvain-la-Neuve. The cross section was found to be a factor of 10 smaller than derived from earlier measurements. It is concluded therefore that nuclear uncertainties cannot explain the discrepancy between observed and predicted primordial 7Li abundances, and an alternative astrophysical solution must be inve...

  14. NMR spectroscopy using liquid crystal solvents

    CERN Document Server

    Emsley, JW

    2013-01-01

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

  15. Quantum mechanical and spectroscopic (FT-IR, FT-Raman,1H,13C NMR, UV-Vis) studies, NBO, NLO, HOMO, LUMO and Fukui function analysis of 5-Methoxy-1H-benzo[d]imidazole-2(3H)-thione by DFT studies

    Science.gov (United States)

    Pandey, Manju; Muthu, S.; Nanje Gowda, N. M.

    2017-02-01

    Theoretical analysis of the molecular structure, spectroscopic (FT-IR, FT-Raman, 1H, 13C NMR, UV-Vis) studies, and thermodynamic characteristics of 5-Methoxy-1H-benzo[d]imidazole-2(3H)-thione (5MBIT) molecule were done by DFT/B3LYP using 6-311++G(d, p) basis set. Theoretical parameters were compared with experimental data. The dipole moment (μ), polarizability (Δα) and first order hyperpolarizability (β) of the molecule were calculated. Thermodynamic properties, HOMO and LUMO energies were determined. Global reactivity parameters and Fukui function of the 5MBIT molecule were predicted.

  16. Using the Doppler broadened γ line of the 10B(n,αγ)7Li reaction for thermal neutron detection

    Science.gov (United States)

    Ben-Galim, Y.; Wengrowicz, U.; Moreh, R.; Orion, I.; Raveh, A.

    2016-02-01

    When a thermal neutron is absorbed by 10B in the 10B(n,α)7Li reaction, there is a chance of 94% that a 478 keV photon be emitted by an excited 7Li nucleus. This reaction is exothermic with a Q-value of 2.31 MeV and the nuclei are emitted with kinetic energies of E(α)=1.47 MeV and E(7Li*)=0.84 MeV. This implies that the 478 keV γ line is emitted by a moving 7Li nucleus and hence is expected to be Doppler broadened. In the present work we suggest to use this broadening of the γ line as a fingerprint for the detection of thermal neutrons using a high resolution gamma spectrometer. We thus developed a Monte Carlo program using a MATLAB code based on a High Purity Germanium (HPGe) detector coupled with a Boron Carbide (B4C) sheet to calculate the γ line broadening. Our simulation shows that the FWHM width of the resulting γ line is 12.6 keV, in good agreement with our measurement. Hence the broadened γ line emitted by the 10B(n,αγ)7Li reaction and detected by a HPGe detector shows that this method is an effective tool for neutron detection while maintaining good gamma discrimination.

  17. New method to evaluate the {sup 7}Li(p, n){sup 7}Be reaction near threshold

    Energy Technology Data Exchange (ETDEWEB)

    Herrera, María S., E-mail: herrera@tandar.cnea.gov.ar [Comisión Nacional de Energía Atómica, Av. Gral. Paz 1499, Buenos Aires B1650KNA (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas, Av. Rivadavia 1917, Ciudad Autónoma de Buenos Aires C1033AAJ (Argentina); Escuela de Ciencia y Tecnología, UNSAM, 25 de Mayo y Francia, Buenos Aires B1650KNA (Argentina); Moreno, Gustavo A. [YPF Tecnología, Baradero S/N, Buenos Aires 1925 (Argentina); Departamento de Física J. J. Giambiagi, Facultad de Ciencias Exactas y Naturales, UBA, Ciudad Universitaria, Ciudad Autónoma de Buenos Aires 1428 (Argentina); Kreiner, Andrés J. [Comisión Nacional de Energía Atómica, Av. Gral. Paz 1499, Buenos Aires B1650KNA (Argentina); Consejo Nacional de Investigaciones Científicas y Técnicas, Av. Rivadavia 1917, Ciudad Autónoma de Buenos Aires C1033AAJ (Argentina); Escuela de Ciencia y Tecnología, UNSAM, 25 de Mayo y Francia, Buenos Aires B1650KNA (Argentina)

    2015-04-15

    In this work a complete description of the {sup 7}Li(p, n){sup 7}Be reaction near threshold is given using center-of-mass and relative coordinates. It is shown that this standard approach, not used before in this context, leads to a simple mathematical representation which gives easy access to all relevant quantities in the reaction and allows a precise numerical implementation. It also allows in a simple way to include proton beam-energy spread affects. The method, implemented as a C++ code, was validated both with numerical and experimental data finding a good agreement. This tool is also used here to analyze scattered published measurements such as (p, n) cross sections, differential and total neutron yields for thick targets. Using these data we derive a consistent set of parameters to evaluate neutron production near threshold. Sensitivity of the results to data uncertainty and the possibility of incorporating new measurements are also discussed.

  18. Transport properties derived from ion-atom collisions: 6Li-6Li+ and 6Li-7Li+ Cases

    Science.gov (United States)

    Bouledroua, Moncef; Bouchelaghem, Fouzia; LPR Team

    2014-10-01

    This investigation treats quantum-mechanically the ion- atom collisions and computes the transport coefficients, such as the coefficients of mobility and diffusion. For the case of lithium, the calculations start by determining the gerade and ungerade potential curves through which ionic lithium approaches ground lithium. Then, by considering the isotopic effects and nuclear spins, the elastic and charge-transfer cross sections are calculated for the case of 6Li+and7Li+ colliding with 6Li. Finally, the temperature-dependent diffusion and mobility coefficients are analyzed, and the results are contrasted with those obtained from literature. The main results of this work have been recently published in. This work has been realized within the frames of the CNEPRU Project D01120110036 of the Algerian Ministry of Higher Education.

  19. Analysis of length distribution of short DNA fragments induced by 7Li ions using the random-breakage model

    Institute of Scientific and Technical Information of China (English)

    KONG Fuquan; ZHAO Kui; ZHAN Yong; CAO Tianguang; NI Meinan; SUI Li; CAI Minghui; ZHUO Yizhong

    2005-01-01

    Deoxyribonucleic acid (DNA) is an important bio-macromolecule. DNA double strand breaks (DSBs) are considered to be the most important initial damage responsible for all biological effects induced by ionizing radiation. In this paper the length distribution of DNA fragments induced by 7Li ionizing radiation is fitted with the random breakage model. In this model, the parameter u is the average number of DSBs on every DNA molecule induced by ionizing radiation. The fitting result shows that the random breakage model cannot describe the distribution of DNA fragments in lower doses, while the random breakage model is in better accordance with the experimental data in higher doses. It is shown that the length distribution of DNA fragments has random statistical feature in higher doses. In this situation, the random breakage model looks like a model without any parameter since the u has specific physical meaning and can directly be obtained from experimental data.

  20. Experiments on iron shield transmission of quasi-monoenergetic neutrons generated by 43- and 68-MeV protons via the {sup 7}Li(p,n) reaction

    Energy Technology Data Exchange (ETDEWEB)

    Nakashima, Hiroshi [Japan Atomic Energy Research Inst., Tokai, Ibaraki (Japan). Tokai Research Establishment; Tanaka, Shun-ichi; Nakao, Noriaki [and others

    1996-03-01

    In order to provide benchmark data of neutrons transmitted through iron shields in the intermediate-energy region, spatial distributions of neutron energy spectra and reaction rates behind and inside the iron shields of thickness up to 130 cm were measured for 43- and 68-MeVp-{sup 7}Li neutrons using a quasi-monoenergetic neutron beam source at the 90-MV AVF cyclotron facility of the TLARA facility in JAERI. The measured data by five kinds of detectors: the BC501A detector, the Bonner ball counter, {sup 238}U and {sup 232}Th fission counters, {sup 7}LiF and {sup nat}LiF TLDs and solid state nuclear track detector, are numerically provided in this report in the energy region between 10{sup -4} eV and the energy of peak neutrons generated by the {sup 7}Li(p,n) reaction. (author).

  1. Helium Bubbles Cavitation Phenomena in Pb-15.7Li and Potential Impact on Tritium Transport Behaviour in HCLL Breeding Channels

    Energy Technology Data Exchange (ETDEWEB)

    Sedano, L. A.

    2007-09-27

    COMPU task is devoted to develop a Process Flow Diagram (PFD) modelling tool for DEMO tritium cycle for HCLL and HCPB blanket lines for DEMO. At the actual stage of definition of HCLL blanket design line this global objective requires to progress specifically on the physical reliability of tritium transport assessments at blanket design level. A rough reliability assessment with the identify cation of physical phenomena determining permeation rates into the coolant was tentatively advanced in COMPU Task Deliverable 1. In HCLL design, the tritium diffusion in the alloy under the flow conditions and radiation effects in Pb15.7Li can be theoretically justifies ed as the rate limiting processes for tritium transfer into the coolant. This Deliverable 2 focuses on the analysis of a specific radiation effect: the potential role of helium bubbles in Pb15.7Li, the discussion of its implications on tritium assessment for HCLL design and consequently the analysis of its quantitative impact (as cycle input) on HCLL PFD tritium cycle design. Thus, the contents of this report investigate: (1) the rationality of the consideration on HCLL design of helium bubble cavitation phenomena in irradiated Pb15.7Li channels on the base of fundamental analysis (He solution states in Pb15.7Li) from empirical clues provided by Pb15.7Li irradiation tests, (2) a preliminary rough He-bubble cavitation design assessment and bases for a more precise FEM calculation for helium bubble cavitation phenomena in HCLL blanket channels, (3) the analysis of direct experimental data and numerical developments needed for a precise cavitation assessment and (4) a proposal of the lay-out and general specifications of an integral proof-of-principle Cavitation Experiment (Cevitex) of Helium in Pb15.7Li. (Author) 40 refs.

  2. 同位素7Li和6Li的性质殊异%The diverse of isotopes 7 Li and 6 Li

    Institute of Scientific and Technical Information of China (English)

    朱正和; 宋江锋; 罗德礼

    2014-01-01

    本文研究了同位素7 Li和6 Li在几个方面的性质差异.用相对论量子力学计算指出,6 Li的电子能级比7 Li的能级低,同时,对电偶极E (1)和磁偶极M (1)的能级跃迁波长,6 Li的跃迁波长都要比7 Li的长.由于7 Li和6 Li的核自旋的大小不同,可以看出在磁场2万高斯和温度100-20 K之间,7 Li的磁极化比6 Li的约大13倍.7 Li和6 Li的磁极化这种差异,也是一种可能的同位素7 Li/6 Li的分离方法.%The diverse of isotopes 7 Li and 6 Li was examined on the several respects.The calculations of relativistic quantum mechanics shows that the energy levels of 6 Li are lower than that of 7 Li, and therefore the transitional wave length of E(1) and M(1) for 6 Li are longer than that of 7 Li.The variation of couple constant due to the different nu-clear spin of 7 Li and 6 Li could be as a basis for the isotope separation between 7 Li and 6 Li.Ratio of the molar intensi-ty of magnetization of 7 Li to 6 Li is about 13 under 100-20 K and 20, 000 gauss, which is favorable to separate out 6 Li.

  3. Using the Doppler broadened γ line of the {sup 10}B(n,αγ){sup 7}Li reaction for thermal neutron detection

    Energy Technology Data Exchange (ETDEWEB)

    Ben-Galim, Y., E-mail: ybgx3@walla.com [Department of Nuclear Engineering, Ben Gurion University (BGU) of the Negev (Israel); Wengrowicz, U. [Department of Nuclear Engineering, Ben Gurion University (BGU) of the Negev (Israel); NRC-Negev, P.O. Box 9001, Beer-Sheva 84190 (Israel); Moreh, R. [Physics Department, Ben Gurion University (BGU) of the Negev, Beer-Sheva 84105 (Israel); Orion, I. [Department of Nuclear Engineering, Ben Gurion University (BGU) of the Negev (Israel); Raveh, A. [Advanced Coatings Center at Rotem Industries Ltd., MishorYamin D.N. Arava 86800 (Israel)

    2016-02-21

    When a thermal neutron is absorbed by {sup 10}B in the {sup 10}B(n,α){sup 7}Li reaction, there is a chance of 94% that a 478 keV photon be emitted by an excited {sup 7}Li nucleus. This reaction is exothermic with a Q-value of 2.31 MeV and the nuclei are emitted with kinetic energies of E(α)=1.47 MeV and E({sup 7}Li*)=0.84 MeV. This implies that the 478 keV γ line is emitted by a moving {sup 7}Li nucleus and hence is expected to be Doppler broadened. In the present work we suggest to use this broadening of the γ line as a fingerprint for the detection of thermal neutrons using a high resolution gamma spectrometer. We thus developed a Monte Carlo program using a MATLAB code based on a High Purity Germanium (HPGe) detector coupled with a Boron Carbide (B{sub 4}C) sheet to calculate the γ line broadening. Our simulation shows that the FWHM width of the resulting γ line is 12.6 keV, in good agreement with our measurement. Hence the broadened γ line emitted by the {sup 10}B(n,αγ){sup 7}Li reaction and detected by a HPGe detector shows that this method is an effective tool for neutron detection while maintaining good gamma discrimination. - Highlights: • Thermal neutron detection by measuring the Doppler broadened 478 keV γ line from the {sup 10}B(n,αγ){sup 7}Li interaction. • Natural Boron Carbide coupled with a HPGe detector were used in this study. • A mathematical Monte-Carlo model for the suggested detector was introduced. • A calibration tool for the suggested detector is introduced. • Experimental results show that the suggested method can be used for neutron detection.

  4. Compact NMR

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-06-01

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

  5. LEGO-NMR spectroscopy: a method to visualize individual subunits in large heteromeric complexes.

    Science.gov (United States)

    Mund, Markus; Overbeck, Jan H; Ullmann, Janina; Sprangers, Remco

    2013-10-18

    Seeing the big picture: Asymmetric macromolecular complexes that are NMR active in only a subset of their subunits can be prepared, thus decreasing NMR spectral complexity. For the hetero heptameric LSm1-7 and LSm2-8 rings NMR spectra of the individual subunits of the complete complex are obtained, showing a conserved RNA binding site. This LEGO-NMR technique makes large asymmetric complexes accessible to detailed NMR spectroscopic studies.

  6. Breakup of 42 MeV 7Li projectiles in the fields of 12C and 197Au nuclei

    Indian Academy of Sciences (India)

    Dhruba Gupta; C Samanta; R Kanungo; P Basu; Subinit Roy; S Kailas; A Chatterjee; B J Roy; K Mahata; A Samant; A Shrivastava

    2001-07-01

    Inclusive cross sections of particles and tritons from the breakup of 42 MeV 7Li by 12C and 197Au targets are presented and analysed in the framework of the Serber model. Spectral distortions due to the targets and relevant reaction mechanisms are discussed.

  7. Synthesis of 8-(dimethylamino)-1-naphthyllithium etherate. Its structure in the solid (X-ray) and in Solution (7Li and 1H NMR)

    NARCIS (Netherlands)

    Koten, G. van; Jastrzebski, J.T.B.H.; Goubitz, K.; Arlen, C.; Pfeffer, M.

    1983-01-01

    The reaction of Bu{4}Li{4} with 4 molar equivalents of 1-(dimethylamino)naphthalene in diethyl ether affords novel 8-(dimethylamino)-1-naphthyllithium. Its molecular structure (X-ray) consists of two 8-(dimethylamino)-1-naphthyl groups each 3 center-2 electron bonded via C(1) to two lithium atoms an

  8. Relation between (e, e') sum rules in {sup 6,7}Li and {sup 4}He nuclei: Experiment and cluster model

    Energy Technology Data Exchange (ETDEWEB)

    Efros, V.D. [National Research Center ' ' Kurchatov Institute' ' , Moscow (Russian Federation); National Research Nuclear University MEPhI (Moscow Engineering Physics Institute), Moscow (Russian Federation); Timchenko, I.S.; Buki, A.Yu. [National Science Center ' ' Kharkov Institute of Physics and Technology' ' , Kharkov (Ukraine)

    2016-09-15

    The sums over (e, e') spectra of {sup 6}Li and {sup 7}Li nuclei which correspond to the longitudinal sum rule are studied. It is suggested that due to the cluster structure of the lithium isotopes these sums may approximately be expressed in terms of such a sum pertaining to the α-particle. Calculation of these sums is performed in the framework of cluster models with antisymmetrization done with respect to all the nucleons. At momentum transfers higher than 0.8 fm{sup -1} the relations expressing the A = 6 or 7 sum in terms of the A = 4 sum prove to be valid with rather high accuracy. In the region of momentum transfers around 1 fm{sup -1} the longitudinal correlation functions of {sup 6}Li and {sup 7}Li nuclei are found to be close to that of the α-particle. Basing on this, the difference between the q values at which the high-q limit of the inelastic sum rule is reached in the {sup 6,7}Li cases and the {sup 4}He case is explained. The experimental longitudinal sums in the range between 0.450 and 1.625 fm{sup -1} are employed to perform comparison with the theoretical sum rule calculated in the framework of cluster models. Out of the experimental sums, those in the range between 0.750 and 1.000 fm{sup -1} in the {sup 6}Li case and between 0.750 and 1.125 fm{sup -1} in the {sup 7}Li case are obtained in the present work. In the {sup 6}Li case a complete agreement between experiment and the calculated sum rule is found while in the {sup 7}Li case an agreement only at a qualitative level is observed. (orig.)

  9. Dynamical 3-Space Predicts Hotter Early Universe: Resolves CMB-BBN 7-Li and 4-He Abundance Anomalies

    Directory of Open Access Journals (Sweden)

    Cahill R. T.

    2010-01-01

    Full Text Available The observed abundances of 7-Li and 4-He are significantly inconsistent with the predictions from Big Bang Nucleosynthesis (BBN when using the $Lambda$CDM cosmological model together with the value for $Omega_B h^2 = 0.0224pm0.0009$ from WMAP CMB fluctuations, with the value from BBN required to fit observed abundances being $0.009 < Omega_B h^2 < 0.013$. The dynamical 3-space theory is shown to predict a 20% hotter universe in the radiation-dominated epoch, which then results in a remarkable parameter-free agreement between the BBN and the WMAP value for $Omega_B h^2$. The dynamical 3-space also gives a parameter-free fit to the supernova redshift data, and predicts that the flawed $Lambda$CDM model would require $Omega_Lambda = 0.73$ and $Omega_M = 0.27$ to fit the 3-space dynamics Hubble expansion, and independently of the supernova data. These results amount to the discovery of new physics for the early universe that is matched by numerous other successful observational and experimental tests.

  10. Dynamical 3-Space Predicts Hotter Early Universe: Resolves CMB-BBN 7-Li and 4-He Abundance Anomalies

    Directory of Open Access Journals (Sweden)

    Cahill R. T.

    2010-01-01

    Full Text Available The observed abundances of 7 Li and 4 He are significantly inconsistent with the pre- dictions from Big Bang Nucleosynthesis (BBN when using the CDM cosmolog- ical model together with the value for B h 2 = 0 : 0224 0 : 0009 from WMAP CMB fluctuations, with the value from BBN required to fit observed abundances being 0 : 009 < B h 2 < 0 : 013. The dynamical 3-space theory is shown to predict a 20% hot- ter universe in the radiation-dominated epoch, which then results in a remarkable parameter-free agreement between the BBN and the WMAP value for B h 2 . The dy- namical 3-space also gives a parameter-free fit to the supernova redshift data, and pre- dicts that the flawed CDM model would require = 0 : 73 and M = 0 : 27 to fit the 3-space dynamics Hubble expansion, and independently of the supernova data. These results amount to the discovery of new physics for the early universe that is matched by numerous other successful observational and experimental tests.

  11. Excitation function shape and neutron spectrum of the 7Li(p ,n )7Be reaction near threshold

    Science.gov (United States)

    Martín-Hernández, Guido; Mastinu, Pierfrancesco; Maggiore, Mario; Pranovi, Lorenzo; Prete, Gianfranco; Praena, Javier; Capote-Noy, Roberto; Gramegna, Fabiana; Lombardi, Augusto; Maran, Luca; Scian, Carlo; Munaron, Enrico

    2016-09-01

    The forward-emitted low energy tail of the neutron spectrum generated by the 7Li(p ,n )7Be reaction on a thick target at a proton energy of 1893.6 keV was measured by time-of-flight spectroscopy. The measurement was performed at BELINA (Beam Line for Nuclear Astrophysics) of the Laboratori Nazionali di Legnaro. Using the reaction kinematics and the proton on lithium stopping power the shape of the excitation function is calculated from the measured neutron spectrum. Good agreement with two reported measurements was found. Our data, along with the previous measurements, are well reproduced by the Breit-Wigner single-resonance formula for s -wave particles. The differential yield of the reaction is calculated and the widely used neutron spectrum at a proton energy of 1912 keV was reproduced. Possible causes regarding part of the 6.5% discrepancy between the 197Au(n ,γ ) cross section measured at this energy by Ratynski and Kappeler [Phys. Rev. C 37, 595 (1988), 10.1103/PhysRevC.37.595] and the one obtained using the Evaluated Nuclear Data File version B-VII.1 are given.

  12. Interaction of loosely bound radioactive {sup 7}Be and stable {sup 7}Li with {sup 9}Be

    Energy Technology Data Exchange (ETDEWEB)

    Verma, S.; Mandal, S.; Ranjit,; Datta, S.K.; Singh, R. [University of Delhi, Department of Physics and Astrophysics, Delhi (India); Das, J.J.; Jhingan, A.; Golda, K.S.; Madhavan, N.; Sugathan, P.; Nath, S.; Varughese, T.; Gehlot, J. [Inter University Accelerator Centre, New Delhi (India); Kalita, K.; Barua, S. [Gauhati University, Department of Physics, Guwahati (India); Sahu, P.K.; John, B.; Nayak, B.K.; Jha, V.; Saxena, A. [Bhabha Atomic Research Centre, Nuclear Physics Division, Mumbai (India)

    2010-06-15

    Quasielastic scattering angular distributions have been measured for the {sup 7}Be+{sup 9}Be system at E{sub lab} = 17, 19 and 21MeV in the angular range {theta}{sub cm}=24 - 57 . An optical model (OM) analysis of these data has been carried out in order to extract optical potential parameters and reaction cross-sections. One-proton stripping cross-sections were also measured for this system at E{sub lab} = 19 and 21MeV. These transfer angular-distribution data were compared with the finite-range distorted-wave Born approximation (FRDWBA) calculations. For the {sup 7}Li+{sup 9}Be system quasielastic scattering angular distributions were measured and emitted light charged particles were detected at E{sub lab} = 15.75, 24.00 and 30.00MeV in the angular range {theta}{sub cm} = 7 - 70 . Fusion cross-sections were obtained by reproducing the measured {alpha} -evaporation spectra from the compound nucleus at backward angles with the statistical model calculations. The ratios of the experimental fusion cross-sections to the total reaction cross-sections (obtained from OM analysis) were found to be small. This result suggests that the break-up process has a strong influence on the fusion process leading to a reduction in the fusion cross-section. (orig.)

  13. Measurement of Nuclear Reaction Q-values with High Accuracy: 7Li(p, n)7Be

    Science.gov (United States)

    White, R. E.; Barker, P. H.; Lovelock, D. M. J.

    1985-01-01

    A technique is described for the measurement of nuclear reaction Q-values with an accuracy of a few parts in 105, in which the ultimate reference is a one-volt standard. As a test of the technique the accurately known threshold energy of the 7Li(p, n)7Be reaction, 1880.51 +/- 0.08 keV, has been remeasured. The value found using the present technique is 1880.443 +/- 0.020 keV, in good agreement with previous values. An attempt to see evidence for atomic excitation effects in the 27A1(p,n)27Si reaction is also discussed. This yielded a new value of 5803.73 +/- 0.12 keV for the threshold of this reaction, again in a good agreement with, but more accurate than, previous values. Further test measurements are summarized. The main application of the technique, in measurements related to the theory of weak interactions, is discussed briefly and the results obtained to date are presented.

  14. Thiol-thione tautomeric analysis, spectroscopic (FT-IR, Laser-Raman, NMR and UV-vis) properties and DFT computations of 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule.

    Science.gov (United States)

    Gökce, Halil; Öztürk, Nuri; Ceylan, Ümit; Alpaslan, Yelda Bingöl; Alpaslan, Gökhan

    2016-06-15

    In this study, the 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule (C7H6N4S) molecule has been characterized by using FT-IR, Laser-Raman, NMR and UV-vis spectroscopies. Quantum chemical calculations have been performed to investigate the molecular structure (thione-thiol tautomerism), vibrational wavenumbers, electronic transition absorption wavelengths in DMSO solvent and vacuum, proton and carbon-13 NMR chemical shifts and HOMOs-LUMOs energies at DFT/B3LYP/6-311++G(d,p) level for all five tautomers of the title molecule. The obtained results show that the calculated vibrational wavenumbers, NMR chemical shifts and UV-vis wavelengths are in a good agreement with experimental data. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Thiol-thione tautomeric analysis, spectroscopic (FT-IR, Laser-Raman, NMR and UV-vis) properties and DFT computations of 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule

    Science.gov (United States)

    Gökce, Halil; Öztürk, Nuri; Ceylan, Ümit; Alpaslan, Yelda Bingöl; Alpaslan, Gökhan

    2016-06-01

    In this study, the 5-(3-pyridyl)-4H-1,2,4-triazole-3-thiol molecule (C7H6N4S) molecule has been characterized by using FT-IR, Laser-Raman, NMR and UV-vis spectroscopies. Quantum chemical calculations have been performed to investigate the molecular structure (thione-thiol tautomerism), vibrational wavenumbers, electronic transition absorption wavelengths in DMSO solvent and vacuum, proton and carbon-13 NMR chemical shifts and HOMOs-LUMOs energies at DFT/B3LYP/6-311 ++G(d,p) level for all five tautomers of the title molecule. The obtained results show that the calculated vibrational wavenumbers, NMR chemical shifts and UV-vis wavelengths are in a good agreement with experimental data.

  16. NMR GHZ

    CERN Document Server

    Laflamme, R; Zurek, W H; Catasti, P; Mariappan, S V S

    1998-01-01

    We describe the creation of a Greenberger-Horne-Zeilinger (GHZ) state of the form |000>+|111> (three maximally entangled quantum bits) using Nuclear Magnetic Resonance (NMR). We have successfully carried out the experiment using the proton and carbon spins of trichloroethylene, and confirmed the result using state tomography. We have thus extended the space of entangled quantum states explored systematically to three quantum bits, an essential step for quantum computation.

  17. The inelastic scattering neutron angular distribution of reaction 7Li(n,n'γ) 7Li ∗ (478 keV) derived from shape analysis of the Doppler broadened γ spectra at 9, 9.5 and 10 MeV

    Science.gov (United States)

    Feizeng, Huang; Shanglian, Bao; Jinquan, Liu; Wentian, Cao; Zhengde, Huang; Lihua, Zhu; Long, Hou

    1995-02-01

    The angular distributions of the inelastic scattered neutrons from the reaction 7Li(n,n'γ) 7Li ∗ (478 keV) were derived from the shape analysis of the Doppler broadened γ spectra at incident neutron energies of 9, 9.5 and 10 MeV. The measured spectra were fitted to the Monte Carlo simulation results to get the Legendre coefficients of the angular distributions of the inelastic neutron scattering in the center-of-mass (CM) system. The derived results are compared with DWBA calculations. The agreements are rather good.

  18. Neutron beam optimization based on a 7Li(p,n)7Be reaction for treatment of deep-seated brain tumors by BNCT

    Science.gov (United States)

    Zahra Ahmadi, Ganjeh; S. Farhad, Masoudi

    2014-10-01

    Neutron beam optimization for accelerator-based Boron Neutron Capture Therapy (BNCT) is investigated using a 7Li(p,n)7Be reaction. Design and optimization have been carried out for the target, cooling system, moderator, filter, reflector, and collimator to achieve a high flux of epithermal neutron and satisfy the IAEA criteria. Also, the performance of the designed beam in tissue is assessed by using a simulated Snyder head phantom. The results show that the optimization of the collimator and reflector is critical to finding the best neutron beam based on the 7Li(p,n)7Be reaction. Our designed beam has 2.49×109n/cm2s epithermal neutron flux and is suitable for BNCT of deep-seated brain tumors.

  19. Synthesis and optical characterization of LiKB4O7, Li2B6O10, and LiCsB6O10 glasses

    Energy Technology Data Exchange (ETDEWEB)

    Adamiv, V.; Teslyuk, I.; Dyachok, Ya.; Romanyuk, G.; Krupych, O.; Mys, O.; Martynyuk-Lototska, I.; Burak, Ya.; Vlokh, R.

    2010-10-01

    In the current work we report on the synthesis of LiKB4O7, Li2B6O10, and LiCsB6O10 borate glasses. The results for their piezo-optic, acousto-optic, acoustic, elastic, refractive, optical transmission, and optical resistance properties are also presented. It is shown that some of these glasses represent efficient acousto-optic materials that are transparent down to the vacuum ultraviolet range and highly resistant to laser radiation.

  20. Synthesis and optical characterization of LiKB4O7, Li2B6O10, and LiCsB6O10 glasses.

    Science.gov (United States)

    Adamiv, V; Teslyuk, I; Dyachok, Ya; Romanyuk, G; Krupych, O; Mys, O; Martynyuk-Lototska, I; Burak, Ya; Vlokh, R

    2010-10-01

    In the current work we report on the synthesis of LiKB(4)O(7), Li(2)B(6)O(10), and LiCsB(6)O(10) borate glasses. The results for their piezo-optic, acousto-optic, acoustic, elastic, refractive, optical transmission, and optical resistance properties are also presented. It is shown that some of these glasses represent efficient acousto-optic materials that are transparent down to the vacuum ultraviolet range and highly resistant to laser radiation.

  1. Indirect determination of Li via 74Ge(n,γ)75mGe activation reaction induced by neutrons from 7Li(p,n)7Be reaction

    Science.gov (United States)

    Kumar, Sanjiv; Reddy, G. L. N.; Rao, Pritty; Verma, Rakesh; Ramana, J. V.; Vikramkumar, S.; Raju, V. S.

    2012-03-01

    An indirect method to determine Li by 74Ge(n,γ)75mGe activation reaction induced in a high purity Ge (detector) crystal by neutrons from the 7Li(p,n)7Be reaction in a typical particle-induced γ-ray emission (PIGE) spectroscopy experimental set-up is described. Performed with proton beams of energies in excess of 1.88 MeV, the threshold energy (Eth) of the 7Li(p,n)7Be reaction, the determination involves the activity measurement of 75mGe isotope that has a half-life of 47.7 s and decays with the emission of 139 keV γ-rays. Rapidity, selectivity and sensitivity down to ppm levels are the attractive features of the method. It is a suitable alternative to 7Li(p,p'γ)7Li reaction based PIGE technique in the analyses of matrices that contain light elements such as Be, B, F, Na and Al in significant proportions. Interferences can arise from elements, for example V and Ti, that have Eth ⩽ 1.88 MeV for (p,n) reaction. In the case of elements such as Cu, Mo which have with Eth > 1.88 MeV, the incident proton beam energy can be judiciously selected to avoid or minimize an interference. The method, under optimized irradiation conditions, does not entail a risk of neutron stimulated degradation of the performance of the detector. Besides analytical purposes, the measurement of the 75mGe activity can serve as a powerful tool to monitor even low (˜25 n/cm2 s) thermal neutron fluxes.

  2. Optical Potential Parameters for Halo Nucleus System 6He+12C from Transfer Reaction11B (7Li, 6He) 12C

    Institute of Scientific and Technical Information of China (English)

    WU Zhen-Dong; XU Xin-Xing; BAI Chun-Lin; YU Ning; JIA Fei; LIN Cheng-Jian; ZHANG Huan-Qiao; LIU Zu-Hua; YANG Feng; AN Guang-Peng; ZHANG Chun-Lei; ZHANG Gao-Long; JIA Hui-Ming

    2009-01-01

    The optical potential parameters for the halo nucleus system 6He+12 C are extracted from fits to the measured angular distributions of 11B(7 Li, 6He)12C reaction at energies of 18.3 and 28.3 MeV with distorted-wave Born approximation analysis. The characters of the obtained optical potential parameters are basically consistent with the results extracted from the fits to the elastic-scattering angular distributions in the literature.

  3. Test of special relativity theory by means of laser spectroscopy on relativistic {sup 7}Li{sup +} ions in the ESR; Test der Speziellen Relativitaetstheorie mittels Laserspektroskopie an relativistischen {sup 7}Li{sup +}-Ionen am ESR

    Energy Technology Data Exchange (ETDEWEB)

    Botermann, Benjamin

    2012-10-31

    The invariance under Lorentz transformation of the laws of physics is a fundamental postulate of modern physics and all theories of the fundamental interactions have been stated in a covariant form. Although the theory of Special Relativity (SR) has been tested and confirmed with high accuracy in a large number of experiments, improved tests are of fundamental interest due to the far-reaching relevance of this postulate. Additionally modern attempts of a unified description of the four fundamental interactions point to possible violations of Lorentz invariance. In this context experiments of the Ives-Stilwell type for a test of time dilation play an important role. High resolution laser spectroscopy is applied on relativistic particle beams to investigate the validity of the relativistic Doppler formula - and therefore of the time dilation factor γ. In the course of this thesis an Ives-Stilwell experiment was performed with {sup 7}Li{sup +} ions at a velocity of 34 % of the speed of light, which were stored at the experimental storage ring (ESR) of the GSI Helmholtzzentrum fuer Schwerionenforschung. The techniques of Λ- as well as saturation spectroscopy were employed on the 1s2s{sup 3}S{sub 1}→1s2p{sup 3}P{sub 2} transition. By a computer based analysis of the fluorescence detection system and utilization of appropriate edge filters the signal to noise ratio was decisively improved and the application of an additional pump laser allowed for the observation of a saturation signal for the first time. The frequency stability of both laser systems was specified by means of a frequency comb to obtain the highest possible accuracy. The data from the beam times were analyzed in the frameworks of the Robertson-Mansouri-Sexl test theory (RMS) and the Standard Model Extension (SME) and the corresponding upper limits of the relevant test parameters of the assigned theories were calculated. The upper limit of the parameter α was improved by a factor of 4 compared to

  4. Synthesis, NMR spectroscopic characterization and structure of a divinyldisilazane-(triphenylphosphine)platinum(0) complex: observation of isotope-induced chemical shifts (1)Δ(12/13)C((195)Pt).

    Science.gov (United States)

    Wrackmeyer, Bernd; Klimkina, Elena V; Schmalz, Thomas; Milius, Wolfgang

    2013-05-01

    Tetramethyldivinyldisilazane-(triphenylphosphine)platinum(0) was prepared, characterized in solid state by X-ray crystallography and in solution by multinuclear magnetic resonance spectroscopy ((1)H, (13)C, (15)N, (29)Si, (31)P and (195)Pt NMR). Numerous signs of spin-spin coupling constants were determined by two-dimensional heteronuclear shift correlations (HETCOR) and two-dimensional (1)H/(1)H COSY experiments. Isotope-induced chemical shifts (1)Δ(12/13)C((195)Pt) were measured from (195)Pt NMR spectra of the title compound as well as of other Pt(0), Pt(II) and Pt(IV) compounds for comparison. In contrast to other heavy nuclei such as (199)Hg or (207)Pb, the "normal" shifts of the heavy isotopomers to low frequencies are found, covering a range of >500 ppb.

  5. Gamow shell model description of radiative capture reactions $^6$Li$(p,\\gamma)$$^7$Be and $^6$Li$(n,\\gamma)$$^7$Li

    CERN Document Server

    Dong, G X; Fossez, K; Płoszajczak, M; Jaganathen, Y; Betan, R M Id

    2016-01-01

    According to standard stellar evolution, lithium abundance is believed to be a useful indicator of the stellar age. However, many evolved stars like red giants show huge fluctuations around expected theoretical abundances that are not yet fully understood. The better knowledge of nuclear reactions that contribute to the creation and destruction of lithium can help to solve this puzzle. In this work we apply the Gamow shell model (GSM) formulated in the coupled-channel representation (GSM-CC) to investigate the mirror radiative capture reactions $^6$Li$(p,\\gamma)$$^7$Be and $^6$Li$(n,\\gamma)$$^7$Li. The cross-sections are calculated using a translationally invariant Hamiltonian with the finite-range interaction which is adjusted to reproduce spectra, binding energies and one-nucleon separation energies in $^{6-7}$Li, $^7$Be. All relevant $E1$, $M1$, and $E2$ transitions from the initial continuum states to the final bound states $J={3/2}_1^-$ and $J={1/2}^-$ of $^7$Li and $^7$Be are included. We demonstrate th...

  6. High-resolution NMR spectroscopy under the fume hood.

    Science.gov (United States)

    Küster, Simon K; Danieli, Ernesto; Blümich, Bernhard; Casanova, Federico

    2011-08-07

    This work reports the possibility to acquire high-resolution (1)H NMR spectra with a fist-sized NMR magnet directly installed under the fume hood. The small NMR sensor based on permanent magnets was used to monitor the trimerization of propionaldehyde catalyzed by indium trichloride in real time by continuously circulating the reaction mixture through the magnet bore in a closed loop with the help of a peristaltic pump. Thanks to the chemical selectivity of NMR spectroscopy the progress of the reaction can be monitored on-line by determining the concentrations of both reactant and product from the area under their respective lines in the NMR spectra as a function of time. This in situ measurement demonstrates that NMR probes can be used in chemistry laboratories, e.g. for reaction optimization, or installed at specific points of interest along industrial process lines. Therefore, it will open the door for the implementation of feedback control based on spectroscopic NMR data.

  7. One-Pot Synthesis, X-Ray Diffraction and MAS NMR Spectroscopic Study of Gallosilicate Nitrate Cancrinite Na8[GaSiO4]6(NO34(H2O6

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2010-01-01

    Full Text Available One-pot synthetic gallosilicate nitrate cancrinite (CAN framework topology have been synthesized under hydrothermal conditions at 100 °C. The synthesized product was characterized by, X-ray powder diffraction, IR, Raman and 29Si, 23Na MAS NMR spectroscopy, SEM and thermogravimetry. The crystal structure refinement of pure nitrate cancrinite has been carried out from X-ray data using Rietveld refinement method. Gallosilicate cancrinite Na8[GaSiO4]6(NO34(H2O6 crystalline hexagonal with space group P63 and a = 12.77981 Å (2, c = 5.20217 Å (1, (Rwp = 0.0696 Rp = 0.0527. The results by MAS NMR spectroscopy confirmed the alternating Si, Ga ordering of the gallosilicate framework for a Si/Ga ratio of 1.0. A distribution of the quadrupolar interaction of the sodium cations caused by the enclatherated water molecules and motional effects can be suggested from the 23Na MAS NMR. Thermogravimetric investigation shows the extent of nitrate entrapment, stability within the cancrinite cage and decomposition properties. SEM clearly shows the hexagonal needle shaped crystals of nitrate cancrinite.

  8. NMR spectroscopic properties (1H at 500 MHz) of deuterated* ribonucleotide-dimers ApU*, GpC*, partially deuterated 2'-deoxyribonucleotide-dimers d(TpA*), d(ApT*), d(GpC*) and their comparison with natural counterparts (1H-NMR window).

    Science.gov (United States)

    Földesi, A; Nilson, F P; Glemarec, C; Gioeli, C; Chattopadhyaya, J

    1993-02-01

    Pure 1'#,2',3',4'#,5',5''-2H6-ribonucleoside derivatives 10-14, 1'#,2',2'',3',4'#,5',5''-2H7-2'-deoxynucleoside blocks 15-18 and their natural-abundance counterparts were used to assemble partially deuterated ribonucleotide-dimers (* indicates deuteration at 1'#,2',3',4'#,5',5''(2H6)): ApU* 21, GpC* 22 and partially deuterated 2'-deoxyribonucleotide-dimers d(TpA*) 23, d(ApT*) 25, d(GpC*) 26 (* indicates deuteration at 1'#,2',2'',3',4'#,5',5''(2H7)) according to the procedure described by Földesi et al. (Tetrahedron, in press). These five partially deuterated oligonucleotides were subsequently compared with their corresponding natural-abundance counterparts by 500 MHz 1H-NMR spectroscopy to evaluate the actual NMR simplifications achieved in the non-deuterated part (1H-NMR window) as a result of specific deuterium incorporation. Detailed one-dimensional 1H-NMR (500 MHz), two-dimensional correlation spectra (DQF-COSY and TOCSY) and deuterium isotope effect on the chemical shifts of oligonucleotides have been presented.

  9. Spectroscopic (FT-IR, (1)H, (13)C NMR, UV), DOS and orbital overlap population analysis of copper complex of (E)-4-(2-(4-nitrophenyl) diazenyl)-N, N bis ((pyridin-2-yl) methyl) benzamine by density functional theory.

    Science.gov (United States)

    Diwaker

    2015-02-05

    The geometric parameters, chemical shifts, FTIR, NMR and orbital overlap population along with DOS (density of states) to know different kinds of interactions for binding of copper atom with (E)-4-(2-(4-nitrophenyl) diazenyl)-N, N bis ((pyridin-2-yl) methyl) benzamine to form its copper complex has been reported by DFT methods. The theoretically predicted values for structural parameters are in agreement with the experimentally reported values. NMR chemical shifts calculated using B3LYP/DFT/GIAO level of theory gives information about binding of copper atom with three nitrogen atoms namely N (3, 8 and 11). Orbital overlap population analysis using DFT/B3LYP/SDD level of theory is used to study the kind of interactions involved in binding of copper with the three nitrogen atoms. DOS studies are done to know about the contribution of alpha, beta electrons to the valence and conduction band. IR spectroscopy investigations gave the absorption bands for the formation of title compound. Electronic spectrum along with HOMO-LUMO energies of the title compound has been investigated using Time-dependent (TD-DFT) approach.

  10. Synthesis, spectroscopic investigations (FT-IR, NMR, UV-Vis, and TD-DFT), and molecular docking of (E)-1-(benzo[d][1, 3]dioxol-6-yl)-3-(6-methoxynaphthalen-2-yl)prop-2-en-1-one

    Science.gov (United States)

    Therasa Alphonsa, A.; Loganathan, C.; Athavan Alias Anand, S.; Kabilan, S.

    2017-02-01

    The compound (E)-1-(benzo [d] [1, 3] dioxol-6-yl)-3-(6-methoxy naphthalen-2-yl) prop-2-en-1-one (AKN) was synthesized and characterized by FT-IR, NMR, and UV-Vis spectrometer. The optimized molecular geometry, bond lengths, bond angles, atomic charges, harmonic vibrational wave numbers and intensities of vibrational bonds of the title compound have been investigated by Time dependent- Density Functional Theory (TD-DFT) using a standard B3LYP method with 6-31 G (d, p) basis set available in the Gaussian 09W package. 1H and 13C NMR chemical shifts of the molecule were calculated using Gauge-independent atomic orbital method (GIAO). Experimental excitation energies of the molecules were matched with the theoretically calculated energies. The atomic charge distributions of the various atoms present in the AKN were obtained by Mulliken charge population analysis. The Molecular Electrostatic Potential (MEP) analysis reveals the sites for electrophilic attack and nucleophilic reactions in the molecule. The difference between the observed and scaled frequencies was small. The HOMO to LUMO transition implies an electron density transfer. The intramolecular contacts have been interpreted using Natural Bond Orbital (NBO) analysis. The calculation results were applied to simulate spectra of the title compound, which show excellent agreement with observed spectra. To provide information about the interactions between human cytochrome protein and the novel compound theoretically, docking studies were carried out using Schrödinger software.

  11. Ab initio calculation on accurate analytic potential energy functions and harmonic frequencies of c3∑+g and B1∏u states of dimer 7Li2

    Institute of Scientific and Technical Information of China (English)

    Yu Ben-Hai; Shi De-Heng; Sun Jin-Feng; Zhu Zun-Lue; Liu Yu-Fang; Yang Xiang-Dong

    2007-01-01

    The comparison between single-point energy scanning (SPES) and geometry optimization (OPT) in determining the equilibrium geometries of c3∑+g and B1∏u states of dimer 7Li2 is made at numerous basis sets by using a symmetryadapted-cluster configuration-interaction (SAC-CI) method in the Gaussian 03 program package. In this paper the difference of the equilibrium geometries obtained by SPES and by OPT is reported. The results obtained by SPES are found to be more reasonable than those obtained by OPT in full active space at the present SAC-CI level of theory. And the conclusion is attained that the cc-PVTZ is a most suitable basis set for these states. The calculated dissociation energies and equilibrium geometries are 0.8818 eV and 0.3090 nm for c3∑+g state, and 0.3668 eV and 0.2932 nm for B1∏u state respectively. The potential energy curves are calculated over a wide internuclear distance range from about 2.5a0 to 37a0 and have a least-squares fit into the Murrell-Sorbie function. According to the calculated analytic potential energy functions, the harmonic frequencies (ωe) and other spectroscopic data (ωeχe, Be and αe) are calculated. Comparison of the theoretical determinations at present work with the experiments and other theories clearly shows that the present work is the most complete effort and thus represents an improvement over previous theoretical results.

  12. Effects of low-temperature catalytic pretreatments on coal structure and reactivity in liquefaction. Final technical report, Volume 2 - hydrogenative and hydrothermal pretreatments and spectroscopic characterization using pyrolysis-GC-MS, CPMAS {sup 13}C NMR and FT-IR

    Energy Technology Data Exchange (ETDEWEB)

    Chunshan Song; Hatcher, P.G.; Saini, A.K.; Wenzel, K.A.

    1998-01-01

    It has been indicated by DOE COLIRN panel that low-temperature catalytic pretreatment is a promising approach to the development of an improved liquefaction process. This work is a fundamental study on effects of pretreatments on coal structure and reactivity in liquefaction. The main objectives of this project are to study the coal structural changes induced by low-temperature catalytic and thermal pretreatments by using spectroscopic techniques; and to clarify the pretreatment-induced changes in reactivity or convertibility of coals. As the second volume of the final report, here we summarize our work on spectroscopic characterization of four raw coals including two subbituminous coals and two bituminous coals, tetrahydrofuran (THF)-extracted but unreacted coals, the coals (THF-insoluble parts) that have been thermally pretreated. in the absence of any solvents and in the presence of either a hydrogen-donor solvent or a non-donor solvent, and the coals (THF-insoluble parts) that have been catalytically pretreated in the presence of a dispersed Mo sulfide catalyst in the absence of any solvents and in the presence of either a hydrogen-donor solvent or a non-donor solvent.

  13. On the influence of crosslinker on template complexation in molecularly imprinted polymers: a computational study of prepolymerization mixture events with correlations to template-polymer recognition behavior and NMR spectroscopic studies.

    Science.gov (United States)

    Shoravi, Siamak; Olsson, Gustaf D; Karlsson, Björn C G; Nicholls, Ian A

    2014-06-12

    Aspects of the molecular-level basis for the function of ethylene glycol dimethacrylate and trimethylolproprane trimethacrylate crosslinked methacrylic acid copolymers molecularly imprinted with (S)-propranolol have been studied using a series of all-component and all-atom molecular dynamics studies of the corresponding prepolymerization systems. The crosslinking agents were observed to contribute to template complexation, and the results were contrasted with previously reported template-recognition behavior of the corresponding polymers. Differences in the extent to which the two crosslinkers interacted with the functional monomer were identified, and correlations were made to polymer-ligand recognition behavior and the results of nuclear magnetic resonance spectroscopic studies studies. This study demonstrates the importance of considering the functional monomer-crosslinker interaction when designing molecularly imprinted polymers, and highlights the often neglected general contribution of crosslinker to determining the nature of molecularly imprinted polymer-template selectivity.

  14. On the Influence of Crosslinker on Template Complexation in Molecularly Imprinted Polymers: A Computational Study of Prepolymerization Mixture Events with Correlations to Template-Polymer Recognition Behavior and NMR Spectroscopic Studies

    Directory of Open Access Journals (Sweden)

    Siamak Shoravi

    2014-06-01

    Full Text Available Aspects of the molecular-level basis for the function of ethylene glycol dimethacrylate and trimethylolproprane trimethacrylate crosslinked methacrylic acid copolymers molecularly imprinted with (S-propranolol have been studied using a series of all-component and all-atom molecular dynamics studies of the corresponding prepolymerization systems. The crosslinking agents were observed to contribute to template complexation, and the results were contrasted with previously reported template-recognition behavior of the corresponding polymers. Differences in the extent to which the two crosslinkers interacted with the functional monomer were identified, and correlations were made to polymer-ligand recognition behavior and the results of nuclear magnetic resonance spectroscopic studies studies. This study demonstrates the importance of considering the functional monomer–crosslinker interaction when designing molecularly imprinted polymers, and highlights the often neglected general contribution of crosslinker to determining the nature of molecularly imprinted polymer-template selectivity.

  15. Vibrational spectroscopic studies, NMR, HOMO-LUMO, NLO and NBO analysis of 1-(2-nitrobenzoyl)-3,5-diphenyl-4,5-dihydro-1H-pyrazole with use X-ray diffractions and DFT calculations

    Science.gov (United States)

    Demir, Sibel; Tinmaz, Feyza; Dege, Necmi; Ilhan, Ilhan Ozer

    2016-03-01

    The crystal and molecular structure of the title compound, 1-(2-nitrobenzoyl)-3,5-diphenyl-4,5-dihydro-1H-pyrazole, was reported and confirmed by single crystal X-ray diffraction and spectroscopic data. The structure, geometry optimization, vibrational frequencies and nuclear magnetic resonance were also investigated. Stability of the molecule arising from hyperconjugative interactions and charge delocalisation was analysed using natural bond orbital analysis. The results show that charge in electron density (ED) in the σ∗ and π∗ antibonding orbitals and second-order delocalisation energies E(2) confirms the occurrence of intramolecular charge transfer within the molecule. Satisfactory theoretical aspects were made for the stable conformer of the molecule using density functional theory DFT-B3LYP methods with the 6-311G++(d,p) basis set.

  16. $\\Sigma^- p$ emission rates in $K^-$ absorptions at rest on $^6$Li, $^7$Li, $^{9}$Be, $^{13}$C and $^{16}$O

    CERN Document Server

    Agnello, M; Bertani, M; Bonomi, G; Botta, E; Bregant, M; Bressani, T; Bufalino, S; Busso, L; Calvo, D; Camerini, P; Dalena, B; De Mori, F; D'Erasmo, G; Feliciello, A; Filippi, A; Fiore, E M; Fontana, A; Fujioka, H; Genova, P; Gianotti, P; Grion, N; Lucherini, V; Marcello, S; Morra, O; Nagae, T; Outa, H; Pantaleo, A; Paticchio, V; Piano, S; Rui, R; Simonetti, G; Wheadon, R; Zenoni, A

    2015-01-01

    An experimental study of the $K^-_{stop}A\\rightarrow \\Sigma^- p A'$ reaction on $A=^6$Li, $^7$Li, $^9$Be, $^{13}$C and $^{16}$O $p$-shell nuclei is presented. The data were collected by the FINUDA spectrometer operating at the DA$\\Phi$NE $\\phi$-factory (LNF-INFN, Italy). Emission rates for the reaction in the mentioned nuclei are measured and compared with the few existing data. The spectra of several observables are discussed; indications of Quasi-Free absorptions by a $(np)$ pair embedded in the $A$ nucleus can be obtained from the study of the missing mass distributions.

  17. All-optical production of dual Bose-Einstein condensates of paired fermions and bosons with 6Li and 7Li

    Science.gov (United States)

    Ikemachi, Takuya; Ito, Aki; Aratake, Yukihito; Chen, Yiping; Koashi, Masato; Kuwata-Gonokami, Makoto; Horikoshi, Munekazu

    2017-01-01

    We report the first all-optical production of dual Bose-Einstein condensates (BECs) of paired 6Li (fermion) and one spin state of 7Li (boson) at the magnetic field where the s-wave interactions between fermions are resonant. Fermions are cooled efficiently by evaporative cooling and they serve as coolant for bosons. As a result, the dual condensates can be achieved by using a simple experimental apparatus and procedures, as in the case of the all-optical production of a single BEC. We show that the all-optical method enables us to realize variety of ultracold Bose-Fermi mixtures.

  18. Präparation eines reinen metastabilen 7 Li +-Ionenstrahls für die Präzisionsspektroskopie im Speicherring

    OpenAIRE

    Merz, Peter

    2000-01-01

    An dem Schwerionenspeicherring TSR (MPI für Kernphysik, Heidelberg) wurde ein 7 Li +-Ionenstrahl geringer Dichte durch RF-Bunchen und Laserkühlung präpariert.Die Phasenraumverteilung in dem Strahl wurde durch Laser- spektroskopie an Ionen im metastabilen Zustand untersucht. Ein umlaufsynchrones, zeitaufgelöstes Meßverfahren für das Fluoreszenzlicht ermöglichte die Bestimmung der räumlichen Struktur mit dieser rein optischen Methode.Durch einen speziellen Präparationsschritt wurden die Ionen i...

  19. Measurements of double-differential neutron emission cross sections of {sup 6}Li and {sup 7}Li for 18 MeV neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Ibaraki, Masanobu; Baba, Mamoru; Matsuyama, Shigeo; Sanami, Toshiya; Win, T.; Miura, Takako; Hirakawa, Naohiro [Tohoku Univ., Sendai (Japan). Faculty of Engineering

    1997-03-01

    Double-differential neutron emission cross sections of {sup 6}Li and {sup 7}Li were measured for 18 MeV neutrons at Tohoku University 4.5 MV Dynamitron facility. Neutron emission spectra were obtained down to 1 MeV at 13 angles with energy resolution good enough to separate discrete levels. A care was taken to eliminate the sample-dependent background due to parasitic neutrons. Experimental results were in fair agreement with the JENDL-3.2 data and a simple model considering a three-body breakup process and discrete level excitations. (author)

  20. Spectroscopic data

    CERN Document Server

    Melzer, J

    1976-01-01

    During the preparation of this compilation, many people contributed; the compilers wish to thank all of them. In particular they appreciate the efforts of V. Gilbertson, the manuscript typist, and those of K. C. Bregand, J. A. Kiley, and W. H. McPherson, who gave editorial assistance. They would like to thank Dr. J. R. Schwartz for his cooperation and encouragement. In addition, they extend their grati­ tude to Dr. L. Wilson of the Air Force Weapons Laboratory, who gave the initial impetus to this project. v Contents I. I ntroduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 . . . . . . . . . . . . . . . . 11. Organization ofthe Spectroscopic Table. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Methods of Production and Experimental Technique . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 Band Systems . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2...

  1. Manufacture and experimental testing of a technological demonstrator to extraction of tritium for loop systems Pb (15.7)Li of the ITER TMB by permeation against vacuum; Fabricacion y pruebas experimentales de un demostrador tecnologico de extraccion de tritio para los sistemas de lazo de Pb (15,7)Li de los TMB de ITER mediante permeacion contra vacio

    Energy Technology Data Exchange (ETDEWEB)

    Sacristan, R.; Bonjoch, I.; Sedano, L.; Veredas, G.

    2012-07-01

    Currently permeation against vacuum (PAV) using technology more promising in terms of the recovery of tritium from the beds of liquid metals, the objective of this work is the development and construction of a technology demonstrator than through a PAV with appropriate design maximize the removal of H2 of a loop Pb (15,7) Li, qualifying in terms of efficiency, the possible application for the extraction of T/D2 in the loops of future fusion reactors.

  2. Low-temperature UV-visible and NMR spectroscopic investigations of O(2) binding to ((6)L)Fe(II), a ferrous heme bearing covalently tethered axial pyridine ligands.

    Science.gov (United States)

    Ghiladi, Reza A; Karlin, Kenneth D

    2002-05-06

    In this report, we describe the reversible dioxygen reactivity of ((6)L)Fe(II) (1) [(6)L = partially fluorinated tetraphenylporphyrin with covalently appended TMPA moiety; TMPA = tris(2-pyridylmethyl)amine] using a combination of low-temperature UV-vis and multinuclear ((1)H and (2)H) NMR spectroscopies. Complex 1, or its pyrrole-deuterated analogue ((6)L-d(8))Fe(II) (1-d(8)), exhibits downfield shifted pyrrole resonances (delta 28-60 ppm) in all solvents utilized [CH(2)Cl(2), (CH(3))(2)C(O), CH(3)CN, THF], indicative of a five-coordinate high-spin ferrous heme, even when there is no exogenous axial solvent ligand present (i.e., in methylene chloride). Furthermore, ((6)L)Fe(II) (1) exhibits non-pyrrolic upfield and downfield shifted peaks in CH(2)Cl(2), (CH(3))(2)C(O), and CH(3)CN solvents, which we ascribed to resonances arising from the intra- or intermolecular binding of a TMPA-pyridyl arm to the ferrous heme. Upon exposure to dioxygen at 193 K in methylene chloride, ((6)L)Fe(II) (1) [UV-vis: lambda(max) = 433 (Soret), 529 (sh), 559 nm] reversibly forms a dioxygen adduct [UV-vis: lambda(max) = 422 (Soret), 542 nm], formulated as the six-coordinate low-spin [delta(pyrrole) 9.3 ppm, 193 K] heme-superoxo complex ((6)L)Fe(III)-(O(2)(-)) (2). The coordination of the tethered pyridyl arm to the heme-superoxo complex as axial base ligand is suggested. In coordinating solvents such as THF, reversible oxygenation (193 K) of ((6)L)Fe(II) (1) [UV-vis: lambda(max) = 424 (Soret), 542 nm] also occurs to give a similar adduct ((6)L)Fe(III)-(O(2)(-)) (2) [UV-vis: lambda(max) = 418 (Soret), 537 nm. (2)H NMR: delta(pyrrole) 8.9 ppm, 193 K]. Here, we are unable to distinguish between a bound solvent ligand or tethered pyridyl arm as axial base ligand. In all solvents, the dioxygen adducts decompose (thermally) to the ferric-hydroxy complex ((6)L)Fe(III)-OH (3) [UV-vis: lambda(max) = 412-414 (Soret), 566-575 nm; approximately delta(pyrrole) 120 ppm at 193 K]. This study on the O(2

  3. Measurement of $^{7}$Be(n,$\\alpha$)$^{4}$He and $^{7}$Be(n,p)$^{7}$Li cross-sections for the Cosmological Lithium Problem

    CERN Multimedia

    We propose to measure in the second experimental area of n TOF the $^{7}$Be(n,$\\alpha$)$^{4}$He and $^{7}$Be(n,p)$^{7}$Li reaction in a wide energy range. Both reactions are of interest for the long- standing "Cosmological $^{7}$Li problem" in Big Bang Nucleosynthesis (BBN). The very high specific activity of $^{7}$Be, and the low cross section of the (n,$\\alpha$) reaction make this measurement extremely dicult. As afirst step, we request some beam time for detector tests at EAR2. For the $^{7}$Be(n,p) reaction, previously measured up to 13 keV, the diculty is mostly associated withthe availability of a high-purity $^{7}$Be sample. To this purpose we ask for three shifts of offline ISOLDE mass separation for the preparation of the sample to be used at n TOF. To this end, a prior endorsement by INTC of the scientific validity and feasibility of the proposed measurement is requested, to start activity on the sample production. The present proposal is part of a wider collaborative effort aimed at measuring neutr...

  4. Folding model analysis of sup 6 sup , sup 7 Li elastic scattering at 12.5-53 MeV/u

    CERN Document Server

    El-Azab-Farid, M

    2002-01-01

    sup 6 sup , sup 7 Li-nucleus double-folding optical potentials have been constructed using the JLM and a gaussian shape of the effective nucleon-nucleon interaction. Angular distributions of the differential cross sections of sup 6 sup , sup 7 Li elastic scattering from sup 1 sup 2 C, sup 2 sup 8 Si, sup 4 sup 0 Ca, sup 5 sup 8 Ni, sup 9 sup 0 Zr and sup 2 sup 0 sup 8 Pb targets at 12.5-53 MeV/u were analyzed using the derived potentials. An energy-dependent reducing renormalization coefficient was required for the real component of the JLM optical potential in order to obtain successful predictions of the observed cross sections even when the projectile density-dependence was considered. A similar behavior was found for calculations based on the density-independent gaussian version of the effective nucleon-nucleon interaction. However, no renormalization was needed when a density-dependence approximation was involved. The energy- and target mass number-dependence in the renormalization factor, real volume in...

  5. Corrosion resistance of Al-based coatings in flowing Pb–15.7Li produced by aluminum electrodeposition from ionic liquids

    Directory of Open Access Journals (Sweden)

    Sven-Erik Wulf

    2016-12-01

    Full Text Available Reduced activation ferritic–martensitic steels are intended to serve as structural materials in different blanket designs, e.g. HCLL, DCLL and WCLL. In these designs the material is supposed to be in direct contact with the flowing liquid breeder material Pb–15.7Li at an operating temperature of up to 550°C. These conditions will lead to severe corrosion attack of the steel and high corrosion rates of up to 400µm per year are reported in the literature. To avoid or reduce corrosion Al-based corrosion barriers were developed in the last years by using electrochemical techniques to deposit aluminum. Until now two processes have been developed. The first one, so called ECA process, is based on volatile toluene electrolytes. Long-term corrosion experiments on these coatings indicated reduced corrosion rates compared to bare Eurofer steel in flowing Pb–15.7Li. However, these Fe–Al scales showed inhomogeneous corrosion attack of the corrosion barrier itself. In this study the improved ECX process was applied to produce Al-based coatings. The short-term corrosion behavior of such barrier coatings was analyzed for up to 4000h by diameter measurements and metallographic examinations. The investigation revealed uniform corrosion in comparison to inhomogeneous attack in case of ECA coated samples and reduced corrosion rates of around 20µm/a even for low exposure times of 4000h.

  6. $\\gamma$ -spectroscopy of n-rich $^{95,96}$Rb nuclei by the incomplete fusion reaction of $^{94}$Kr on $^{7}$Li

    CERN Multimedia

    We propose an experiment with MINIBALL coupled to T-REX to investigate n-rich $^{95,96}$Rb nuclei by the incomplete fusion reaction of $^{94}$Kr on $^{7}$Li. The nuclei of interest will be populated by transfer of a triton into $^{94}$Kr, forming the excited $^{97}$Rb nucleus, followed by the emission of an alpha particle, which will be detected in the Si telescopes of T-REX. The $^{97}$Rb product will evaporate 1 or 2 (with the highest probability) neutrons leading to $^{96}$Rb or $^{95}$Rb, respectively. The aim of the experiment is twofold: \\\\ i) to perform a $\\gamma$- spectroscopy study of $^{95,96}$Rb nuclei with N=58,59, the structure of which is of particular interest in investigating the transition towards stable deformation at N=60, \\\\ ii) to acquire experience in using incomplete fusion reactions with the weakly bound $^{7}$Li target, in order to perform, at a later stage with HIE-ISOLDE, similar measurements induced by n-rich radioactive beams of Sn and Hg, for which at least 5 MeV/nucleon are need...

  7. The 181Ta(7Li,5n)183Os reaction: Measurement and analysis of the excitation function and isomeric cross-section ratios

    Science.gov (United States)

    Ismail, M.; Sharma, R. P.; Rashid, M. H.

    1998-03-01

    Excitation function and isomeric cross-section ratios for the production of 183Osm,g by 7Li-induced reactions on 181Ta are obtained from the measurements of the residual activities by the conventional stacked-foils technique from threshold to 50 MeV. The excitation function and isomeric cross-section ratios for nuclear reaction 181Ta(7Li,5n)183Osm,g are compared with the theoretical statistical model calculation by using the ALICE/91, STAPRE, and CASCADE codes. In the energy range of the present measurement the excitation functions are fitted fairly well by both the geometry dependent hybrid (GDH) model and the hybrid model of Blann with initial exciton number n0=7 (nn=4, np=3, nh=0) using the ALICE/91 code. The experimental isomeric cross-section ratios are also reproduced fairly well by the calculation using the STAPRE code. However, the CASCADE code calculations slightly underpredict the cross section but reproduce the shape. In general, the statistical model under a suitable set of global assumptions, can reproduce the excitation function as well as isomeric cross-section ratios.

  8. Parsec-scale Variations in the 7Li i/6Li i Isotope Ratio Toward IC 348 and the Perseus OB 2 Association

    Science.gov (United States)

    Knauth, D. C.; Taylor, C. J.; Ritchey, A. M.; Federman, S. R.; Lambert, D. L.

    2017-01-01

    Measurements of the lithium isotopic ratio in the diffuse interstellar medium from high-resolution spectra of the Li i λ6708 resonance doublet have now been reported for a number of lines of sight. The majority of the results for the 7Li/6Li ratio are similar to the solar system ratio of 12.2, but the line of sight toward o Per, a star near the star-forming region IC 348, gave a ratio of about two, the expected value for gas exposed to spallation and fusion reactions driven by cosmic rays. To examine the association of IC 348 with cosmic rays more closely, we measured the lithium isotopic ratio for lines of sight to three stars within a few parsecs of o Per. One star, HD 281159, has 7Li/6Li ≃ 2 confirming production by cosmic rays. The lithium isotopic ratio toward o Per and HD 281159 together with published analyses of the chemistry of interstellar diatomic molecules suggest that the superbubble surrounding IC 348 is the source of the cosmic rays. Based on observations obtained with the Hobby-Eberly Telescope, which is a joint project of the University of Texas at Austin, the Pennsylvania State University, Ludwig-Maximilians-Universität München, and Georg-August-Universität Göttingen.

  9. Experimental studies on the neutron emission spectrum and induced radioactivity of the sup 7 Li(d,n) reaction in the 20-40 MeV region

    CERN Document Server

    Baba, M; Hagiwara, M; Sugimoto, M; Miura, T; Kawata, N; Yamadera, A; Orihara, H

    2002-01-01

    To improve the data accuracy of the neutron emission spectrum of the sup 7 Li(d,n) reaction and the radioactivity ( sup 7 Be, sup 3 H, etc.) accumulated in the sup 7 Li target in IFMIF, we have measured the neutron emission spectrum and the radioactivity of sup 7 Be induced in the lithium target for 25 MeV deuterons at the Tohoku University AVF cyclotron (K=110) facility. Neutron spectra were measured with the time-of-flight (TOF) method at four laboratory angles by using a beam swinger system and a well collimated TOF channel. Induced radioactivity was measured by detecting the gamma-rays from sup 7 Be with a pure Ge detector. Experimental results are compared with other experimental data. The present result of neutron emission spectra are in qualitative agreement with other experimental data but that of sup 7 Be production was much larger than expected by the recent codes. Measurement will be extended to several incident energies up to 40 MeV.

  10. Experimental studies on the neutron emission spectrum and induced radioactivity of the {sup 7}Li(d,n) reaction in the 20-40 MeV region

    Energy Technology Data Exchange (ETDEWEB)

    Baba, M. E-mail: babam@cyric.tohoku.ac.jp; Aoki, T.; Hagiwara, M.; Sugimoto, M.; Miura, T.; Kawata, N.; Yamadera, A.; Orihara, H

    2002-12-01

    To improve the data accuracy of the neutron emission spectrum of the {sup 7}Li(d,n) reaction and the radioactivity ({sup 7}Be, {sup 3}H, etc.) accumulated in the {sup 7}Li target in IFMIF, we have measured the neutron emission spectrum and the radioactivity of {sup 7}Be induced in the lithium target for 25 MeV deuterons at the Tohoku University AVF cyclotron (K=110) facility. Neutron spectra were measured with the time-of-flight (TOF) method at four laboratory angles by using a beam swinger system and a well collimated TOF channel. Induced radioactivity was measured by detecting the gamma-rays from {sup 7}Be with a pure Ge detector. Experimental results are compared with other experimental data. The present result of neutron emission spectra are in qualitative agreement with other experimental data but that of {sup 7}Be production was much larger than expected by the recent codes. Measurement will be extended to several incident energies up to 40 MeV.

  11. Molecular structure, spectroscopic (FT-IR, FT-Raman, NMR, UV) studies and first-order molecular hyperpolarizabilities of 1,2-bis(3-methoxy-4-hydroxybenzylidene)hydrazine by density functional method

    Science.gov (United States)

    Subramanian, N.; Sundaraganesan, N.; Jayabharathi, J.

    2010-07-01

    Quantum chemical calculations of energies, geometrical structure and vibrational wavenumbers of 1,2-bis(3-methoxy-4-hydroxybenzylidene)hydrazine [vanillin azine (VA)] were carried out by using density functional (DFT/B3LYP) method with 6-31G(d) as basis set. The optimized geometrical parameters obtained by DFT calculations are in good agreement with single crystal XRD data. The vibrational spectral data obtained from solid phase FT-IR and FT-Raman spectra are assigned based on the results of the theoretical calculations. The observed spectra are found to be in good agreement with calculated values. The electric dipole moment ( μ) and the first hyperpolarizability ( β) values of the investigated molecule have been computed using ab initio quantum mechanical calculations. The calculation results also show that the VA molecule might have microscopic nonlinear optical (NLO) behavior with non-zero values. A detailed interpretation of the infrared and Raman spectra of VA was also reported. The energy and oscillator strength calculated by time-dependent density functional theory (TD-DFT) results complements with the experimental findings. The calculated HOMO and LUMO energies show that charge transfer occurs within the molecule. The theoretical NMR chemical shifts complement with experimentally measured ones.

  12. Synthesis, X-ray crystallography, spectroscopic (FT-IR, 1H &13C NMR and UV), computational (DFT/B3LYP) and enzymes inhibitory studies of 7-hydroximinocholest-5-en-3-ol acetate

    Science.gov (United States)

    Ahmad, Faheem; Parveen, Mehtab; Alam, Mahboob; Azaz, Shaista; Malla, Ali Mohammed; Alam, Mohammad Jane; Lee, Dong-Ung; Ahmad, Shabbir

    2016-07-01

    The present study reports the synthesis of 7-Hydroximinocholest-5-en-3-ol acetate (syn. 3β-acetoxycholest-5-en-7-one oxime; in general, steroidal oxime). The identity of steroidal molecule was confirmed by NMR, FT-IR, MS, CHN microanalysis and X-ray crystallography. DFT calculations on the titled molecule have been performed. The molecular structure and spectra interpreted by Gaussian hybrid computational analysis theory (B3LYP) are found to be in good correlation with the experimental data obtained from the various spectrophotometric techniques. The vibrational bands appearing in the FTIR are assigned with great accuracy using harmonic frequencies along with intensities and animated modes. Molecular properties like HOMO-LUMO analysis, chemical reactivity descriptors, MEP mapping, dipole moment and natural atomic charges have been presented at the same level of theory. Moreover, the Hirshfeld analysis was carried out to ascertain the secondary interactions and associated 2D fingerprint plots. The percentages of various interactions are pictorialized by fingerprint plots of Hirshfeld surface. Steroidal oxime exhibited promising inhibitory activity against acetylcholinesterase (AChE) as compared to the reference drug, tacrine. Molecular docking was performed to introduce steroidal molecules into the X-ray crystal structures of acetylcholinesterase at the active site to find out the probable binding mode. The results of molecular docking admitted that steroidal oxime may exhibit enzyme inhibitor activity.

  13. Spectroscopic (FT-IR, FT-Raman and UV-Visible) investigations, NMR chemical shielding anisotropy (CSA) parameters of 2,6-Diamino-4-chloropyrimidine for dye sensitized solar cells using density functional theory.

    Science.gov (United States)

    Gladis Anitha, E; Joseph Vedhagiri, S; Parimala, K

    2015-02-05

    The molecular structure, geometry optimization, vibrational frequencies of organic dye sensitizer 2,6-Diamino-4-chloropyrimidine (DACP) were studied based on Hartree-Fock (HF) and density functional theory (DFT) using B3LYP methods with 6-311++G(d,p) basis set. Ultraviolet-Visible (UV-Vis) spectrum was investigated by time dependent DFT (TD-DFT). Features of the electronic absorption spectrum in the UV-Visible regions were assigned based on TD-DFT calculation. The absorption bands are assigned to transitions. The interfacial electron transfer between semiconductor TiO2 electrode and dye sensitizer DACP is due to an electron injection process from excited dye to the semiconductor's conduction band. The observed and the calculated frequencies are found to be in good agreement. The energies of the frontier molecular orbitals (FMOS) have also been determined. The chemical shielding anisotropic (CSA) parameters are calculated from the NMR analysis, Stability of the molecule arising from hyperconjugative interactions and charge delocalization has been analyzed using natural bond orbital (NBO) analysis. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Spectroscopic (FT-IR, FT-Raman, UV, 1H and 13C NMR) profiling and theoretical calculations of (2E)-2-[3-(1H-imidazol-1-yl)-1-phenylpropylidene]hydrazinecarboxamide: An anticonvulsant agent

    Science.gov (United States)

    Haress, Nadia G.; Govindarajan, Munusamy; AL-Wabli, Reem I.; Almutairi, Maha S.; Al-Alshaikh, Monirah A.; Al-Saadi, Abdulaziz A.; Attia, Mohamed I.

    2016-08-01

    Vibrational characteristics of the anticonvulsant agent, (2E)-2-[3-(1H-imidazol-1-yl)-1-phenylpropylidene]hydrazinecarboxamide ((2E)-IPHC) have been investigated. The computational data are obtained by adopting ab initio Hartree-Fock (HF) and DFT/B3LYP/6-31 + G(d,p) methods. The most stable conformer is identified by a potential energy scan. The optimized geometrical parameters indicated that the overall symmetry of the most stable conformer is CS. Atoms in molecules (AIM) analysis is contained out and the chemical bondings between the atoms are as characterized. Mulliken atomic charges and simulated thermo-molecular (heat capacity and enthalpy) characteristics of the (2E)-IPHC molecule also have been analyzed. The magnitude of the molecular electrostatic potential (MEP) of oxygen, hydrogen, and nitrogen atoms as well as phenyl and imidazole rings in the title molecule were investigated along with their contribution to the biological activity. The energy gap between HOMO and LUMO orbitals has been found to be 5.1334 eV in the gaseous phase. Excitation energies, oscillator strength and wavelengths were computed by the time-dependent density function theory (TD-DFT) approach. Predicted wavenumbers have been assigned and they are consistent with the experimental values. The 1H and 13C nuclear magnetic resonance (NMR) chemical shifts of the (2E)-IPHC molecule were computed by the gauge independent atomic orbital (GIAO) method and were compared with the experimental results.

  15. Spectroscopic (FT-IR, FT-Raman, UV, 1H and 13C NMR) profiling and computational studies on methyl 5-methoxy-1H-indole-2-carboxylate: A potential precursor to biologically active molecules

    Science.gov (United States)

    Almutairi, Maha S.; Xavier, S.; Sathish, M.; Ghabbour, Hazem A.; Sebastian, S.; Periandy, S.; Al-Wabli, Reem I.; Attia, Mohamed I.

    2017-04-01

    Methyl 5-methoxy-1H-indole-2-carboxylate (MMIC) was prepared via esterification of commercially available 5-methoxyindole-2-carboxylic acid. The title molecule MMIC was characterised using FT-IR and FT-Raman in the ranges of 4000-500 and 4000-50 cm-1, respectively. The fundamental modes of the vibrations were assigned and the UV-visible spectrum of the MMIC molecule was recorded in the range of 200-400 nm to explore its electronic nature. The HOMO-LUMO energy distribution was calculated and the bonding and anti-bonding structures of the title molecule were studied and analysed using the natural bond orbital (NBO) approach. The reactivity of the MMIC molecule was also investigated and both the positive and negative centres of the molecule were identified using chemical descriptors and molecular electrostatic potential (MEP) analysis. The chemical shifts of the 1H and 13C NMR spectra were noted and the magnetic field environment of the MMIC molecule are discussed. The non-linear optical (NLO) properties of the title molecule were studied based on its calculated values of polarisability and hyperpolarisability. All computations were obtained by DFT methods using the 6-311++G (d,p) basis set.

  16. Synthesis, spectroscopic (UV-Vis, FT-IR and NMR), single crystal XRD of 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate: A comprehensive experimental and computational study

    Science.gov (United States)

    Arockia doss, M.; Rajarajan, G.; Thanikachalam, V.; Selvanayagam, S.; Sridhar, B.

    2017-01-01

    A piperidin-4-one containing picrate 3,5-diethyl -2,6-di(thiophen-2-yl)piperidin-4-on-1-ium picrate [3,5-DPPP] was synthesized. The molecular structure of 3,5-DPPP was confirmed by FT-IR, NMR, Uv-Vis, single crystal XRD analysis and DFT and HF methods with 6-31G(d,p) basis set. The XRD data confirm the transfer of protons from picric acid (O2) to piperidin-4-one ring (N1). The 3,5-DPPP compound is stabilized by the presence of intermolecular and intramolecular hydrogen bonds (N-H⋯O, C-H⋯S and C-H⋯O). Density functional theory and HF calculations have been used widely for calculating a wide variety of molecular properties such as optimized structure, FT-IR and Uv-Vis spectra, and provided reliable results which are in agreement with experimental data. The charge density data have been used to understand the properties of molecular systems. Furthermore, several quantum chemical insights have been obtained in the form of the total and partial density of states, the HOMO-LUMO energy gap and electrostatic potential map etc. In addition, the polarizability and first hyperpolarizability were calculated to show the potential applications of 3,5-DPPP in nonlinear optics.

  17. Comprehensive quantum chemical and spectroscopic (FTIR, FT-Raman, 1H, 13C NMR) investigations of (1,2-epoxyethyl)benzene and (1,2-epoxy-2-phenyl)propane

    Science.gov (United States)

    Arjunan, V.; Anitha, R.; Devi, L.; Mohan, S.; Yang, Haifeng

    2015-01-01

    Aromatic epoxides are causative factors for mutagenic and carcinogenic activity of polycyclic arenes. The 1,2- or 2,3-epoxy compounds are widely used to a considerable extent in the textile, plastics, pharmaceutical, cosmetics, detergent and photochemical industries. The FTIR and FT-Raman spectra of (1,2-epoxyethyl)benzene and (1,2-epoxy-2-phenyl)propane are recorded in the regions 4000-400 cm-1 and 4000-100 cm-1, respectively. The observed fundamentals are assigned to different normal modes of vibration. The structure of the compound has been optimised with B3LYP method using 6-311++G** and cc-pVTZ basis sets. The IR and Raman intensities are determined. The total electron density and molecular electrostatic potential surfaces of the molecule are constructed by using B3LYP/6-311++G(d,p) method to display electrostatic potential (electron + nuclei) distribution. The electronic properties HOMO and LUMO energies were measured. Natural bond orbital analysis of the compounds has been performed to indicate the presence of intramolecular charge transfer. The 1H and 13C NMR chemical shifts of the molecules have been analysed.

  18. Studies of DNA-binding properties of lafutidine as adjuvant anticancer agent to calf thymus DNA using multi-spectroscopic approaches, NMR relaxation data, molecular docking and dynamical simulation.

    Science.gov (United States)

    Yang, Hongqin; Tang, Peixiao; Tang, Bin; Huang, Yanmei; He, Jiawei; Li, Shanshan; Li, Hui

    2017-06-01

    The interactions between lafutidine (LAF) and calf thymus DNA (ctDNA) have been investigated both experimentally and theoretically. UV-vis absorption studies confirmed that LAF binds to ctDNA through non-covalent interactions. Fluorescence quenching and time-resolved fluorescence spectroscopy studies showed that the binding of LAF with ctDNA occurred through static quenching mechanism, resulting in the formation of a LAF-ctDNA complex. The binding constants (K) of the complex were found to be around 10(3)M(-1) via NMR relaxation rates and fluorescence data, and the calculated thermodynamic parameters indicated that hydrogen bonds and van der Waals forces played major roles in the binding of LAF to ctDNA. The changes in CD spectra indicated that LAF induced a slight perturbation on the base stacking and helicity of B-DNA. A comparative study of the LAF-ctDNA complex with respect to potassium iodide quenching experiments and competition displacement assays with ethidium bromide, acridine orange, and Hoechst 33258 probes suggested that LAF interacted with ctDNA by minor groove mode. Molecular docking analysis further supported the minor groove binding. Molecular dynamics simulation indicated that LAF depart from the C-G region of DNA, but it can steadily bind with the middle part of DNA composed by A-T base pairs. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Search for the p{sub 1/2{sup -}} resonance in {sup 7}He with the {sup 7}Li(d,{sup 2}He) reaction and measurement of the deuteron electrodisintegration under 180 at the S-DALINAC

    Energy Technology Data Exchange (ETDEWEB)

    Ryezayeva, N.

    2006-07-15

    The present work contains two parts, both devoted to the investigation of light nuclei. In the first part of the thesis the structure of the exotic {sup 7}He nucleus is studied. The disappearance of the usual magic numbers in extremely neutron-rich nuclei implies a considerable modification in the spin-orbit interaction. Recent experiments yield contradictory results about a possible existence of the p{sub 1/2{sup -}} spin-orbit partner of the {sup 7}He ground state with a dominant p{sub 3/2{sup -}} single-particle character. In order to clarify this question a study of the {sup 7}Li(d,{sup 2}He){sup 7}He reaction has been performed using a 171 MeV deuteron beam provided by the cyclotron at Kernfysisch Versneller Insituut (KVI) in Groningen. The experiment was carried out in April 2003. The setup at KVI offers a resolution {delta}E {approx} 150 keV (FWHM) in the measured spectra, better than the line width of the ground state of {sup 7}He. The unbound {sup 2}He system was identified by detecting coincidences between two protons with small relative energy. The data were taken over the angular range {theta}{sub cm}=0 -11.3 . A possible resonance at an excitation energy E{sub x}=(1.45{sub -0.5}{sup +0.7}) MeV with a width {gamma}=(2.0{sub -1.1}{sup +1.0}) MeV is suggested by a decomposition of the spectrum using known resonances, the breakup behaviour of {sup 7}He and quasifree charge-exchange contributions, taking into account the cluster structure of {sup 7}Li. Gamow-Teller strengths for transitions to the lowest states in {sup 7}He are in remarkable agreement with results from ab initio Quantum Monte Carlo calculations. The neutron spectroscopic factor S{sub n}=0.64{+-}0.09 of the {sup 7}He ground state ({sup 7}He={sup 6}He x n) is extracted by an R-matrix analysis. In the second part of the thesis the deuteron breakup has been studied in the {sup 2}H(e,e{sup '}) reaction at {theta}=180 . The present measurements were performed in March and April 2006 at the

  20. Experimental spectroscopic (FTIR, FT-Raman, FT-NMR, UV-Visible) and DFT studies of 1-ethyl-1,4-dihydro-7-methyl-4oxo-1,8 napthyridine-3-carboxylic acids.

    Science.gov (United States)

    Muthu, S; Elamurugu Porchelvi, E

    2013-12-01

    The solid phase FTIR and FT-Raman spectra of 1-ethyl-1,4-dihydro-7-methyl-4oxo-1,8 napthyridine-3-carboxylic acid (EDMONCA) have been recorded in the regions 4000-500 and 4000-400 cm(-1) respectively. The equilibrium geometry, harmonic vibrational frequencies have been investigated by DFT/B3LYP and B3PW91 methods with 6-311G (d,p) basis set. The different between the observed and scaled wave number values of most of the fundamental is very small. The assignments of the vibrational spectra have been carried out with the aid of normal coordinate analysis (NCA) following the scaled quantum mechanical force field methodology (SQMFFM). Stability of the molecule arising from hyper conjugative interactions, charge delocalization has been analyzed using natural bond orbital (NBO) analysis. UV-Visible spectrum of the compound was recorded and the electronic properties HOMO and LOMO energies were measured. The electric dipole moment (μD) and first hyperpolarizability (βtot) values of the investigated molecule were computed using ab initio quantum mechanical calculations. The calculated results also show that the EDMONCA molecule may have microscopic nonlinear optics (NLO) behavior with non-zero values. (1)H and (13)C NMR spectra were recorded and (1)H and (13)C nuclear magnetic resonance chemical shift of the molecule were calculated using the gauge independent atomic orbital (GIAO) method. Thermal stability of EDMONCA was studied by thermogravimetric analysis (TGA). Next Fukui function was calculated to explain the chemical selectivity or reactivity site in EDMONCA. Finally molecular electrostatic potential (MEP) and other molecular properties were performed. Copyright © 2013 Elsevier B.V. All rights reserved.

  1. Synthesis and NMR Spectral Studies of the 7-C60-Adduct of N,N-(Tetrachlorophthaloyl Dehydroabietylamine

    Directory of Open Access Journals (Sweden)

    Zhi Zhou

    2012-04-01

    Full Text Available The 7-C60-adduct of N,N-(tetrachlorophthaloyldehydroabietylamine was synthesized for the first time and characterized by IR, UV-vis, mass and NMR spectral studies. The 1H-NMR and 13C-NMR resonance signals of the new compound are unambiguously assigned by using homo- and heteronuclear 2D NMR spectroscopic techniques such as COSY, ROESY, HSQC and HMBC. The C1 symmetric structure with 6,6-junction of compound was determined.

  2. 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.

    Science.gov (United States)

    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

  3. 1H-NMR spectroscopic characteristics of serum from patients with esophageal squamous cell carcinoma%食管鳞癌患者血清核磁共振氢谱特征研究

    Institute of Scientific and Technical Information of China (English)

    姜玉章; 孙晓阳; 史昆波; 尹起范

    2011-01-01

    1H-nuclear magnetic resonance spectroscopy ( 1H-NMRs ) analysis was performed on serum specimens obtained from 60 preoperative patients with esophageal squamous cell carcinoma ( ESCC )and 30 healthy controls, and supernatant from 2 ESCC cell lines Eca-109 and TE-13.The characteristic fingerprint was profiled with 1H-NMRs data in healthy controls.Serum 1H-NMRs from 60 preoperative patients with ESCC were measured and compared with the 1H-NMRs from 30 healthy controls.We found some specific peaks in 1H-NMRs profile of serum specimens from ESCC patients, especially at 1.0-1.2 mg/L and 3.4 - 3.6 mg/L.The results were verified by the 1H-NMRs measurement on the supernatant from 2 ESCC cell lines Eca-109 and TE-3.Our results suggest that this two absorption peaks may be characteristic for ESCC and 1H-NMRs analysis on serum specimens may provide information for early diagnosis of ESCC.%运用核磁共振波谱仪测试30名正常人和60例术前食管鳞癌患者血清、2株食管鳞癌细胞株(Eca-109和TE-13)的细胞培养上清液的核磁共振氢谱(1H-NMR).利用1H-NMR分析软件构建了正常人血清1H-NMR图谱.将食管鳞癌患者与正常人的血清1H-NMR峰叠加处理进行比较发现,二者血清样品的波谱多处存在差异,尤其在1.0~1.2 mg/L和3.4~3.6 mg/L明显,推测可能为食管鳞癌血清的特征峰.2株食管鳞癌细胞株细胞培养上清液的1H-NMR也证实上述结果.提示借助特征峰检测,有助于食管鳞癌的早期诊断.

  4. The acquisition of multidimensional NMR spectra within a single scan

    Science.gov (United States)

    Frydman, Lucio; Scherf, Tali; Lupulescu, Adonis

    2002-01-01

    A scheme enabling the complete sampling of multidimensional NMR domains within a single continuous acquisition is introduced and exemplified. Provided that an analyte's signal is sufficiently strong, the acquisition time of multidimensional NMR experiments can thus be shortened by orders of magnitude. This could enable the characterization of transient events such as proteins folding, 2D NMR experiments on samples being chromatographed, bring the duration of higher dimensional experiments (e.g., 4D NMR) into the lifetime of most proteins under physiological conditions, and facilitate the incorporation of spectroscopic 2D sequences into in vivo imaging investigations. The protocol is compatible with existing multidimensional pulse sequences and can be implemented by using conventional hardware; its performance is exemplified here with a variety of homonuclear 2D NMR acquisitions. PMID:12461169

  5. NMR of lignins

    Science.gov (United States)

    John Ralph; Larry L. Landucci

    2010-01-01

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

  6. Designing of high-resolution photoresists: use of modern NMR techniques for evaluating lithographic performance

    Indian Academy of Sciences (India)

    Debmalya Roy; P K Basu; P Raghunathan; S V Eswaran

    2004-06-01

    Applications of improved 1-D/ 2-D NMR spectroscopic techniques have been reviewed for quantitatively estimating the incorporation of different monomers and degree of linearity in resin microstructure. Comparison of the NMR data with those from lithography leads to a distinct correlation between resin microstructure and lithographic performance. A novel photoresist mechanism is proposed in a positive photoresist; also, using modern NMR techniques, the crosslinking mechanism in a negative photoresist has been studied.

  7. Ab initio calculations of accurate dissociation energy and analytic potential energy function for the second excited state B1П of 7LiH

    Institute of Scientific and Technical Information of China (English)

    Shi De-Heng; Liu Yu-Fang; Sun Jin-Feng; Zhu Zun-Lùe; Yang Xiang-Dong

    2006-01-01

    The reasonable dissociation limit of the second excited singlet state B1П of 7LiH molecule is obtained. The obtained over the internuclear distance ranging from about 0.10 nm to 0.54 nm, and has a least-square fit to the analytic compared with previous theoretical results. The equilibrium internuclear distance obtained by geometry optimization is found to be quite different from that obtained by single-point energy scanning under the same calculation condition.comparison of the theoretical calculations of dissociation energies, equilibrium interatomic distances and the analytic potential energy function with those obtained by previous theoretical results clearly shows that the present work is more theories.

  8. Measurements of neutron energy spectra from 7Li(p,n)7Be reaction with Bonner sphere spectrometer, Nested Neutron Spectrometer and ROSPEC.

    Science.gov (United States)

    Atanackovic, J; Matysiak, W; Witharana, S; Dubeau, J; Waker, A J

    2014-10-01

    Neutron spectrometry measurements were carried out at the McMaster Accelerator Laboratory (MAL), which is equipped with a 3-MV Van de Graaff-type accelerator. Protons were accelerated onto a thick natural lithium target inducing the (7)Li(p,n)(7)Be threshold reaction. Depending on the proton energy, slightly different poly-energetic neutron fields were produced. Neutron spectra were measured at two incident proton energies: 2.15 and 2.24 MeV, which produced poly-energetic neutrons with maximum kinetic energies of 401 and 511 keV, respectively. Measurements were performed at a distance of 1.5 m from the target in the forward direction with three different instruments: Bonner sphere spectrometer, Nested Neutron Spectrometer and ROtational proton recoil SPECtrometer.

  9. A Comprehensive Theoretical Analysis of 6,7Li + 64Zn Elastic Scattering in a Wide Angular Range Around the Coulomb Barrier

    Science.gov (United States)

    Ibraheem, Awad A.; Aygun, M.

    2016-08-01

    In this paper, the elastic scattering angular distributions of 6,7Li on 64Zn have been investigated by using various nuclear potentials. For this, we use the phenomenological Woods-Saxon potential, the real double folding potential with the density-independent M3Y effective interaction supplemented with an imaginary part in Woods-Saxon form and the double folding potentials multiplied with a normalization factor of the real and imaginary parts via the density-independent and CDM3Y6 density-dependent versions of the M3Y effective interaction have been used. The results have been compared with each other as well as with the experimental data. It has been observed that the agreement between the theoretical results and earlier reported data is perfect. Finally, the change of the total reaction cross sections with energy has been investigated.

  10. Elastic and inelastic scattering of {sup 6}Li + {sup 18}O versus {sup 7}Li + {sup 18}O and {sup 6}Li + {sup 16}O

    Energy Technology Data Exchange (ETDEWEB)

    Rudchik, Adam T., E-mail: rudchik@kinr.kiev.ua [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kliczewski, Stanislaw [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Chercas, Kostyantyn A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Kemper, Kirby W. [Physics Department, Florida State University, Tallahassee, FL 32306-4350 (United States); Koshchy, Evgeniy I. [Kharkiv National University, pl. Svobody 4, 61077 Kharkiv (Ukraine); Rusek, Krzysztof [National Centre for Nuclear Research, ul. Hoża 69, PL-00-681 Warsaw (Poland); Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Rudchik, Andryi A.; Mezhevych, Sergyi Yu.; Pirnak, Valeryi M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Plujko, Volodymyr A. [Taras Shevchenko Kyiv National University, vul. Volodymyrs' ka 64, 01033 Kyiv (Ukraine); Ponkratenko, Oleg A. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine); Choiński, Jaroslaw [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Czech, Bronislaw; Siudak, Regina; Szczurek, Antoni [H. Niewodniczański Institute of Nuclear Physics, Polish Academy of Sciences, ul. Radzikowskiego 152, PL-31-342 Cracow (Poland); Stolarz, Anna [Heavy Ion Laboratory of Warsaw University, ul. L. Pasteura 5A, PL-02-093 Warsaw (Poland); Zelinskyi, Ruslan M. [Institute for Nuclear Research, Ukrainian Academy of Sciences, Prospect Nauki 47, 03680 Kyiv (Ukraine)

    2014-02-15

    Inverse kinematics scattering of {sup 18}O on {sup 6}Li at E{sub lab}({sup 18}O) = 114 MeV was measured to obtain elastic and inelastic scattering cross sections. In this way cross sections for excited states in {sup 6}Li and {sup 18}O were determined. The data were analyzed within the optical model and coupled reaction channel method. The {sup 6}Li + {sup 18}O optical potential as well as the {sup 6}Li and {sup 18}O deformation parameters were deduced. Contributions of different nuclear processes to the {sup 6}Li + {sup 18}O elastic and inelastic scattering were explored. The isotopic differences between the {sup 6,7}Li + {sup 18}O and {sup 6}Li + {sup 16,18}O potential parameters were determined.

  11. Experimental and Calculated Effectiveness of a Radiochromic Dye Film to Stopping 21 MeV 7Li- and 64 MeV 16O Ions

    DEFF Research Database (Denmark)

    Olsen, Kjeld J; Hansen, Johnny

    1984-01-01

    particles developed by Katz et al. The experiment was designed to test calculations particularly in the Bragg-peak region of the slowing down particles where significant deviation between theory and experiment was found. Fitting of the characteristic D37 dose and the size of the radiation sensitive element......Relative radiation effectiveness, RE, of 21 MeV 7Li and 64 MeV 16O ions being completely stopped in a tissue equivalent film dose meter has been measured as a function of penetration depth and energy, and the results have been compared with calculations based on a δ-ray theory for heavy charged...... in the detector, which are important parameters in the theoretical model, does not improve the overall correlation between theory and experiment. It is concluded that disagreement between theoretical and experimental RE-values below 1.5 MeV/amu is partly due to lack of equivalence between the δ-ray spectrum...

  12. Cell killing, nuclear damage and apoptosis in Chinese hamster V79 cells after irradiation with heavy-ion beams of (16)O, (12)C and (7)Li.

    Science.gov (United States)

    Pathak, Rupak; Dey, Subrata Kumar; Sarma, Asiti; Khuda-Bukhsh, Anisur Rahman

    2007-08-15

    Chinese hamster V79 cells were exposed to high LET (linear energy transfer) (16)O-beam (625keV/mum) radiation in the dose range of 0-9.83Gy. Cell survival, micronuclei (MN), chromosomal aberrations (CA) and induction of apoptosis were studied as a follow up of our earlier study on high LET radiations ((7)Li-beam of 60keV/mum and (12)C-beam of 295keV/mum) as well as (60)Co gamma-rays. Dose dependent decline in surviving fraction was noticed along with the increase of MN frequency, CA frequency as well as percentage of apoptosis as detected by nuclear fragmentation assay. The relative intensity of DNA ladder, which is a useful marker for the determination of the extent of apoptosis induction, was also increased in a dose dependent manner. Additionally, expression of tyrosine kinase lck-1 gene, which plays an important role in response to ionizing radiation induced apoptosis, was increased with the increase of radiation doses and also with incubation time. The present study showed that all the high LET radiations were generally more effective in cell killing and inflicting other cytogenetic damages than that of low LET gamma-rays. The dose response curves revealed that (7)Li-beam was most effective in cell killing as well as inducing other nuclear damages followed by (12)C, (16)O and (60)Co gamma-rays, in that order. The result of this study may have some application in biological dosimetry for assessment of genotoxicity in heavy ion exposed subjects and in determining suitable doses for radiotherapy in cancer patients where various species of heavy ions are now being generally used.

  13. Fuskite® preliminary experimental tests based on permeation against vacuum for hydrogen recovery as a potential application in Pb15.7Li loop systems.

    Energy Technology Data Exchange (ETDEWEB)

    Sacristán, R., E-mail: mrosa.sacristan@sener.es [SENER Ingeniería y Sistemas, C/ Provença 392, 5a, 08025 Barcelona (Spain); Veredas, G. [EURATOM-CIEMAT Fusion Assoc., Fusion Technology Division, Av. Complutense 40, 28040 Madrid (Spain); Bonjoch, I. [SENER Ingeniería y Sistemas, C/ Provença 392, 5a, 08025 Barcelona (Spain); Peñalva, I. [UPV/EHU, Departamento de Ingeniería Nuclear y Mecánica de Fluidos, Alameda de Urquijo s/n, 48013 Bilbao (Spain); Calderón, E. [SENER Ingeniería y Sistemas, C/ Provença 392, 5a, 08025 Barcelona (Spain); Alberro, G. [UPV/EHU, Departamento de Ingeniería Nuclear y Mecánica de Fluidos, Alameda de Urquijo s/n, 48013 Bilbao (Spain); Balart, D. [SENER Ingeniería y Sistemas, Avda. Zugazarte 56, 48930 Las Arenas, Vizcaya (Spain); Sarrionandia-Ibarra, A. [UPV/EHU, Departamento de Ingeniería Nuclear y Mecánica de Fluidos, Alameda de Urquijo s/n, 48013 Bilbao (Spain); Pérez, V. [SENER Ingeniería y Sistemas, Avda. Zugazarte 56, 48930 Las Arenas, Vizcaya (Spain); Ibarra, A. [EURATOM-CIEMAT Fusion Assoc., Fusion Technology Division, Av. Complutense 40, 28040 Madrid (Spain); Legarda, F. [UPV/EHU, Departamento de Ingeniería Nuclear y Mecánica de Fluidos, Alameda de Urquijo s/n, 48013 Bilbao (Spain)

    2014-10-15

    Highlights: • Full material characterization as far as hydrogen transport properties are concern. • Quantification of permeator leaks and material degasification. • Analysis of H{sub 2} recovered by means of permeation against vacuum in different conditions. • Hydrogen recovery efficiencies determination. - Abstract: Tritium recovery in fusion reactors is one of the main goals in R and D, as a limited inventory is available and its uneconomic production. That is the reason why efficient technologies are indispensable to be developed in order to achieve fast tritium recovery and its subsequent reuse in the system for increasing its self-sufficiency. In this work a flexible tritium recovery demonstrator prototype based on permeation against vacuum concept has been designed and manufactured, as well as all necessary equipment for a Pb15.7Li loop implementation in order to test and demonstrate that an in-pipe integrated solution is possible, and at the same time, to validate the manufacturing process. Thus, efficient rates for more optimized future models could be then extrapolated. The aim of this paper is to show the different testing results that have been carried out in this research project. These results include permeation properties of the material considered for the permeator, as long as it has been manufactured with a novel technique, Selective Laser Melting. They also include vacuum tests on the permeator to quantify possible leakages and to set up and analyze the capability to generate vacuum inside the permeator, and finally, permeation tests with the prototype, in a first stage with a gas mixture of hydrogen and argon inside the loop instead of Pb15.7Li.

  14. Astrophysical S-factor of T(4He, γ)7Li reaction at E cm = 15.7 keV

    Science.gov (United States)

    Bystritsky, V. M.; Dudkin, G. N.; Emets, E. G.; Filipowicz, M.; Krylov, A. R.; Nechaev, B. A.; Nurkin, A.; Padalko, V. N.; Philippov, A. V.; Sadovsky, A. B.

    2017-07-01

    The astrophysical S-factor of the reaction T(4He, γ)7Li is measured for the first time at the center of mass energy E cm = 15.7 keV, lower than the energy range of the Standard Big Bang Nucleosynthesis (SBBN) model. The experiment is performed on a Hall pulsed accelerator (TPU, Tomsk). An acceleration pulse length of 10 μs allows one to suppress the background of cosmic radiation and the ambient medium by five orders of magnitude. A beam intensity of 5 × 1014 4He+ ions per pulse allows one to measure an extremely low reaction yield. The yield of γ-quanta with the energies E γ 0 = 2483.7 keV and E γ 1 = 2006.1 keV is registered by NaI(Tl) detectors with the efficiency ɛ = 0.331 ± 0.026. A method for direct measurement of the background from the chain of reactions T(4He, 4He)T→T(T, 2 n)X→( n, γ) and/or ( n, n'γ) which ends by neutron activation of materials surrounding the target is proposed and implemented in this study. The value of the astrophysical S-factor of the reaction T(4He, γ)7Li S αt ( E cm = 15.7 keV) = 0.091 ± 0.032 keV b provides the choice from the set of experimental data for the astrophysical S αt -factor in favor of experimental data [4] with S αt ( E cm = 0) = 0.1067 ± 0.0064 keV b.

  15. Solid State NMR Studies of Energy Conversion and Storage Materials

    Science.gov (United States)

    Jankuru Hennadige, Sohan Roshel De Silva

    NMR (Nuclear magnetic resonance) spectroscopy is utilized to study energy conversion and storage materials. Different types of NMR techniques including Magic Angle Spinning, Cross-polarization and relaxation measurement experiments were employed. Four different projects are discussed in this dissertation. First, three types of CFx battery materials were investigated. Electrochemical studies have demonstrated different electrochemical performances by one type, delivering superior performance over the other two. 13C and 19F MAS NMR techniques are employed to identify the atomic/molecular structural factors that might account for differences in electrochemical performance among different types. Next as the second project, layered polymer dielectrics were investigated by NMR. Previous studies have shown that thin film capacitors are improved by using alternate layers of two polymers with complementary properties: one with a high breakdown strength and one with high dielectric constant as opposed to monolithic layers. 13C to 1H cross-polarization techniques were used to investigate any inter-layer properties that may cause the increase in the dielectric strength. The third project was to study two types of thermoelectric materials. These samples were made of heavily doped phosphorous and boron in silicon by two different methods: ball-milled and annealed. These samples were investigated by NMR to determine the degree of disorder and obtain insight into the doping efficiency. The last ongoing project is on a lithium-ion battery system. The nature of passivating layers or the solid electrolyte interphase (SEI) formed on the electrodes surface is important because of the direct correlation between the SEI and the battery life time/durability. Multinuclear (7Li, 19F, 31P) techniques are employed to identify the composition of the SEI formation of both positive and negative electrodes.

  16. Solid-state NMR studies of Al-doped and Al{sub 2}O{sub 3}-coated LiCoO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Youngil; Kim, Dongmin; Lee, Hyeyeoun [Dongbu Advanced Research Inst., Daejeon (Korea). Chemical Analysis Team; Woo, Ae Ja [Ewha Womans Univ., Seoul (Korea); Han, Kyoo Seung [Chungnam National Univ., Daejeon (Korea). Dept. of Fine Chemicals Engineering and Chemistry; Ryu, D. [Electronics and Telecommunications Research Inst., Daejeon (Korea); Sohn, Daewon [Hanyang Univ., Seoul (Korea). Dept. of Chemistry

    2004-11-30

    As a cathode material for commercial lithium rechargeable battery, Al-doped and Al{sub 2}O{sub 3}-coated LiCoO{sub 2} were structurally characterized and compared by using solid-state {sup 7}Li and {sup 27}Al magic angle spinning (MAS) NMR. The structural states of lithium and aluminum in those samples were successfully identified by calculation of NMR spectra. {sup 7}Li MAS NMR spectra of samples had shown similar features having more than three lithium sites, which were determined as quadrupole coupling constant with the same asymmetric parameter ({eta} = 0.1); C{sub Q} = 1.10 MHz for octahedral site, and C{sub Q} 2.97 MHz and C{sub Q} = 3.83 MHz for shoulders. {sup 27}Al MAS NMR spectra of samples, however, showed significant difference in two observed aluminum sites. In the simulation of NMR spectrum for Al{sub 2}O{sub 3}-coated LiCoO{sub 2}, the values of C{sub Q} and {eta} were obtained; 4.45 MHz and {eta} = 0.86 for tetrahedral site and 4.31 MHz and {eta} = 0.81 for octahedral.

  17. Bare astrophysical S(E)-factor for the {sup 6}Li(d, {alpha}){sup 4}He and {sup 7}Li(p, {alpha}){sup 4}He reactions at astrophysical energies

    Energy Technology Data Exchange (ETDEWEB)

    Pizzone, R.G.; Spitaleri, C.; Lattuada, M.; Musumarra, A.; Pellegriti, M.G.; Romano, S.; Tumino, A.; Cherubini, S.; Figuera, P.; Miljanic, D.; Rolfs, C.; Typel, S.; Wolter, H.H.; Castellani, V.; Degl' Innocenti, S.; Imperio, A

    2003-05-05

    The Trojan Horse Method has been applied to study the {sup 7}Li(p, {alpha}){sup 4}He and {sup 6}(Li(d, {alpha}){sup 4}He reactions through the {sup 7}Li(d, {alpha}{alpha})n and {sup 6}Li({sup 6}Li, {alpha}{alpha}){sup 4}He three body processes, respectively. The electron screening potential deduced from these experiments is much larger than the adiabatic approximation prediction for both cases; the systematic discrepancy between data and theoretical predictions is thus confirmed. Astrophysical implications of these measurements are also discussed.

  18. Treatment of the Mirror 3H(α, γ) 7Li and 3He(α, γ) 7Be Reactions in the Algebraic Version of the Resonating Group Model

    Science.gov (United States)

    Solovyev, A. S.; Igashov, S. Yu; Tchuvil'sky, Yu M.

    2014-12-01

    A unified microscopic approach based on the algebraic version of the resonating group model has been realized for description of the radiative capture reactions 3H(α, γ)7Li and 3He(α, γ)7Be, which play an important role for modern nuclear astrophysics. The astrophysical S-factors of the reactions and branching ratios between capture to the ground and first excited states of the 7Li and 7Be nuclei have been calculated. The comparison with the most recent experimental data demonstrates a good agreement.

  19. Authenticity study of Phyllanthus species by NMR and FT-IR techniques coupled with chemometric methods

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Maiara S.; Pereira-Filho, Edenir R.; Ferreira, Antonio G. [Universidade Federal de Sao Carlos (UFSCAR), SP (Brazil). Dept. de Quimica; Boffo, Elisangela F. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; Figueira, Glyn M., E-mail: maiarassantos@yahoo.com.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil). Centro Pluridisciplinar de Pesquisas Quimicas, Biologicas e Agricolas

    2012-07-01

    The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as 'quebra-pedras' in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, {sup 1}H HR-MAS NMR and {sup 1}H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques. (author)

  20. Authenticity study of Phyllanthus species by NMR and FT-IR Techniques coupled with chemometric methods

    Directory of Open Access Journals (Sweden)

    Maiara S. Santos

    2012-01-01

    Full Text Available The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as "quebra-pedras" in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, ¹H HR-MAS NMR and ¹H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques.

  1. Computing the Vibrational and Vibrational-rotational Energy Eigenvalues of 7Li2 by the Symplectic Scheme-matrix Algorithm%计算7Li2振动能级煌振动-转动能级的辛格式矩阵法

    Institute of Scientific and Technical Information of China (English)

    何建锋; 刘学深; 丁培柱

    2004-01-01

    利用辛格式矩阵法计算了双原子分子7Li2在A1∑+u态的振动能级和振动-转动能级,并与Ley-Koo等的计算结果作了比较.结果显示,辛格式矩阵法是收敛的和可靠的,是计算双原子分子的振动能级和振动-转动能级的合理的数值方法.

  2. (F(8)TPP)Fe(II)/O(2) reactivity studies [F(8)TPP = tetrakis(2,6-difluorophenyl)porphyrinate(2-)]: spectroscopic (UV-Visible and NMR) and kinetic study of solvent-dependent (Fe/O(2) = 1:1 or 2:1) reversible O(2)-reduction and ferryl formation.

    Science.gov (United States)

    Ghiladi, R A; Kretzer, R M; Guzei, I; Rheingold, A L; Neuhold, Y M; Hatwell, K R; Zuberbühler, A D; Karlin, K D

    2001-11-05

    )Fe(II) (1)/O(2) reaction was also examined at reduced temperatures in noncoordinating solvents (toluene, CH(2)Cl(2)), where UV-visible and (2)H and (19)F NMR spectroscopies also revealed the presence of a reversibly formed adduct, formulated as the peroxo-bridged dinuclear complex [(F(8)TPP)Fe(III)](2)-(O(2)(2)(-)) (3) [CH(2)Cl(2): UV-visible, 414 (Soret), 535 nm; (2)H NMR, delta(pyrrole) 17.5 ppm]. Dioxygen-uptake spectrophotometric titrations revealed a stoichiometry of 2 (F(8)TPP)Fe(II) (1) per O(2) upon full formation of 3. Addition of a nitrogenous base, 4-(dimethylamino)pyridine, to a cold solution of 3 in dichloromethane gave rapid formation of the iron(IV)-oxo ferryl species (DMAP)(F(8)TPP)Fe(IV)==O (4), based upon UV-visible [417 (Soret), 541 nm] and (2)H NMR (delta(pyrrole) = 3.5 ppm) spectroscopic characterization. These detailed investigations into the O(2)-adducts and "ferryl" species formed from (F(8)TPP)Fe(II) (1) may be potentially important for a full understanding of our ongoing heme-copper oxidase model studies, which employ 1 or similar "tethered" (i.e., covalently attached Cu-chelate) porphyrin analogues in heme/Cu heterobinuclear systems.

  3. NMR at 900 MHz

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    @@ An important factor in the development of solutionstate NMR has always been th e ability to produce stable and homogeneous magnetic fields. As higher and higher field strengths are reached the pressure is growing on manufacturers to produce NMR systems with greatly improved spectral resolution and signal to noise ratio. The introduction of the Varian 900 MHz INOVA system in August 2000 featuring Oxford Instruments 21.1 T magnet represents the latest pioneering development in NMR technology.

  4. Optimization of a neutron production target and a beam shaping assembly based on the 7Li( p, n) 7Be reaction for BNCT

    Science.gov (United States)

    Burlon, A. A.; Kreiner, A. J.; Valda, A. A.; Minsky, D. M.; Somacal, H. R.; Debray, M. E.; Stoliar, P.

    2005-02-01

    In this work a thick LiF target was studied through the 7Li( p, n) 7Be reaction as a neutron source for Accelerator-Based Boron Neutron Capture Therapy (AB-BNCT) to provide a testing ground for numerical simulations aimed at producing an optimized neutron production target and beam shaping assembly design. Proton beams in the 1.88-2.0 MeV energy range were produced with the tandem accelerator TANDAR ( TANDem ARgentino) at the Comisión Nacional de Energía Atómica (CNEA) in Buenos Aires, Argentina. A cylindrical water-filled head-phantom, containing a boric acid sample, was irradiated to study the resulting neutron flux. The dose deposited in the boric acid sample was inferred through the Compton-suppressed detection of the gamma radiation produced from the 10B( n, αγ) 7Li capture reaction. The thermal neutron flux was evaluated using bare and Cd-covered activation gold foils. In all cases, Monte Carlo simulations have been done showing good agreement with the experimental results. Extensive MCNP simulation trials have then been performed after the preliminary calculation tool validation in order to optimize a neutron beam shaping assembly. These simulations include a thick Li metal target (instead of LiF), a whole-body phantom, two different moderator-reflector assemblies (Al/AlF 3/LiF, Fluental ®, as moderator and lead as reflector and a combination of Al, PTFE (polytetrafluoroethylene) and LiF as moderator and lead as reflector) and the treatment room. The doses were evaluated for proton bombarding energies of 1.92 MeV (near to the threshold of the reaction), 2.0 MeV, 2.3 MeV (near the reaction resonance) and 2.5 MeV, and for three Fluental ® and Al/PTFE/LiF moderator thicknesses (18, 26 and 34 cm). In a later instance, the effect of the specific skin radiosensitivity (an RBE of 2.5 for the 10B( n, α) 7Li reaction) and a 10B uptake 50% greater than the healthy tissue one, was considered for the scalp. To evaluate the doses in the phantom, a comparison of

  5. Evaluation of the characteristics of boron-dose enhancer (BDE) materials for BNCT using near threshold {sup 7}Li(p,n){sup 7}Be direct neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Bengua, Gerard [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennann-gun, Osaka 590-0494 (Japan); Kobayashi, Tooru [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennann-gun, Osaka 590-0494 (Japan); Tanaka, Kenichi [Research Institute for Radiation Biology and Medicine, Hiroshima University, Kasumi, Minami-ku, Hiroshima 734-8553 (Japan); Nakagawa, Yoshinobu [National Kagawa Children' s Hospital, Zentsuji-cho, Zentsuji, Kagawa 765-8501 (Japan)

    2004-03-07

    The characteristics of a number of candidate boron-dose enhancer (BDE) materials for boron neutron capture therapy (BNCT) using near threshold {sup 7}Li(p,n){sup 7}Be direct neutrons were evaluated based on the treatable protocol depth (TPD), defined in this paper. Simulation calculations were carried out by means of MCNP-4B transport code for candidate BDE materials, namely, (C{sub 2}H{sub 4}){sub n}, (C{sub 2}H{sub 3}F){sub n}, (C{sub 2}H{sub 2}F{sub 2}){sub n}, (C{sub 2}HF{sub 3}){sub n}, (C{sub 2}D{sub 4}){sub n}, (C{sub 2}F{sub 4}){sub n}, beryllium metal, graphite, D{sub 2}O and {sup 7}LiF. Dose protocols applied were those used for intra-operative BNCT treatment for brain tumour currently used in Japan. The maximum TPD (TPD{sub max}) for each BDE material was found to be between 4 cm and 5 cm in the order of (C{sub 2}H{sub 4}){sub n} < (C{sub 2}H{sub 3}F){sub n} < (C{sub 2}H{sub 2}F{sub 2}){sub n} < (C{sub 2}HF{sub 3}){sub n} < beryllium metal < (C{sub 2}D{sub 4}){sub n} < graphite < (C{sub 2}F{sub 4}){sub n} < D{sub 2}O < {sup 7}LiF. Based on the small and arbitrary variations in the TPD{sub max} for these materials, an explicit advantage of a candidate BDE material could not be established from the TPD{sub max} alone. The dependence of TPD on BDE thickness was found to be influenced by the type of BDE material. For materials with hydrogen, sharp variations in TPD were observed, while those without hydrogen exhibited more moderate fluctuations in TPD as the BDE thickness was varied. The BDE thickness corresponding to TPD{sub max} (BDE(TPD{sub max})) was also found to depend on the type of BDE material used. Thicker BDE(TPD{sub max}), obtained mostly for BDE materials without hydrogen, significantly reduced the dose rates within the phantom. The TPD{sub max}, the dependence of TPD on BDE thickness and the BDE (TPD{sub max}) were ascertained as appropriate optimization criteria in choosing suitable BDE materials for BNCT. Among the candidate BDE materials

  6. Assignments of 1H and 13C NMR Signals of Mogroside IVa

    Institute of Scientific and Technical Information of China (English)

    ZHANGJian-ye; YANGXiu-wei

    2003-01-01

    Aim To investigate the structure of mogroside IVa isolated from traditional Chinese medicine fructus momordicae [fruits of Siraitia grosvenori (Swingle) C. Jeffery] and summarize the NMR characteristics of the structure. Methods Cormnon extraction, separafion and purification methods were used. Various NMR techniques including 1H NMR,13C NMR, DEPT, 1H-1H COSY, HSQC, HMBC, NOESY and molecular model simulated by comtmter were used to elucidate the structure. Results 1H and 13C NMR signals of mogroside IVa were assigned, and spectroscopic basis was obtained for identification of such type of compounds. Conclusion 1D and 2D NMR techniques including 1H-1H COSY, HSQC, HMBC, NOESY spectra are powerful tools for structure analysis. The structure determined by NMR methods is identical with energy minimized conformation simulated by computer.

  7. NMR studies of nucleic acid dynamics

    Science.gov (United States)

    Al-Hashimi, Hashim M.

    2013-12-01

    Nucleic acid structures have to satisfy two diametrically opposite requirements; on one hand they have to adopt well-defined 3D structures that can be specifically recognized by proteins; on the other hand, their structures must be sufficiently flexible to undergo very large conformational changes that are required during key biochemical processes, including replication, transcription, and translation. How do nucleic acids introduce flexibility into their 3D structure without losing biological specificity? Here, I describe the development and application of NMR spectroscopic techniques in my laboratory for characterizing the dynamic properties of nucleic acids that tightly integrate a broad set of NMR measurements, including residual dipolar couplings, spin relaxation, and relaxation dispersion with sample engineering and computational approaches. This approach allowed us to obtain fundamental new insights into directional flexibility in nucleic acids that enable their structures to change in a very specific functional manner.

  8. Analysis of human urine metabolites using SPE and NMR spectroscopy

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Nuclear magnetic resonance (NMR) spectroscopic analysis of metabonome/metabolome has widespread applications in biomedical science researches. However, most of NMR resonances for urinary metabolites remain to be fully assigned. In the present study, human urine samples from two healthy volunteers were pre-treated with C18 solid-phase extraction and the resultant 5 sub-fractions were subjected to one- and two-dimensional NMR studies, including 1H J-Resolved, 1H-1H COSY, 1H-1H TOCSY, 1H-13C HSQC, and HMBC 2D NMR. More than 70 low molecular weight metabolites were identified, and complete assignments of 1H and 13C resonances including many complex coupled spin systems were obtained.

  9. 31P NMR Study on Some Phosphorus-Containing Compounds

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    31P NMR has become a widely applied spectroscopic probe of the structure of phosphorus-containing compounds. Meanwhile, the application of 31P NMR has been rapidly expanded to biochemistry and medicinal chemistry of phosphorus-containing compounds because the growing importance of the phosphorus compounds is now widely realized. We report here the results of 31P NMR study on some phosphorus-containing compounds, namely, O-alkyl O-4-nitrophenyl methyl phosphonates with different alkyl chain-length (MePO-n), 4-nitrophenyl alkylphenylphosphinates with different alkyl chain-length (PhP-n), diethyl phosphono- acetonitrile anion and diethyl phosphite anion . Our results indicate that 31P NMR can not only be applied to not only the study of the hydrolytic reactions of MePO-8 and PhP-8 but also be applied to the study of the presence of the anions of diethylphosphonoacetonitrile and diethyl phosphite in nucleophilic reactions.

  10. The role of electrostatic interactions and solvent polarity on the 15N NMR shielding of azines

    Science.gov (United States)

    Modesto-Costa, Lucas; Gester, Rodrigo M.; Manzoni, Vinícius

    2017-10-01

    The nitrogen-15 nuclear magnetic resonance (15N NMR) shielding of azines is very sensitive to the chemical environment. Theoretically, specific interactions are important on the calculation of their spectroscopic properties. However, the choice of the solvent model for the description of NMR shielding constants is still a subject of discussion. In this context, we analyse the role of electrostatic interactions on 15N NMR shielding as function of solvent polarity using the sequential-Quantum Mechanics/Molecular Mechanics approach methodology. Excellent agreement with experimental data of the NMR shielding was obtained without the inclusion of explicit solvent molecules either for polar or non polar solvents.

  11. Quasi-monoenergetic neutron energy spectra for 246 and 389 MeV (7)Li(p,n) reactions at angles from 0 degrees to 300 degrees

    CERN Document Server

    Iwamoto, Y; Nakamura, T; Nakashima, H; Mares, V; Itoga, T; Matsumoto, T; Nakane, Y; Feldbaumer, E; Jaegerhofer, L; Pioch, C; Tamii, A; Satoh, D; Masuda, A; Sato, T; Iwase, H; Yashima, H; Nishiyama, J; Hagiwara, M; Hatanaka, K; Sakamoto, Y

    2011-01-01

    The authors measured the neutron energy spectra of a quasi-monoenergetic (7)Li(p,n) neutron source with 246 and 389 MeV protons set at seven angles (0 degrees, 2.5 degrees, 5 degrees, 10 degrees, 15 degrees, 20 degrees and 30 degrees), using a time-of-flight (TOF) method employing organic scintillators NE213 at the Research Center for Nuclear Physics (RCNP) of Osaka University. The energy spectra of the source neutrons were precisely deduced down to 2 MeV at 0 degrees and 10 MeV at other angles. The cross-sections of the peak neutron production reaction at 0 degrees were on the 35-40 mb line of other experimental data, and the peak neutron angular distribution agreed well with the Taddeucci formula. Neutron energy spectra below 100 MeV at all angles were comparable, but the shapes of the continuum above 150 MeV changed considerably with the angle. In order to consider the correction required to derive the response in the peak region from the measured total response for high-energy neutron monitors such as DAR...

  12. Spectroscopy of particle-phonon coupled states in $^{133}$Sb by the cluster transfer reaction of $^{132}$Sn on $^{7}$Li

    CERN Multimedia

    We propose to investigate, with MINIBALL coupled to T-REX, the one-valence-proton $^{133}$Sb nucleus by the cluster transfer reaction of $^{132}$Sn on $^{7}$Li. The excited $^{133}$Sb will be populated by transfer of a triton into $^{132}$Sn, followed by the emission of an $\\alpha$-particle (detected in T-REX) and 2 neutrons. The aim of the experiment is to locate states arising from the coupling of the valence proton of $^{133}$Sb to the collective low-lying phonon excitations of $^{132}$Sn (in particular the 3$^−$). According to calculations in the weak-coupling approach, these states lie in the 4$\\, - \\,$5 MeV excitation energy region and in the spin interval 1/2$\\, - \\,$ 19/2, i.e., in the region populated by the cluster transfer reaction. The results will be used to perform advanced tests of different types of nuclear interactions, usually employed in the description of particle-phonon coupled excitations. States arising from couplings of the proton with simpler core excitations, involving few nucleons...

  13. What is the best proton energy for accelerator-based BNCT using the 7Li(p,n)7Be reaction?

    Science.gov (United States)

    Allen, D A; Beynon, T D

    2000-05-01

    With a growing interest in the use of accelerator-based epithermal neutron sources for BNCT programs, in particular those based upon the 7Li(p,n)7Be reaction, there is a need to address the question of "what is the best proton energy to use?" This paper considers this question by using radiation transport calculations to investigate a range of proton energies from 2.15 to 3.5 MeV and a range of moderator sizes. This study has moved away completely from the use of empty therapy beam parameters and instead defines the beam quality and optimizes the moderator design using widely accepted in-phantom treatment planning figures of merit. It is concluded that up to a proton energy of about 2.8 MeV there is no observed variation in the achievable therapy beam quality, but a price is paid in terms of treatment time for not choosing the upper limit of this range. For higher proton energies, the beam quality falls, but with no improvement in treatment time for optimum configurations.

  14. Mechanical Property and Intergranular Corrosion Sensitivity of Zn-Free and Zn-Microalloyed Al-2.7Cu-1.7Li-0.3Mg Alloys

    Science.gov (United States)

    Li, Jin-feng; Xu, Long; Cai, Chao; Chen, Yong-lai; Zhang, Xu-hu; Zheng, Zi-qiao

    2014-11-01

    The influence of 0.72 pct Zn addition on the tensile properties of Al-2.7Cu-1.7Li-0.3Mg alloys was investigated. Their intergranular corrosion (IGC) dependence on aging [T6 type at 423 K (150 °C) and 448 K (175 °C) and T8 type at 423 K (150 °C)] time was studied. An IGC diagram associated with aging process was established. The addition of 0.72 pct Zn enhanced the strength of the Al-Li alloy with T6 type aging at 448 K (175 °C). With aging process, the corrosion mode of the T6-aged Al-Li alloys was changed in the following order: pitting and local IGC (initial aging stage), general IGC (underaging stage), local IGC (near peak-aging stage), and pitting (overaging stage) again. The IGC depth was increased first and then decreased with aging time extension. The corrosion potential change of grains and the microstructure variation were used to explain the IGC sensitivity of the Al-Li alloy with different tempers. Meanwhile, 0.72 pct Zn addition decreased the IGC sensitivity of the Al-Li alloy, especially the T6-aged Al-Li alloy.

  15. A microdosimetric study of {sup 10}B(n,{alpha}){sup 7}Li and {sup 157}Gd(n,{gamma}) reactions for neutron capture therapy

    Energy Technology Data Exchange (ETDEWEB)

    Wang, C.K.C.; Sutton, M.; Evans, T.M. [Georgia Inst. of Tech., Atlanta, GA (United States); Laster, B.H. [Brookhaven National Lab., Upton, NY (United States). Medical Dept.

    1999-01-01

    This paper presents the microdosimetric analysis for the most interesting cell survival experiment recently performed at the Brookhaven National Laboratory (BNL). In this experiment, the cells were first treated with a gadolinium (Gd) labeled tumor-seeking boronated porphyrin (Gd-BOPP) or with BOPP alone, and then irradiated with thermal neutrons. The resulting cell-survival curves indicate that the {sup 157}Gd(n,{gamma}) reactions are very effective in cell killing. The death of a cell treated with Gd-BOPP was attributed to either the {sup 10}B(n,{alpha}){sup 7}Li reactions or the {sup 157}Gd(n,{gamma}) reactions (or both). However, the quantitative relationship between the two types of reaction and the cell-survival fraction was not clear. This paper presents the microdosimetric analysis for the BNL experiment based on the measured experimental parameters, and the results clearly suggest a quantitative relationship between the two types of reaction and the cell survival fraction. The results also suggest new research in gadolinium neutron capture therapy (GdNCT) which may lead to a more practical modality than the boron neutron capture therapy (BNCT) for treating cancers.

  16. NMR logging apparatus

    Energy Technology Data Exchange (ETDEWEB)

    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.

  17. NMR logging apparatus

    Science.gov (United States)

    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.

  18. NMR studies of metalloproteins.

    Science.gov (United States)

    Li, Hongyan; Sun, Hongzhe

    2012-01-01

    Metalloproteins represent a large share of the proteomes, with the intrinsic metal ions providing catalytic, regulatory, and structural roles critical to protein functions. Structural characterization of metalloproteins and identification of metal coordination features including numbers and types of ligands and metal-ligand geometry, and mapping the structural and dynamic changes upon metal binding are significant for understanding biological functions of metalloproteins. NMR spectroscopy has long been used as an invaluable tool for structure and dynamic studies of macromolecules. Here we focus on the application of NMR spectroscopy in characterization of metalloproteins, including structural studies and identification of metal coordination spheres by hetero-/homo-nuclear metal NMR spectroscopy. Paramagnetic NMR as well as (13)C directly detected protonless NMR spectroscopy will also be addressed for application to paramagnetic metalloproteins. Moreover, these techniques offer great potential for studies of other non-metal binding macromolecules.

  19. UC Merced NMR Instrumentation Acquisition

    Science.gov (United States)

    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

  20. FT-IR, NMR SPECTROSCOPIC and QUANTUM MECHANICAL ...

    African Journals Online (AJOL)

    ... and The Authors. Printed in Ethiopia ..... often attributed to the neglected anharmonicity and incomplete inclusion of electronic correlation ... molecule receptor systems using ferrocene's “atomic ball bearing” character as the flexible element.

  1. HIGH FIELD 13C NMR SPECTROSCOPIC ANALYSIS OF THE ...

    African Journals Online (AJOL)

    a

    chloroform-methanol mixture (2:1) for 20 h under nitrogen atmosphere. The extracts were dried ... carbons showed three signals at 173.338, 173.302 and 172.887 ppm. Referring to .... composition of the oil is calculated as: Percentage of Sat ...

  2. NMR study of the paramagnetic state of low-dimensional magnets LiCu{sub 2}O{sub 2} and NaCu{sub 2}O{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Sadykov, A. F., E-mail: sadykov@imp.uran.ru; Piskunov, Yu. V.; Gerashchenko, A. P.; Ogloblichev, V. V.; Smol’nikov, A. G.; Verkhovskii, S. V.; Arapova, I. Yu.; Volkova, Z. N.; Mikhalev, K. N. [Russian Academy of Sciences, Mikheev Institute of Metal Physics, Ural Branch (Russian Federation); Bush, A. A. [Moscow State Technical University of Radio Engineering, Electronics, and Automation (Russian Federation)

    2017-02-15

    A comprehensive NMR study of the magnetic properties of single crystal LiCu{sub 2}O{sub 2} (LCO) and NaCu{sub 2}O{sub 2} (NCO) is carried out in the paramagnetic region of the compounds for various orientations of single crystals in an external magnetic field. The values of the electric-field gradient (EFG) tensor, as well as the dipole and transferred hyperfine magnetic fields for {sup 63,65}Cu, {sup 7}Li, and {sup 23}Na nuclei are determined. The results are compared with the data obtained in previous NMR studies of the magnetically ordered state of LCO/NCO cuprates.

  3. A combination of novel solid-state NMR methods and related software to study molecular assemblies and biomolecules

    NARCIS (Netherlands)

    Gradmann, S.H.E.

    2013-01-01

    Solid-state Nuclear Magnetic Resonance (ssNMR) is a versatile spectroscopic method that can be applied to various samples relevant in life and material science and provides atomic insight into molecular structure, dynamics and assembly. The present thesis describes the diversity and utility of ssNMR

  4. BOOK REVIEW: NMR Imaging of Materials

    Science.gov (United States)

    Blümich, Bernhard

    2003-09-01

    spectroscopic methods to weight or filter the spin signals represents the core of the book. This is a subject where Blümich is deeply involved with substantial contributions. The chapter includes a lot of ideas to provide MR contrast between different regions based on their mobility, diffusion, spin couplings or NMR spectra. After describing NMR imaging methods for solids with broad lines, Blümich spends time on applications in the last two chapters of the book. This part is really fun to read. It underlines the effort to bring NMR into many kinds of manufacturing. Car tyres and high-voltage cables are just two such areas. Elastomeric materials, green-state ceramics and food science represent other interesting fields of applications. This part of the book represents a personal but nevertheless extensive compilation of modern applications. As a matter of course the MOUSE is presented, a portable permanent-magnet based NMR developed by Blümich and his co-workers. Thus the book is not only of interest to NMR spectroscopists but also to people in material science and chemical engineering. The bibliography and indexing are excellent and may serve as an attractive reference source for NMR spectroscopists. The book is the first on the subject and likely to become the standard text for NMR imaging of materials as the books by Abragam, Slicher and Ernst et al are for NMR spectroscopy. The purchase of this beautiful book for people dealing with NMR spectroscopy or medical MRI is highly recommended. Ralf Ludwig

  5. Flavonoids from Curcuma longa leaves and their NMR assignments.

    Science.gov (United States)

    Jiang, Chia-Ling; Tsai, Sheng-Fa; Lee, Shoei-Sheng

    2015-01-01

    Chemical investigation of the n-BuOH-soluble fraction of the EtOH extract of the aerial part of Curcuma longa led to the isolation of 11 flavonol glycosides and one dihydroflavonol glucoside (1) via chromatography over Sephadex LH-20 and Lobar RP-18 columns. Although they are known, the 1H and 13C NMR data recorded in CD3OD rather than the common DMSO-d6 are doubly checked via extensive 2D NMR spectroscopic analyses, leading to some revisions of the reported data, especially for the glycon part.

  6. In situ NMR analysis of fluids contained in sedimentary rock

    Science.gov (United States)

    de Swiet TM; Tomaselli; Hurlimann; Pines

    1998-08-01

    Limitations of resolution and absorption in standard chemical spectroscopic techniques have made it difficult to study fluids in sedimentary rocks. In this paper, we show that a chemical characterization of pore fluids may be obtained in situ by magic angle spinning (MAS) nuclear magnetic resonance (NMR), which is normally used for solid samples. 1H MAS-NMR spectra of water and crude oil in Berea sandstone show sufficient chemical shift resolution for a straightforward determination of the oil/water ratio. Copyright 1998 Academic Press.

  7. Spectroscopic Investigation of the Mechanism of Photocatalysis

    Directory of Open Access Journals (Sweden)

    Yoshio Nosaka

    2014-11-01

    Full Text Available Reaction mechanisms of various kinds of photocatalysts have been reviewed based on the recent reports, in which various spectroscopic techniques including luminol chemiluminescence photometry, fluorescence probe method, electron spin resonance (ESR, and nuclear magnetic resonance (NMR spectroscopy were applied. The reaction mechanisms elucidated for bare and modified TiO2 were described individually. The modified visible light responsive TiO2 photocatalysts, i.e., Fe(III-deposited metal-doped TiO2 and platinum complex-deposited TiO2, were studied by detecting paramagnetic species with ESR, •O2− (or H2O2 with chemiluminescence photometry, and OH radicals with a fluorescence probe method. For bare TiO2, the difference in the oxidation mechanism for the different crystalline form was investigated by the fluorescence probe method, while the adsorption and decomposition behaviors of several amino acids and peptides were investigated by 1H-NMR spectroscopy.

  8. The cross-section data from neutron activation experiments on niobium in the NPI p-7Li quasi-monoenergetic neutron field

    Directory of Open Access Journals (Sweden)

    Simakov S.P.

    2010-10-01

    Full Text Available The reaction of protons on 7Li target produces the high-energy quasi- monoenergetic neutron spectrum with the tail to lower energies. Proton energies of 19.8, 25.1, 27.6, 30.1, 32.6, 35.0 and 37.4 MeV were used to obtain quasi-monoenergetic neutrons with energies of 18, 21.6, 24.8, 27.6, 30.3, 32.9 and 35.6 MeV, respectively. Nb cross-section data for neutron energies higher than 22.5 MeV do not exist in the literature. Nb is the important material for fusion applications (IFMIF as well. The variable-energy proton beam of NPI cyclotron is utilized for the production of neutron field using thin lithium target. The carbon backing serves as the beam stopper. The system permits to produce neutron flux density about 109  n/cm2/s in peak at 30 MeV neutron energy. The niobium foils of 15 mm in diameter and approx. 0.75 g weight were activated. The nuclear spectroscopy methods with HPGe detector technique were used to obtain the activities of produced isotopes. The large set of neutron energies used in the experiment allows us to make the complex study of the cross-section values. The reactions (n,2n, (n,3n, (n,4n, (n,He3, (n,α and (n,2nα are studied. The cross-sections data of the (n,4n and (n,2nα are obtained for the first time. The cross-sections of (n,2n and (n,α reactions for higher neutron energies are strongly influenced by low energy tail of neutron spectra. This effect is discussed. The results are compared with the EAF-2007 library.

  9. Measurement of neutron energy spectra and neutron dose rates from {sup 7}Li(p,n){sup 7}Be reaction induced on thin LiF target

    Energy Technology Data Exchange (ETDEWEB)

    Atanackovic, Jovica, E-mail: atanacjz@gmail.com [Ontario Power Generation, Whitby, ON, Canada L1N 9E3 (Canada); Atomic Energy of Canada Limited, Chalk River Laboratories, Chalk River, Canada K0J 1J0 (Canada); Matysiak, Witold [University of Florida Proton Therapy Institute, Jacksonville, FL 32206 (United States); Dubeau, Jacques; Witharana, Sampath [DETEC, Gatineau, QC, Canada J8T 4J1 (Canada); Waker, Anthony [University of Ontario Institute of Technology, Oshawa, ON, Canada L1H 7K4 (Canada)

    2015-02-21

    The measurements of neutron energy spectra and neutron dose rates were performed using the KN Van de Graaff accelerator, located at the McMaster University Accelerator Laboratory (MAL). Protons were accelerated on the thin lithium fluoride (LiF) target and produced mono-energetic neutrons which were measured using three different spectrometers: Bonner Sphere Spectrometer (BSS), Nested Neutron Spectrometer (NNS), and Rotational Proton Recoil Spectrometer (ROSPEC). The purpose of this work is (1) measurement and quantification of low energy accelerator neutron fields in terms of neutron fluence and dose, (2) comparison of results obtained by three different instruments, (3) comparison of measurements with Monte Carlo simulations based on theoretical neutron yields from {sup 7}Li(p,n){sup 7}Be nuclear reaction, and (4) comparison of results obtained using different neutron spectral unfolding methods. The nominal thickness of the LiF target used in the experiment was 50μg/cm{sup 2}, which corresponds to the linear thickness of 0.19μm and results in approximately 6 keV energy loss for the proton energies used in the experiment (2.2, 2.3, 2.4 and 2.5 MeV). For each of the proton energies, neutron fluence per incident proton charge was measured and several dosimetric quantities of interest in radiation protection were derived. In addition, theoretical neutron yield calculations together with the results of Monte Carlo (MCNP) modeling of the neutron spectra are reported. Consistent neutron fluence spectra were obtained with three detectors and good agreement was observed between theoretically calculated and measured neutron fluences and derived dosimetric quantities for investigated proton energies at 2.3, 2.4 and 2.5 MeV. In the case of 2.2 MeV, some plausibly explainable discrepancies were observed.

  10. Optimization of the proton chopper for {sup 7}Li(p,n) neutron spectrometry using a {sup 3}He ionization chamber

    Energy Technology Data Exchange (ETDEWEB)

    Matysiak, W., E-mail: matysiw@mcmaster.c [Department of Medical Physics and Applied Radiation Sciences, McMaster University, Hamilton, ON, L8S 4K1 (Canada); Chettle, D.R.; Prestwich, W.V.; Byun, S.H. [Department of Medical Physics and Applied Radiation Sciences, McMaster University, Hamilton, ON, L8S 4K1 (Canada)

    2011-02-11

    Thick target {sup 7}Li(p,n) neutron spectra were measured with a {sup 3}He ion chamber in the proton energy region between 1.95 and 2.3 MeV using the McMaster pulsed accelerator neutron source. The pulsed neutron beam was produced by an electrostatic proton chopper to reject the slow neutron detection events, which seriously limit the fast neutron counting rate of the {sup 3}He ion chamber. To collect both arrival time and energy information of {sup 3}He detection events, a custom two-dimensional time-energy analyzer was built using a time scaler and a successive approximation peak-sensing ADC. At each proton energy, the optimum chopper operation was determined by taking into account the two competing requirements: high fast-to-slow neutron ratio and reasonable fast neutron counting rate. The proton pulse widths used were 10 {mu}s for 1.95 and 2.1 MeV proton energies, whereas a shorter, 5 {mu}s proton pulse was used for 2.3 MeV acquisition. The raw data were analyzed using three spectral unfolding methods: a simple division by detection efficiency, an iterative algorithm, and a regularized constrained inversion method. The three methods gave consistent neutron fluence spectra within 20% above 30 keV. Thanks to the enhanced fast-to-slow neutron ratio of the pulsed beam, the full detector response function could be employed in unfolding, which led to an extension of the dynamic energy range as well as a better stability of unfolding process in the low energy region.

  11. Ab initio calculation of accurate dissociation energy,potential energy curve and dipole moment function for the A1∑+ state 7LiH molecule

    Institute of Scientific and Technical Information of China (English)

    Shi De-Heng; Liu Yu-Fang; Sun Jin-Feng; Yang Xiang-Dong; Zhu Zun-Lue

    2006-01-01

    The reasonable dissociation limit of the A1∑+ state 7LiH molecule is obtained. The accurate dissociation energy and the equilibrium geometry of this state are calculated using a symmetry-adapted-cluster configuration-interaction method in complete active space for the first time. The whole potential energy curve and the dipole moment function for the A1∑+ state are calculated over a wide internuclear separation range from about 0.1 to 1.4 nm. The calculated equilibrium geometry and dissociation energy of this potential energy curve are of Re=0.2487 nm and De=1.064 eV,respectively. The unusual negative values of the anharmonicity constant and the vibration-rotational coupling constant are of wexe=-4.7158cm-1 and αe=-0.08649cm-1, respectively. The vertical excitation energy from the ground to the A1∑+ state is calculated and the value is of 3.613eV at 0.15875nm (the equilibrium position of the ground state).The highly anomalous shape of this potential energy curve, which is exceptionally flat over a wide radial range around the equilibrium position, is discussed in detail. The harmonic frequency value of 502.47cm-1 about this state is approximately estimated. Careful comparison of the theoretical determinations with those obtained by previous theories about the A1∑+ state dissociation energy clearly shows that the present calculations are much closer to the experiments than previous theories, thus represents an improvement.

  12. Mobility and relaxation determinations of lithium in lithium aluminate ceramics using solid-state NMR spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, F.F.; Peterson, E.S. [Idaho National Engineering Lab., Idaho Falls, ID (United States); Stebbins, J.F. [Stanford Univ., CA (United States)] [and others

    1995-02-01

    Lithium aluminate is one of the materials being considered for fusion reactor blankets. When preparing the ceramic, it is important to be able to monitor the microstructures since it is a controlling factor in the rate of tritium release from the blanket. Nuclear magnetic resonance spectroscopy (NMR) has been shown to be a useful tool for the nondestructive analysis of ceramics. Studies detailed in this paper include spectral acquisition, assignment, spin-lattice relaxation time measurements, temperature effects, their correlation to structure, and material purity. The ceramic of interest was lithium aluminate, LiAl{sub 5}O{sub 8}. This material was studied by observation of the NMR active nuclei {sup 6}Li, {sup 7}Li, and {sup 27}Al. For these nuclei, spin-lattice relaxation times (T{sub 1}) were measured and were found to vary considerably, correlating to the presence of paramagnetic impurities within the crystalline lattice. Previous research has shown that the coordination about the aluminum nucleus can be determined using {sup 27}Al NMR spectroscopy. Aluminum-27 NMR spectroscopy was successfully applied, and it provided valuable insight into composition of the ceramic. 20 refs., 4 figs., 3 tabs.

  13. Benford distributions in NMR

    CERN Document Server

    Bhole, Gaurav; Mahesh, T S

    2014-01-01

    Benford's Law is an empirical law which predicts the frequency of significant digits in databases corresponding to various phenomena, natural or artificial. Although counter intuitive at the first sight, it predicts a higher occurrence of digit 1, and decreasing occurrences to other larger digits. Here we report the Benford analysis of various NMR databases and draw several interesting inferences. We observe that, in general, NMR signals follow Benford distribution in time-domain as well as in frequency domain. Our survey included NMR signals of various nuclear species in a wide variety of molecules in different phases, namely liquid, liquid-crystalline, and solid. We also studied the dependence of Benford distribution on NMR parameters such as signal to noise ratio, number of scans, pulse angles, and apodization. In this process we also find that, under certain circumstances, the Benford analysis can distinguish a genuine spectrum from a visually identical simulated spectrum. Further we find that chemical-sh...

  14. In situ solid-state NMR spectroscopy of electrochemical cells: batteries, supercapacitors, and fuel cells.

    Science.gov (United States)

    Blanc, Frédéric; Leskes, Michal; Grey, Clare P

    2013-09-17

    Electrochemical cells, in the form of batteries (or supercapacitors) and fuel cells, are efficient devices for energy storage and conversion. These devices show considerable promise for use in portable and static devices to power electronics and various modes of transport and to produce and store electricity both locally and on the grid. For example, high power and energy density lithium-ion batteries are being developed for use in hybrid electric vehicles where they improve the efficiency of fuel use and help to reduce greenhouse gas emissions. To gain insight into the chemical reactions involving the multiple components (electrodes, electrolytes, interfaces) in the electrochemical cells and to determine how cells operate and how they fail, researchers ideally should employ techniques that allow real-time characterization of the behavior of the cells under operating conditions. This Account reviews the recent use of in situ solid-state NMR spectroscopy, a technique that probes local structure and dynamics, to study these devices. In situ NMR studies of lithium-ion batteries are performed on the entire battery, by using a coin cell design, a flat sealed plastic bag, or a cylindrical cell. The battery is placed inside the NMR coil, leads are connected to a potentiostat, and the NMR spectra are recorded as a function of state of charge. (7)Li is used for many of these experiments because of its high sensitivity, straightforward spectral interpretation, and relevance to these devices. For example, (7)Li spectroscopy was used to detect intermediates formed during electrochemical cycling such as LixC and LiySiz species in batteries with carbon and silicon anodes, respectively. It was also used to observe and quantify the formation and growth of metallic lithium microstructures, which can cause short circuits and battery failure. This approach can be utilized to identify conditions that promote dendrite formation and whether different electrolytes and additives can help

  15. Enhanced efficiency of solid-state NMR investigations of energy materials using an external automatic tuning/matching (eATM) robot

    Science.gov (United States)

    Pecher, Oliver; Halat, David M.; Lee, Jeongjae; Liu, Zigeng; Griffith, Kent J.; Braun, Marco; Grey, Clare P.

    2017-02-01

    We have developed and explored an external automatic tuning/matching (eATM) robot that can be attached to commercial and/or home-built magic angle spinning (MAS) or static nuclear magnetic resonance (NMR) probeheads. Complete synchronization and automation with Bruker and Tecmag spectrometers is ensured via transistor-transistor-logic (TTL) signals. The eATM robot enables an automated "on-the-fly" re-calibration of the radio frequency (rf) carrier frequency, which is beneficial whenever tuning/matching of the resonance circuit is required, e.g. variable temperature (VT) NMR, spin-echo mapping (variable offset cumulative spectroscopy, VOCS) and/or in situ NMR experiments of batteries. This allows a significant increase in efficiency for NMR experiments outside regular working hours (e.g. overnight) and, furthermore, enables measurements of quadrupolar nuclei which would not be possible in reasonable timeframes due to excessively large spectral widths. Additionally, different tuning/matching capacitor (and/or coil) settings for desired frequencies (e.g.7Li and 31P at 117 and 122 MHz, respectively, at 7.05 T) can be saved and made directly accessible before automatic tuning/matching, thus enabling automated measurements of multiple nuclei for one sample with no manual adjustment required by the user. We have applied this new eATM approach in static and MAS spin-echo mapping NMR experiments in different magnetic fields on four energy storage materials, namely: (1) paramagnetic 7Li and 31P MAS NMR (without manual recalibration) of the Li-ion battery cathode material LiFePO4; (2) paramagnetic 17O VT-NMR of the solid oxide fuel cell cathode material La2NiO4+δ; (3) broadband 93Nb static NMR of the Li-ion battery material BNb2O5; and (4) broadband static 127I NMR of a potential Li-air battery product LiIO3. In each case, insight into local atomic structure and dynamics arises primarily from the highly broadened (1-25 MHz) NMR lineshapes that the eATM robot is uniquely

  16. Study of the {sup 7}Be(p,{gamma}){sup 8}B and {sup 7}Li(n,{gamma}){sup 8}Li capture reactions using the shell model embedded in the continuum

    Energy Technology Data Exchange (ETDEWEB)

    Bennaceur, K.; Ploszajczak, M. [Grand Accelerateur National d`Ions Lourds (GANIL), 14 - Caen (France); Nowacki, F. [Grand Accelerateur National d`Ions Lourds (GANIL), 14 - Caen (France)]|[Strasbourg-1 Univ., 67 (France). Lab. de Physique Theorique; Okolowicz, J. [Grand Accelerateur National d`Ions Lourds (GANIL), 14 - Caen (France)]|[Institute of Nuclear Physics, Krakow (Poland)

    1999-02-01

    The realistic shell model which includes the coupling between many-particle (quasi-)bound states and the continuum of one-particle scattering states is applied to the spectroscopy of mirror nuclei: {sup 8}B and {sup 8}Li, as well as to the description of low energy cross sections (the astrophysical S factors) in the capture reactions: {sup 7}Be(p,{gamma}){sup 8}B and {sup 7}Li(n,{gamma}){sup 8}Li. (author) 49 refs.

  17. Au, Bi, Co and Nb cross-section measured by quasimonoenergetic neutrons from p + {sup 7}Li reaction in the energy range of 18–36 MeV

    Energy Technology Data Exchange (ETDEWEB)

    Majerle, M., E-mail: majerle@ujf.cas.cz; Bém, P.; Novák, J.; Šimečková, E.; Štefánik, M.

    2016-09-15

    Au, Bi, Co and Nb samples were irradiated several times with quasi-monoenergetic neutrons from p + {sup 7}Li reaction in the energy range of 18–36 MeV. The activities of the samples were measured with the HPGe detector and the reaction rates were calculated. The cross-sections were extracted using the SAND-II method with the reference cross-sections from the EAF-2010 database. The uncertainties of the final results are discussed.

  18. Indirect determination of Li via {sup 74}Ge(n,{gamma}){sup 75m}Ge activation reaction induced by neutrons from {sup 7}Li(p,n){sup 7}Be reaction

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Sanjiv, E-mail: sanjucccm@rediffmail.com [National Centre for Compositional Characterization of Materials, BARC, ECIL Post, Hyderabad 500062 (India); Reddy, G.L.N.; Rao, Pritty [National Centre for Compositional Characterization of Materials, BARC, ECIL Post, Hyderabad 500062 (India); Verma, Rakesh [Analytical Chemistry Division, BARC, Mumbai 400085 (India); Ramana, J.V.; Vikramkumar, S.; Raju, V.S. [National Centre for Compositional Characterization of Materials, BARC, ECIL Post, Hyderabad 500062 (India)

    2012-03-01

    An indirect method to determine Li by {sup 74}Ge(n,{gamma}){sup 75m}Ge activation reaction induced in a high purity Ge (detector) crystal by neutrons from the {sup 7}Li(p,n){sup 7}Be reaction in a typical particle-induced {gamma}-ray emission (PIGE) spectroscopy experimental set-up is described. Performed with proton beams of energies in excess of 1.88 MeV, the threshold energy (E{sub th}) of the {sup 7}Li(p,n){sup 7}Be reaction, the determination involves the activity measurement of {sup 75m}Ge isotope that has a half-life of 47.7 s and decays with the emission of 139 keV {gamma}-rays. Rapidity, selectivity and sensitivity down to ppm levels are the attractive features of the method. It is a suitable alternative to {sup 7}Li(p,p Prime {gamma}){sup 7}Li reaction based PIGE technique in the analyses of matrices that contain light elements such as Be, B, F, Na and Al in significant proportions. Interferences can arise from elements, for example V and Ti, that have E{sub th} Less-Than-Or-Slanted-Equal-To 1.88 MeV for (p,n) reaction. In the case of elements such as Cu, Mo which have with E{sub th} > 1.88 MeV, the incident proton beam energy can be judiciously selected to avoid or minimize an interference. The method, under optimized irradiation conditions, does not entail a risk of neutron stimulated degradation of the performance of the detector. Besides analytical purposes, the measurement of the {sup 75m}Ge activity can serve as a powerful tool to monitor even low ({approx}25 n/cm{sup 2} s) thermal neutron fluxes.

  19. NMR clinical imaging and spectroscopy: Its impact on nuclear medicine

    Energy Technology Data Exchange (ETDEWEB)

    1990-02-02

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

  20. NMR clinical imaging and spectroscopy: Its impact on nuclear medicine

    Energy Technology Data Exchange (ETDEWEB)

    1990-02-02

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

  1. Spectroscopic analysis and control

    Science.gov (United States)

    Tate; , James D.; Reed, Christopher J.; Domke, Christopher H.; Le, Linh; Seasholtz, Mary Beth; Weber, Andy; Lipp, Charles

    2017-04-18

    Apparatus for spectroscopic analysis which includes a tunable diode laser spectrometer having a digital output signal and a digital computer for receiving the digital output signal from the spectrometer, the digital computer programmed to process the digital output signal using a multivariate regression algorithm. In addition, a spectroscopic method of analysis using such apparatus. Finally, a method for controlling an ethylene cracker hydrogenator.

  2. Teaching NMR Using Online Textbooks

    Directory of Open Access Journals (Sweden)

    Joseph P. Hornak

    1999-12-01

    Full Text Available Nuclear magnetic resonance (NMR spectroscopy has almost become an essential analytical tool for the chemist. High-resolution one- and multi-dimensional NMR, timedomain NMR, and NMR microscopy are but a few of the NMR techniques at a chemist's disposal to determine chemical structure and dynamics. Consequently, even small chemistry departments are finding it necessary to provide students with NMR training and experience in at least some of these techniques. The hands-on experience is readily provided with access to state-of-the-art commercial spectrometers. Instruction in the principles of NMR is more difficult to achieve as most instructors try to teach NMR using single organic or analytical chemistry book chapters with static figures. This paper describes an online textbook on NMR spectroscopy called The Basics of NMR (http://www.cis.rit.edu/htbooks/nmr/ suitable for use in teaching the principles of NMR spectroscopy. The book utilizes hypertext and animations to present the principles of NMR spectroscopy. The book can be used as a textbook associated with a lecture or as a stand-alone teaching tool. Conference participants are encouraged to review the textbook and evaluate its suitability for us in teaching NMR spectroscopy to undergraduate chemistry majors.

  3. Occurrence, biological activities and 13C NMR data of amides from Piper (Piperaceae

    Directory of Open Access Journals (Sweden)

    Jeferson C. do Nascimento

    2012-01-01

    Full Text Available This manuscript describes an update review with up to 285 references concerning the occurrence of amides from a variety of species of the genus Piper (Piperaceae. Besides addressing occurrence, this review also describes the biological activities attributed to extracts and pure compounds, a compiled 13C NMR data set, the main correlations between structural and NMR spectroscopic data of these compounds, and employment of hyphened techniques such as LC-MS, GC-MS and NMR for analysis of amides from biological samples and crude Piper extracts.

  4. Study of a Conformational Equilibrium of Lisinopril by HPLC, NMR, and DFT

    Science.gov (United States)

    Bouabdallah, Sondes; Ben Dhia, Med Thaieb; Driss, Med Rida

    2014-01-01

    The isomerization of lisinopril has been investigated using chromatographic, NMR spectroscopic, and theoretical calculations. The NMR data, particularly the NOEDIFF experiments, show that the major species that was eluted first is the trans form. The proportion was 77% and 23% for the trans and cis, respectively. The thermodynamic parameters (ΔH, ΔS, and ΔG) were determined by varying the temperature in the NMR experiments. The interpretations of the experimental data were further supported by DFT/B3LYP calculations. PMID:24707291

  5. Occurrence, biological activities and {sup 13}C NMR data of amides from Piper (Piperaceae)

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Jeferson C. do; Paula, Vanderlucia F. de [Universidade Estadual do Sudoeste da Bahia, Jequie, BA (Brazil). Dept. de Quimica e Exatas; David, Jorge M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; David, Juceni P., E-mail: jmdavid@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Fac. de Farmacia

    2012-07-01

    This manuscript describes an update review with up to 285 references concerning the occurrence of amides from a variety of species of the genus Piper (Piperaceae). Besides addressing occurrence, this review also describes the biological activities attributed to extracts and pure compounds, a compiled {sup 13}C NMR data set, the main correlations between structural and NMR spectroscopic data of these compounds, and employment of hyphened techniques such as LC-MS, GC-MS and NMR for analysis of amides from biological samples and crude Piper extracts. (author)

  6. Study of a Conformational Equilibrium of Lisinopril by HPLC, NMR, and DFT

    Directory of Open Access Journals (Sweden)

    Sondes Bouabdallah

    2014-01-01

    Full Text Available The isomerization of lisinopril has been investigated using chromatographic, NMR spectroscopic, and theoretical calculations. The NMR data, particularly the NOEDIFF experiments, show that the major species that was eluted first is the trans form. The proportion was 77% and 23% for the trans and cis, respectively. The thermodynamic parameters (ΔH, ΔS, and ΔG were determined by varying the temperature in the NMR experiments. The interpretations of the experimental data were further supported by DFT/B3LYP calculations.

  7. Spectroscopic studies of copper enzymes

    Energy Technology Data Exchange (ETDEWEB)

    Dooley, D.M.; Moog, R.; Zumft, W.; Koenig, S.H.; Scott, R.A.; Cote, C.E.; McGuirl, M.

    1986-05-01

    Several spectroscopic methods, including absorption, circular dichroism (CD), magnetic CD (MCD), X-ray absorption, resonance Raman, EPR, NMR, and quasi-elastic light-scattering spectroscopy, have been used to probe the structures of copper-containing amine oxidases, nitrite reductase, and nitrous oxide reductase. The basic goals are to determine the copper site structure, electronic properties, and to generate structure-reactivity correlations. Collectively, the results on the amine oxidases permit a detailed model for the Cu(II) sites in these enzymes to be constructed that, in turn, rationalizes the ligand-binding chemistry. Resonance Raman spectra of the phenylhydrazine and 2,4-dinitrophenyl-hydrazine derivatives of bovine plasma amine oxidase and models for its organic cofactor, e.g. pyridoxal, methoxatin, are most consistent with methoxatin being the intrinsic cofactor. The structure of the Cu(I) forms of the amine oxidases have been investigated by X-ray absorption spectroscopy (XAS); the copper coordination geometry is significantly different in the oxidized and reduced forms. Some anomalous properties of the amine oxidases in solution are explicable in terms of their reversible aggregation, which the authors have characterized via light scattering. Nitrite and nitrous oxide reductases display several novel spectral properties. The data suggest that new types of copper sites are present.

  8. NMR, Water and Plants

    NARCIS (Netherlands)

    As, van H.

    1982-01-01

    This Thesis describes the application of a non-destructive pulsed proton NMR method mainly to measure water transport in the xylem vessels of plant stems and in some model systems. The results are equally well applicable to liquid flow in other biological objects than plants, e.g. flow of blood and

  9. Single-sided NMR

    CERN Document Server

    Casanova, Federico; Blümich, Bernhard

    2011-01-01

    Single-Sided NMR describes the design of the first functioning single-sided tomograph, the related measurement methods, and a number of applications. One of the key advantages to this method is the speed at which the images are obtained.

  10. Autonomous driving in NMR.

    Science.gov (United States)

    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.

  11. Spectroscopic Dosimeter Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Analysis of Phase I test data demonstrates that the Photogenics Spectroscopic Dosimeter will detect neutron energies from 0.8 up to 600 MeV. The detector...

  12. Soils, Pores, and NMR

    Science.gov (United States)

    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 samples (Haber-Pohlmeier et al. 2010). Third, relaxometric information forms the basis of understanding magnetic resonance imaging (MRI) results. The general difficulty of imaging in soils are the inherent fast T2 relaxation times due to i) the small pore sizes, ii) presence of paramagnetic ions in the solid matrix, and iii) diffusion in internal gradients. The last point is important, since echo times can not set shorter than about 1ms for imaging purposes. The way out is either the usage of low fields for imaging in soils or special ultra-short pulse sequences, which do not create echoes. In this presentation we will give examples on conventional imaging of macropore fluxes in soil cores (Haber-Pohlmeier et al. 2010), and the combination with relaxometric imaging, as well as the advantages and drawbacks of low-field and ultra-fast pulse imaging. Also first results on the imaging of soil columns measured by SIP in Project A3 are given. Haber-Pohlmeier, S., S. Stapf, et al. (2010). "Waterflow Monitored by Tracer Transport in Natural Porous Media Using MRI." Vadose Zone J.: submitted. Haber-Pohlmeier, S., S. Stapf, et al. (2010). "Relaxation in a

  13. NMR for chemists and biologists

    CERN Document Server

    Carbajo, Rodrigo J

    2013-01-01

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

  14. NMR magnet technology at MIT

    Energy Technology Data Exchange (ETDEWEB)

    Williams, J.E.C.; Bobrov, E.S.; Iwasa, Y.; Punchard, W.F.B.; Wrenn, J.; Zhukovsky, A. (Massachusetts Inst. of Tech., Cambridge, MA (United States). Francis Bitter National Magnet Lab.)

    1992-01-01

    The design and construction of high field superconducting NMR magnets has much in common with other types of adiabatic superconducting magnets. However, two issues have a particular relevance to NMR magnets. They are field drift and homogeneity. In this paper the control of these factors in the particular context of high field NMR spectrometer magnets is examined.

  15. NMR studies of polysaccharides from brown seaweeds

    Energy Technology Data Exchange (ETDEWEB)

    Noseda, M.D.; Tisher, C.A.; Gorin, P.A.J.; Duarte, M.E.R. [Parana Univ., Curitiba, PR (Brazil). Dept. de Bioquimica; Cerezo, A.S. [Buenos Aires Univ. Nacional (Argentina). Dept. de Quimica Organica

    1997-12-31

    Alginic acid is the major intercellular polysaccharide serving as matrix in the brown algae and is comprised of an unbranched chain of (1->4)-linked {beta}-D-mannuronic acid (M) and {alpha}-L-guluronic acid (G), arranged in a blockwise fashion. The composition of the monomer residues and the block structure varies depending on the source of the polymer. The selective binding of cations to alginate accounts for its ability to form gels, which is dependent on the number and lenght of the G-blocks. They are widely used industrially for their ability to retain water, and for their gelling, viscosifying and stabilizing properties (Smidsrod and draget, 1996). In this study, alginate composition and block structure in Sargassum stenophyllum has been determined by chemical methods and NMR spectroscopic analysis. (author) 4 refs., 3 figs.

  16. Following lithiation fronts in paramagnetic electrodes with in situ magnetic resonance spectroscopic imaging

    Science.gov (United States)

    Tang, Mingxue; Sarou-Kanian, Vincent; Melin, Philippe; Leriche, Jean-Bernard; Ménétrier, Michel; Tarascon, Jean-Marie; Deschamps, Michaël; Salager, Elodie

    2016-11-01

    Li-ion batteries are invaluable for portable electronics and vehicle electrification. A better knowledge of compositional variations within the electrodes during battery operation is, however, still needed to keep improving their performance. Although essential in the medical field, magnetic resonance imaging of solid paramagnetic battery materials is challenging due to the short lifetime of their signals. Here we develop the scanning image-selected in situ spectroscopy approach, using the strongest commercially available magnetic field gradient. We demonstrate the 7Li magnetic resonance spectroscopic image of a 5 mm-diameter operating battery with a resolution of 100 μm. The time-resolved image-spectra enable the visualization in situ of the displacement of lithiation fronts inside thick paramagnetic electrodes during battery operation. Such observations are critical to identify the key limiting parameters for high-capacity and fast-cycling batteries. This non-invasive technique also offers opportunities to study devices containing paramagnetic materials while operating.

  17. Structure Determination of Unknown Organic Liquids Using NMR and IR Spectroscopy: A General Chemistry Laboratory

    Science.gov (United States)

    Pavel, John T.; Hyde, Erin C.; Bruch, Martha D.

    2012-01-01

    This experiment introduced general chemistry students to the basic concepts of organic structures and to the power of spectroscopic methods for structure determination. Students employed a combination of IR and NMR spectroscopy to perform de novo structure determination of unknown alcohols, without being provided with a list of possible…

  18. Self-Association of N-Methylacetamide Examined by Infrared and NMR Spectroscopies

    Science.gov (United States)

    Schenck, Heather L.; Hui, KaWai

    2011-01-01

    These spectroscopic experiments investigate polarity and concentration effects on self-association behavior in N-methylacetamide. Inquiry can be limited to the concentration dependence of hydrogen bonding and estimation of dimerization constant (NMR studies) or to the effect of solvent polarity on extent of hydrogen bonding (IR studies). The…

  19. Self-Association of N-Methylacetamide Examined by Infrared and NMR Spectroscopies

    Science.gov (United States)

    Schenck, Heather L.; Hui, KaWai

    2011-01-01

    These spectroscopic experiments investigate polarity and concentration effects on self-association behavior in N-methylacetamide. Inquiry can be limited to the concentration dependence of hydrogen bonding and estimation of dimerization constant (NMR studies) or to the effect of solvent polarity on extent of hydrogen bonding (IR studies). The…

  20. Structure Determination of Unknown Organic Liquids Using NMR and IR Spectroscopy: A General Chemistry Laboratory

    Science.gov (United States)

    Pavel, John T.; Hyde, Erin C.; Bruch, Martha D.

    2012-01-01

    This experiment introduced general chemistry students to the basic concepts of organic structures and to the power of spectroscopic methods for structure determination. Students employed a combination of IR and NMR spectroscopy to perform de novo structure determination of unknown alcohols, without being provided with a list of possible…

  1. NMR study of 1,4-dihydropyridine derivatives endowed with long alkyl and functionalized chains

    Energy Technology Data Exchange (ETDEWEB)

    Suarez, Margarita; Salfran, Esperanza; Rodriguez, Hortensia; Coro, Julieta, E-mail: msuarez@fq.uh.c [Universidad de La Habana (Cuba). Facultad de Quimica. Lab. de Sintesis Organica; Molero, Dolores; Saez, Elena [Universidad Complutense, Madrid (Spain). CAI-RMN; Martinez-Alvarez, Roberto; Martin, Nazario [Universidad Complutense, Madrid (Spain). Facultad de Quimica. Dept. de Quimica Organica I

    2011-07-01

    The {sup 1}H , {sup 13}C and {sup 15}N NMR spectroscopic data for 1,4-dihydropyridine endowed with long alkyl and functionalized chain on C-3 and C-5, have been fully assigned by combination of one- and two dimensional experiments (DEPT, HMBC, HMQC, COSY, nOe). (author)

  2. Study of the spectroscopic characteristics of methyl (ligand) cobaloximes and their antibacterial activity

    Indian Academy of Sciences (India)

    N Navaneetha; P A Nagarjun; S Satyanarayana

    2007-01-01

    Spectroscopic characterization (IR, NMR and electronic spectra) of methyl (ligand) cobaloxime was done, where ligand = pyrazole, dimethyl pyrazole, alanine and alanine methyl ester. The frequency changes in the IR spectra and shifts in the NMR were explained on the basis of basicity of the ligand, steric hindrance, HSAB principle and - back-bonding from metal to ligand. Alanine and alanine methyl ester form more stable complexes than pyrazole and dimethyl pyrazole. Based on their IR and 1H NMR spectra it is inferred that pyrazole and dimethylpyrazole bind to Co (III) via N-2 ring nitrogen, i.e. monodentate coordination.

  3. NMR of unfolded proteins

    Indian Academy of Sciences (India)

    Amarnath Chtterjee; Ashutosh Kumar; Jeetender Chugh; Sudha Srivastava; Neel S Bhavesh; Ramakrishna V Hosur

    2005-01-01

    In the post-genomic era, as more and more genome sequences are becoming known and hectic efforts are underway to decode the information content in them, it is becoming increasingly evident that flexibility in proteins plays a crucial role in many of the biological functions. Many proteins have intrinsic disorder either wholly or in specific regions. It appears that this disorder may be important for regulatory functions of the proteins, on the one hand, and may help in directing the folding process to reach the compact native state, on the other. Nuclear magnetic resonance (NMR) has over the last two decades emerged as the sole, most powerful technique to help characterize these disordered protein systems. In this review, we first discuss the significance of disorder in proteins and then describe the recent developments in NMR methods for their characterization. A brief description of the results obtained on several disordered proteins is presented at the end.

  4. Molecular structure, NMR, UV-Visible, vibrational spectroscopic and HOMO, LUMO analysis of (E)-1-(2, 6-bis (4-methoxyphenyl)-3, 3-dimethylpiperidine-4-ylidene)-2-(3-(3, 5-dimethyl-1H-pyrazol-1-yl) pyrazin-2-yl) hydrazine by DFT method

    Science.gov (United States)

    Alphonsa, A. Therasa; Loganathan, C.; Anand, S. Athavan Alias; Kabilan, S.

    2016-02-01

    We have synthesized (E)-1-(2, 6-bis (4-methoxyphenyl)-3, 3-dimethylpiperidine-4-ylidene)-2-(3-(3, 5-dimethyl-1H-pyrazol-1-yl) pyrazin-2-yl) hydrazine (PM6). It was characterized using FT-IR, FT-Raman, 1H NMR, 13C NMR techniques. To interpret the experimental data, ab initio computations of the vibrational frequencies were carried out using the Gaussian 09 program followed by the full optimizations done using Density Functional Theory (DFT) at B3LYP/6-311 G(d,p) level. The combined use of experiments and computations allowed a firm assignment of the majority of observed bands for the compound. The calculated stretching frequencies have been found to be in good agreement with the experimental frequencies. The electronic and charge transfer properties have been explained on the basis of highest occupied molecular orbitals (HOMOs), lowest unoccupied molecular orbitals (LUMOs) and density of states (DOS). The absorption spectra have been computed by using time dependent density functional theory (TD-DFT). 1H and 13C NMR spectra were recorded and 1H and 13C NMR chemical shifts of the molecule were calculated using the gauge independent atomic orbital (GIAO) method. From the optimized geometry of the molecule, molecular electrostatic potential (MEP) distribution, frontier molecular orbitals (FMOs) of the title compound have been calculated in the ground state theoretically. The theoretical results showed good agreement with the experimental values.

  5. NMR studies of metalloproteins

    OpenAIRE

    Li, H; H. Sun

    2011-01-01

    Metalloproteins represent a large share of the proteomes, with the intrinsic metal ions providing catalytic, regulatory, and structural roles critical to protein functions. Structural characterization of metalloproteins and identification of metal coordination features including numbers and types of ligands and metal-ligand geometry, and mapping the structural and dynamic changes upon metal binding are significant for understanding biological functions of metalloproteins. NMR spectroscopy has...

  6. Dose distributions in a human head phantom for neutron capture therapy using moderated neutrons from the 2.5 MeV proton-7Li reaction or from fission of 235U

    Science.gov (United States)

    Tanaka, Kenichi; Kobayashi, Tooru; Sakurai, Yoshinori; Nakagawa, Yoshinobu; Endo, Satoru; Hoshi, Masaharu

    2001-10-01

    The feasibility of neutron capture therapy (NCT) using an accelerator-based neutron source of the 7Li(p,n) reaction produced by 2.5 MeV protons was investigated by comparing the neutron beam tailored by both the Hiroshima University radiological research accelerator (HIRRAC) and the heavy water neutron irradiation facility in the Kyoto University reactor (KUR-HWNIF) from the viewpoint of the contamination dose ratios of the fast neutrons and the gamma rays. These contamination ratios to the boron dose were estimated in a water phantom of 20 cm diameter and 20 cm length to simulate a human head, with experiments by the same techniques for NCT in KUR-HWNIF and/or the simulation calculations by the Monte Carlo N-particle transport code system version 4B (MCNP-4B). It was found that the 7Li(p,n) neutrons produced by 2.5 MeV protons combined with 20, 25 or 30 cm thick D2O moderators of 20 cm diameter could make irradiation fields for NCT with depth-dose characteristics similar to those from the epithermal neutron beam at the KUR-HWNIF.

  7. Dose distributions in a human head phantom for neutron capture therapy using moderated neutrons from the 2.5 MeV proton-{sup 7}Li reaction or from fission of {sup 235}U

    Energy Technology Data Exchange (ETDEWEB)

    Tanaka, Kenichi [Department of Nuclear Engineering, Kyoto University, Yoshida-honmachi, Sakyo-ku, Kyoto (Japan); Kobayashi, Tooru; Sakurai, Yoshinori [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennan-gun, Osaka (Japan); Nakagawa, Yoshinobu [National Kagawa Children' s Hospital, Zentsuji-cho, Zentsuji, Kagawa (Japan); Endo, Satoru [Department of Applied Nuclear Physics, Hiroshima University, Kagamiyama, Higashi-Hiroshima, Hiroshima (Japan); Hoshi, Masaharu [Research Institute for Radiation Biology and Medicine, Hiroshima University, Kasumi, Minami-ku, Hiroshima (Japan)

    2001-10-01

    The feasibility of neutron capture therapy (NCT) using an accelerator-based neutron source of the {sup 7}Li(p,n) reaction produced by 2.5 MeV protons was investigated by comparing the neutron beam tailored by both the Hiroshima University radiological research accelerator (HIRRAC) and the heavy water neutron irradiation facility in the Kyoto University reactor (KUR-HWNIF) from the viewpoint of the contamination dose ratios of the fast neutrons and the gamma rays. These contamination ratios to the boron dose were estimated in a water phantom of 20 cm diameter and 20 cm length to simulate a human head, with experiments by the same techniques for NCT in KUR-HWNIF and/or the simulation calculations by the Monte Carlo N-particle transport code system version 4B (MCNP-4B). It was found that the {sup 7}Li(p,n) neutrons produced by 2.5 MeV protons combined with 20, 25 or 30 cm thick D{sub 2}O moderators of 20 cm diameter could make irradiation fields for NCT with depth-dose characteristics similar to those from the epithermal neutron beam at the KUR-HWNIF. (author)

  8. Characteristics of boron-dose enhancer dependent on dose protocol and {sup 10}B concentration for BNCT using near-threshold {sup 7}Li(p,n){sup 7}Be direct neutrons

    Energy Technology Data Exchange (ETDEWEB)

    Tanaka, Kenichi [Research Institute for Radiation Biology and Medicine, Hiroshima University, Kasumi, Minami-ku, Hiroshima 734-8553 (Japan); Kobayashi, Tooru [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennann-gun, Osaka 590-0494 (Japan); Bengua, Gerard [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennann-gun, Osaka 590-0494 (Japan); Nakagawa, Yoshinobu [National Kagawa Children' s Hospital, Zentsuji-cho, Zentsuji, Kagawa 765-8501 (Japan); Endo, Satoru [Research Institute for Radiation Biology and Medicine, Hiroshima University, Kasumi, Minami-ku, Hiroshima 734-8553 (Japan); Hoshi, Masaharu [Research Institute for Radiation Biology and Medicine, Hiroshima University, Kasumi, Minami-ku, Hiroshima 734-8553 (Japan)

    2005-01-07

    The dependence of boron-dose enhancer (BDE) characteristics on dose protocol and {sup 10}B concentration was evaluated for BNCT using near-threshold {sup 7}Li(p,n){sup 7}Be direct neutrons. The treatable protocol depth (TPD) was utilized as an evaluation index. MCNP calculations were performed for near-threshold {sup 7}Li(p,n){sup 7}Be at a proton energy of 1.900 MeV and for a polyethylene BDE. The effect of dose protocol on BDE characteristics was reflected in terms of the optimum BDE thickness needed for maximum TPD which was found to be independent of the treatable dose but was observed to vary for different combinations of the tolerance doses for heavy charged particles and gamma rays. For the {sup 10}B concentration dependence, the TPD was increased by increasing the T/N ratio, i.e., the ratio of the {sup 10}B concentration in the tumour ({sup 10}B{sub Tumour}) to that in the normal tissue ({sup 10}B{sub Normal}), and by increasing {sup 10}B{sub Tumour} and {sup 10}B{sub Normal} at constant T/N ratio. It was found that the use of BDE becomes unnecessary from the viewpoint of increasing the TPD, when {sup 10}B{sub Tumour} is over a certain level which is decided by the conditions of the dose protocol.

  9. Study of the reduction in detection limits of track detectors used for {sup 10}B(n,α){sup 7}Li reaction rate measure through annealing and chemical etching experiments; Estudo da reducao nos limites de deteccao de detectores de tracos utilizados na medida de taxa de reacao {sup 10}B(n, α){sup 7}Li atraves de experimentos de annealing e ataque quimico

    Energy Technology Data Exchange (ETDEWEB)

    Vasconcellos, Herminiane L.; Smilgys, Barbara; Guedes, Sandro, E-mail: hluizav@ifi.unicamp.br [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Instituto de Fisica Gleb Wataghin; Castro, Vinicius A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Engenharia Nuclear

    2013-08-15

    The Boron Neutron Capture Therapy (BNCT) is an experimental radiotherapy for cancer treatment. It is based on {sup 10}B(n, α){sup 7}Li reaction, which can be measured by track detectors capable of recording events that strike them. With this recording, it is possible to determine the number of alpha particles and recoiling Lithium-7 nucleus, reaction products, and from this information, which amount of radiation dose a patient is exposed to. In this work, PADC detectors were characterized, irradiated at the IEA-R1 IPEN/CNEN reactor to assess the contribution of the{sup 10}B(n, α){sup 7}Li reaction and protons from fast neutron scattering with the elements that compounds the tissue. With the aim of reducing the proton background, the detectors were subjected to heating experiments at 80°C for periods in the range 0-100 hours. This was done in order to restore partially modified structure of the detector, causing a reduction in the size and density of tracks. This effect is known as annealing. For the visualization of tracks at microscope, detectors were made three chemical attacks with sodium hydroxide (NaOH) for 30, 60 and 90 minutes at 70°C. It was observed a reduction in the track density achieving a plateau heating time of 50 hours. For detectors that have not undergone annealing and were etched with another etchant, PEW solution, a reduction of 87% in track density was obtained. (author)

  10. High-resolution NMR characterization of a spider-silk mimetic composed of 15 tandem repeats and a CRGD motif

    OpenAIRE

    McLachlan, Glendon D; Slocik, Joseph; Mantz, Robert; Kaplan, David; Cahill, Sean; Girvin, Mark; Greenbaum, Steve

    2008-01-01

    Multidimensional solution NMR spectroscopic techniques have been used to obtain atomic level information about a recombinant spider silk construct in hexafluoro-isopropanol (HFIP). The synthetic 49 kDa silk-like protein mimics authentic silk from Nephila clavipes, with the inclusion of an extracellular matrix recognition motif. 2D 1H-15N HSQC NMR spectroscopy reveals 33 cross peaks, which were assigned to amino acid residues in the semicrystalline repeat units. Signals from the amorphous segm...

  11. {sup 7}Li and {sup 19}F diffusion coefficients and thermal properties of non-aqueous electrolyte solutions for rechargeable lithium batteries

    Energy Technology Data Exchange (ETDEWEB)

    Capiglia, C.; Saito, Y.; Kageyama, H. [Osaka National Research Inst., AIST, Ikeda (Japan); Mustarelli, P. [Consiglio Nazionale delle Ricerche, Pavia (Italy). Centro di Studio per la Termodinamica ed Elettrochimica dei Sistemi Salini Fusi e Solidi; Pavia Univ. (Italy). Ist. di Fisica Chimica; Iwamoto, T.; Tabuchi, T.; Tukamoto, H. [Japan Storage Battery Co. Ltd., Kyoto (Japan). Corporate Research and Development Center

    1999-09-01

    In this paper, electrolyte solutions of ethylene carbonate (EC) and ethylene methylene carbonate (EMC) with different salts as LiPF{sub 6}, LiBF{sub 4} and LiN(SO{sub 2}C{sub 2}F{sub 5}){sub 2} were prepared and characterized using Pulsed Field Gradient (PFG) NMR and DSC. Cation transport numbers, {tau}{sup +}, ranging between 0.37 and 0.49 were obtained. The maximum value of 0.49 was obtained in the case of a 0.5 M solution of LiBF{sub 4} in 2:8 EC:EMC. The DSC data suggest that the increase of EMC stabilizes the electrolyte solution towards low temperature, and than a 2:8 EC:EMC ratio assures good stability at low temperature to the electrolyte solution. While LiN(SO{sub 2}C{sub 2}F{sub 5}){sub 2} seems to score the best in terms of low temperature stability, LiPF{sub 6} may offer the best cost/performances compromise. (orig.)

  12. Labelling analysis for ¹³C MFA using NMR spectroscopy.

    Science.gov (United States)

    Jouhten, Paula; Maaheimo, Hannu

    2014-01-01

    NMR spectroscopy is an efficient method for analyzing (13)C labelling of cellular metabolites. The strength of it is especially the ability to provide direct quantitative positional information on the (13)C labelling status of carbon atoms in metabolites. NMR spectroscopic methods allow also for detection of contiguously (13)C-labelled fragments in the carbon backbones of the metabolites. Furthermore, the recent developments of NMR spectroscopy hardware have substantially improved the sensitivity of the methods. In this chapter we describe a method for analyzing the (13)C labelling of the biomass amino acids for metabolic flux analysis, sample preparation for NMR spectroscopy, acquiring and processing the NMR spectra, and extracting the (13)C labelling information from the NMR data. Different NMR methods are applied depending on the (13)C labelling strategy chosen. These strategies include uniform (13)C labelling, positional (13)C labelling, or a combination of both. Not only the preparation of sample for analysis of (13)C labelling in proteinogenic amino acids in biomass is described, but also the necessary modifications to the method when analysis of (13)C labelling in free metabolic intermediates is of interest. Finally the strategies for using the different NMR-detected (13)C labelling data in (13)C MFA are discussed.

  13. Transformer-coupled NMR probe

    Science.gov (United States)

    Utsuzawa, Shin; Mandal, Soumyajit; Song, Yi-Qiao

    2012-03-01

    In this study, we propose an NMR probe circuit that uses a transformer with a ferromagnetic core for impedance matching. The ferromagnetic core provides a strong but confined coupling that result in efficient energy transfer between the sample coil and NMR spectrometer, while not disturbing the B1 field generated by the sample coil. We built a transformer-coupled NMR probe and found that it offers comparable performance (loss NQR.

  14. Shell model and spectroscopic factors

    Energy Technology Data Exchange (ETDEWEB)

    Poves, P. [Madrid Univ. Autonoma and IFT, UAM/CSIC, E-28049 (Spain)

    2007-07-01

    In these lectures, I introduce the notion of spectroscopic factor in the shell model context. A brief review is given of the present status of the large scale applications of the Interacting Shell Model. The spectroscopic factors and the spectroscopic strength are discussed for nuclei in the vicinity of magic closures and for deformed nuclei. (author)

  15. Magic Angle Spinning NMR Metabolomics

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Z.

    2016-05-31

    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.

  16. Structural properties of carbon nanotubes derived from 13C NMR

    KAUST Repository

    Abou-Hamad, E.

    2011-10-10

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

  17. Study of β-NMR for Liquid Biological Samples

    CERN Document Server

    Beattie, Caitlin

    2017-01-01

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

  18. TDPAC and β-NMR applications in chemistry and biochemistry

    Science.gov (United States)

    Jancso, Attila; Correia, Joao G.; Gottberg, Alexander; Schell, Juliana; Stachura, Monika; Szunyogh, Dániel; Pallada, Stavroula; Lupascu, Doru C.; Kowalska, Magdalena; Hemmingsen, Lars

    2017-06-01

    Time differential perturbed angular correlation (TDPAC) of γ-rays spectroscopy has been applied in chemistry and biochemistry for decades. Herein we aim to present a comprehensive review of chemical and biochemical applications of TDPAC spectroscopy conducted at ISOLDE over the past 15 years, including elucidation of metal site structure and dynamics in proteins and model systems. β-NMR spectroscopy is well established in nuclear physics, solid state physics, and materials science, but only a limited number of applications in chemistry have appeared. Current endeavors at ISOLDE advancing applications of β-NMR towards chemistry and biochemistry are presented, including the first experiment on 31Mg2+ in an ionic liquid solution. Both techniques require the production of radioisotopes combined with advanced spectroscopic instrumentation present at ISOLDE.

  19. Three dimensional nuclear magnetic resonance spectroscopic imaging of sodium ions using stochastic excitation and oscillating gradients

    Energy Technology Data Exchange (ETDEWEB)

    Frederick, B.deB. [California Univ., Berkeley, CA (United States)]|[Lawrence Berkeley Lab., CA (United States)

    1994-12-01

    Nuclear magnetic resonance (NMR) spectroscopic imaging of {sup 23}Na holds promise as a non-invasive method of mapping Na{sup +} distributions, and for differentiating pools of Na{sup +} ions in biological tissues. However, due to NMR relaxation properties of {sup 23}Na in vivo, a large fraction of Na{sup +} is not visible with conventional NMR imaging methods. An alternate imaging method, based on stochastic excitation and oscillating gradients, has been developed which is well adapted to measuring nuclei with short T{sub 2}. Contemporary NMR imaging techniques have dead times of up to several hundred microseconds between excitation and sampling, comparable to the shortest in vivo {sup 23}Na T{sub 2} values, causing significant signal loss. An imaging strategy based on stochastic excitation has been developed which greatly reduces experiment dead time by reducing peak radiofrequency (RF) excitation power and using a novel RF circuit to speed probe recovery. Continuously oscillating gradients are used to eliminate transient eddy currents. Stochastic {sup 1}H and {sup 23}Na spectroscopic imaging experiments have been performed on a small animal system with dead times as low as 25{mu}s, permitting spectroscopic imaging with 100% visibility in vivo. As an additional benefit, the encoding time for a 32x32x32 spectroscopic image is under 30 seconds. The development and analysis of stochastic NMR imaging has been hampered by limitations of the existing phase demodulation reconstruction technique. Three dimensional imaging was impractical due to reconstruction time, and design and analysis of proposed experiments was limited by the mathematical intractability of the reconstruction method. A new reconstruction method for stochastic NMR based on Fourier interpolation has been formulated combining the advantage of a several hundredfold reduction in reconstruction time with a straightforward mathematical form.

  20. Applications of high resolution NMR to geochemistry: crystalline, glass, and molten silicates

    Energy Technology Data Exchange (ETDEWEB)

    Schneider, E.

    1985-11-01

    The nuclear spin interactions and the associated quantum mechanical dynamics which are present in solid state NMR are introduced. A brief overview of aluminosilicate structure is presented and crystalline structure is then reviewed, with emphasis on the contributions made by /sup 29/Si NMR spectroscopy. The local structure of glass aluminosilicates as observed by NMR, is presented with analysis of the information content of /sup 29/Si spectra. A high-temperature (to 1300/sup 0/C) NMR spectroscopic investigation of the local environment and dynamics of molecular motion in molten aluminosilicates is described. A comparison is made of silicate liquid, glass, and crystalline local structure. The atomic and molecular motions present in a melt are investigated through relaxation time (T/sub 1/ and T/sub 2/) measurements as a function of composition and temperature for /sup 23/Na and /sup 29/Si.

  1. Efficient cellular solid-state NMR of membrane proteins by targeted protein labeling

    Energy Technology Data Exchange (ETDEWEB)

    Baker, Lindsay A. [University of Oxford, Oxford Particle Imaging Centre, The Wellcome Trust Centre for Human Genetics, Division of Structural Biology, Nuffield Department of Medicine (United Kingdom); Daniëls, Mark; Cruijsen, Elwin A. W. van der; Folkers, Gert E.; Baldus, Marc, E-mail: m.baldus@uu.nl [Utrecht University, NMR Spectroscopy, Department of Chemistry, Faculty of Science, Bijvoet Center for Biomolecular Research (Netherlands)

    2015-06-15

    Solid-state NMR spectroscopy (ssNMR) has made significant progress towards the study of membrane proteins in their native cellular membranes. However, reduced spectroscopic sensitivity and high background signal levels can complicate these experiments. Here, we describe a method for ssNMR to specifically label a single protein by repressing endogenous protein expression with rifampicin. Our results demonstrate that treatment of E. coli with rifampicin during induction of recombinant membrane protein expression reduces background signals for different expression levels and improves sensitivity in cellular membrane samples. Further, the method reduces the amount of time and resources needed to produce membrane protein samples, enabling new strategies for studying challenging membrane proteins by ssNMR.

  2. NMR Studies of 3-Acylcamphor

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    NMR studies of some chiral 3-acyclcamphor were conducted.A complete assignment was given to 3-(4-pyridyl)carbonylcamphor by the 2D NMR technology.Assignments were also given to other b -diketones.The results showed that those 3-acylcamphors exist in the enol forms,while 2-benzoyl menthone exists in diketon form.

  3. NMR in pulsed magnetic field

    KAUST Repository

    Abou-Hamad, Edy

    2011-09-01

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

  4. Calibration of the radiation monitors from DESY and SPring-8 at the quasi-mono-energetic neutron beams using 100 and 300 MeV 7Li(p,n) reaction at RCNP in Osaka Japan in November 2014

    Science.gov (United States)

    Leuschner, Albrecht; Asano, Yoshihiro; Klett, Alfred

    2017-09-01

    At the ring cyclotron facility of the Research Center for Nuclear Physics (RCNP) Osaka University, Osaka, Japan a series of measurement campaigns had been continued with quasi mono-energetic neutron beams in November 2014. A 7Li target was bombarded with 100 and 300 MeV protons and the generated neutron beams were directed into a long time-of-flight tunnel at 0 and 25 degrees deflection angle with respect to the proton beam. At a distance of 41 m the cross section of the neutron beam was large enough for the illumination of square meter sized objects like extended range rem-counters. The research institutes SPring-8/RIKEN, Japan, and DESY, Germany, participated in this campaign for the calibration of 4 different types of active ambient dose rate monitors: LB 6411, LB 6411-Pb, LB 6419 and LB 6420. The measurements of their responses are reported and compared with the calculated values.

  5. Measurement of Cross Sections for the 10B(n,α)'7Li Reaction at 4.0 and 5.0 MeV Using an Asymmetrical Twin Gridded Ionization Chamber

    Institute of Scientific and Technical Information of China (English)

    ZHANG Guo-Hui; LIU Xiang; LIU Jia-Ming; XUE Zhi-Hua; WU Hao; CHEN Jin-Xiang

    2011-01-01

    @@ Cross sections of the 10B(n, α) 7Li reaction (including the total, the "leaking" alpha, forward alpha and backward alpha parts) at En=4.0 and 5.OMcV were measured using an asymmetrical twin gridded ionization chamber and two back-to-back 10B samples.Measurements were performed at the 4.5MV Van de Graaff accelerator of Peking University.Monoenergetic neutrons were produced through the 2H(d, n)3 He reaction with a deuterium gas target.Absolute neutron flux was determined by a 238 U sample set inside the gridded ionization chamber and a BF3 long counter was employed as a neutron flux monitor and for normalization.The present results are compared with previous measurements and evaluations.

  6. Structural Biology: Practical NMR Applications

    CERN Document Server

    Teng, Quincy

    2005-01-01

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

  7. Fundamentals of Protein NMR Spectroscopy

    CERN Document Server

    Rule, Gordon S

    2006-01-01

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

  8. High-power electron beam tests of a liquid-lithium target and characterization study of (7)Li(p,n) near-threshold neutrons for accelerator-based boron neutron capture therapy.

    Science.gov (United States)

    Halfon, S; Paul, M; Arenshtam, A; Berkovits, D; Cohen, D; Eliyahu, I; Kijel, D; Mardor, I; Silverman, I

    2014-06-01

    A compact Liquid-Lithium Target (LiLiT) was built and tested with a high-power electron gun at Soreq Nuclear Research Center (SNRC). The target is intended to demonstrate liquid-lithium target capabilities to constitute an accelerator-based intense neutron source for Boron Neutron Capture Therapy (BNCT) in hospitals. The lithium target will produce neutrons through the (7)Li(p,n)(7)Be reaction and it will overcome the major problem of removing the thermal power >5kW generated by high-intensity proton beams, necessary for sufficient therapeutic neutron flux. In preliminary experiments liquid lithium was flown through the target loop and generated a stable jet on the concave supporting wall. Electron beam irradiation demonstrated that the liquid-lithium target can dissipate electron power densities of more than 4kW/cm(2) and volumetric power density around 2MW/cm(3) at a lithium flow of ~4m/s, while maintaining stable temperature and vacuum conditions. These power densities correspond to a narrow (σ=~2mm) 1.91MeV, 3mA proton beam. A high-intensity proton beam irradiation (1.91-2.5MeV, 2mA) is being commissioned at the SARAF (Soreq Applied Research Accelerator Facility) superconducting linear accelerator. In order to determine the conditions of LiLiT proton irradiation for BNCT and to tailor the neutron energy spectrum, a characterization of near threshold (~1.91MeV) (7)Li(p,n) neutrons is in progress based on Monte-Carlo (MCNP and Geant4) simulation and on low-intensity experiments with solid LiF targets. In-phantom dosimetry measurements are performed using special designed dosimeters based on CR-39 track detectors.

  9. NMR molecular photography

    CERN Document Server

    Khitrin, A K; Fung, B M; Khitrin, Anatoly K.; Ermakov, Vladimir L.

    2002-01-01

    A procedure is described for storing a 2D pattern consisting of 32x32 = 1024 bits in a spin state of a molecular system and then retrieving the stored information as a stack of NMR spectra. The system used is a nematic liquid crystal, the protons of which act as spin clusters with strong intramolecular interactions. The technique used is a programmable multi-frequency irradiation with low amplitude. When it is applied to the liquid crystal, a large number of coherent long-lived 1H response signals can be excited, resulting in a spectrum showing many sharp peaks with controllable frequencies and amplitudes. The spectral resolution is enhanced by using a second weak pulse with a 90 phase shift, so that the 1024 bits of information can be retrieved as a set of well-resolved pseudo-2D spectra reproducing the input pattern.

  10. Online T5 learning model to enhance chemistry students’ understanding of NMR spectroscopy

    Directory of Open Access Journals (Sweden)

    Saksri Supasorn

    2014-08-01

    Full Text Available Regular lecture-based teaching approaches sometimes fail to enhance students’ understanding of some practice-based chemistry topics such as Nuclear Magnetic Resonance (NMR spectroscopy. A new task-based approach called the T5 learning model was introduced for 48 students studying NMR in the Spectroscopic Methods for Chemical Identification course in 2011. Four different NMR learning environments based on T5 learning models were developed. The students were requested to participate in the following online processes in each environment: 1 complete an individual task, 2 provide feedback and evaluate three anonymous peer tasks, 3 adjust their individual task and evaluate peer feedback, 4 complete a team task and evaluate the effort of each group member, and 5 get feedback from instructor to fulfill understanding. The result showed that the students obtained post-achievement NMR score (mean 24.25, SD 4.80 statistically significantly higher than pre- achievement score (mean 12.29, SD 1.69 at p-value of 0.05. In addition, the implementation of T5-D4LP NMR course in each year during 2010-2012 showed that the students achieved high score (about 70% in the NMR topics. The student evaluation of the T5 NMR learning environments revealed that they agreed that peer feedback with instructor facilitation engaged them in deep learning and effectively promoted their conceptual understanding.

  11. Recent Advances in Solution NMR: Fast Methods and Heteronuclear Direct Detection

    Energy Technology Data Exchange (ETDEWEB)

    Felli, I.C. [CERM and Depatment of Chemistry, University of Florence, 50019 (Italy); Brutscher, B. [DSV-IBS, 38027 Grenoble (France)

    2009-07-01

    Today, NMR spectroscopy is the technique of choice to investigate molecular structure, dynamics, and interactions in solution at atomic resolution. A major limitation of NMR spectroscopy for the study of biological macromolecules such as proteins, nucleic acids, and their complexes, has always been its low sensitivity, a consequence of the weak magnetic spin interactions. Therefore many efforts have been invested in the last decade to improve NMR instrumentation in terms of experimental sensitivity. As a result of these efforts, the availability of high-field magnets, cryogenically cooled probes, and probably in the near future hyper-polarization techniques, the intrinsic NMR sensitivity has increased by at least one order of magnitude. Stimulated by new challenges in the life sciences, these technical improvements have triggered the development of new NMR methods for the study of molecular systems of increasing size and complexity. Herein, we focus on two examples of recently developed NMR methodologies. First, advanced multidimensional data acquisition schemes provide a speed increase of several orders of magnitude. Second, NMR methods based on the direct detection of low-gamma nuclei present a new spectroscopic tool, highly complementary to conventional NMR techniques. These new methods provide powerful new NMR tools for the study of short-lived molecules, large and intrinsically unstructured proteins, paramagnetic systems, as well as for the characterization of molecular kinetic processes at atomic resolution. These examples illustrate how NMR is continuously adapting to the new challenges in the life sciences, with the focus shifting from the characterization of single biomolecules to an integrated view of interacting molecular networks observed at varying levels of biological organization. (authors)

  12. Chiral Ionic Liquids in Chromatographic Separation and Spectroscopic Discrimination

    Science.gov (United States)

    Li, Min; Bwambok, David K.; Fakayode, Sayo O.; Warner, Isiah M.

    Chiral ionic liquids (CILs) are a subclass of ionic liquids (ILs) in which the cation, anion, or both may be chiral. The chirality can be central, axial, or planar. CILs possess a number of unique advantageous properties which are inherited from ionic liquids including negligible vapor pressure, wide liquidus temperature range, high thermal stability, and high tunability. Due to their dual functionalities as chiral selectors and chiral solvents simultaneously, CILs recently have been widely used both in enantiomeric chromatographic separation and in chiral spectroscopic discrimination. In this chapter, the various applications of CILs in chiral chromatographic separations such as GC, HPLC, CE, and MEKC are reviewed. The applications of CILs in enantiomeric spectroscopic discrimination using techniques such as NMR, fluorescence, and NIR are described. In addition, chiral recognition and separation mechanism using the CILs as chiral selectors or chiral solvents is also discussed.

  13. Studies on the Interactions between Potassium oxalato oxodiperoxovanadate and Histidine by NMR and MS

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Multi-nuclear NMR and ESI-MS have been applied to study the interactions between oxalato-oxodiperoxovanadate and histidine in neutral solution. Coordination between the complex and histidine was monitored by 51V NMR. A pair of new isomers produced via vanadium atom binding separately to N1 and N3 of the imidazole ring of histidine was characterized by several spectroscopic methods. Experimental results show that the structure activity relationship of peroxovanadium complexes bearing organic ligands may be related to the specific recognition between peroxovanadium and histidine residue of tyrosine phosphatase.

  14. NMR spectrometers as "magnetic tongues"

    DEFF Research Database (Denmark)

    Malmendal, Anders; Amoresano, Claudia; Trotta, Roberta

    2011-01-01

    opened up the possibility to calibrate the sensory perception. In this frame, we have tested the potentiality of nuclear magnetic resonance spectroscopy as a predictive tool to measure sensory descriptors. In particular, we have used an NMR metabolomic approach that allowed us to differentiate...... the analyzed samples based on their chemical composition. We were able to correlate the NMR metabolomic fingerprints recorded for canned tomato samples to the sensory descriptors bitterness, sweetness, sourness, saltiness, tomato and metal taste, redness, and density, suggesting that NMR might be a very useful...

  15. Annual reports on NMR spectroscopy

    CERN Document Server

    Webb, Graham A; McCarthy, M J

    1995-01-01

    Over recent years, no other technique has grown to such importance as that of NMR spectroscopy. It is used in all branches of science where precise structural determination is required and where the nature of interactions and reactions in solution is being studied. Annual Reports on NMR Spectroscopy has established itself as a means for the specialist and non-specialist alike to become familiar with new applications of the technique in all branches of chemistry, including biochemistry, and pharmaceutics. This volume focuses on theoretical aspects of NMR nuclear shielding and on applications of

  16. β-NMR sample optimization

    CERN Document Server

    Zakoucka, Eva

    2013-01-01

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

  17. Integrative NMR for biomolecular research.

    Science.gov (United States)

    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 ).

  18. Compact orthogonal NMR field sensor

    Science.gov (United States)

    Gerald, II, Rex E.; Rathke, Jerome W [Homer Glen, IL

    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.

  19. Optical pumping and xenon NMR

    Energy Technology Data Exchange (ETDEWEB)

    Raftery, M. Daniel [Univ. of California, Berkeley, CA (United States)

    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.

  20. Optical pumping and xenon NMR

    Energy Technology Data Exchange (ETDEWEB)

    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.

  1. NMR characterization of thin films

    Science.gov (United States)

    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.

  2. (1)H-(13)C NMR-Based Profiling of Biotechnological Starch Utilization.

    Science.gov (United States)

    Sundekilde, Ulrik K; Meier, Sebastian

    2016-10-04

    Starch is used in food- and nonfood applications as a renewable and degradable source of carbon and energy. Insight into the chemical detail of starch degradation remains challenging as the starch constituents amylose and amylopectin are homopolymers. We show that considerable molecular detail of starch fragmentation can be obtained from multivariate analysis of spectral features in optimized (1)H-(13)C NMR spectroscopy of starch fragments to identify relevant features that distinguish processes in starch utilization. As a case study, we compare the profiles of starch fragments in commercial beer samples. Spectroscopic profiles of homooligomeric starch fragments can be excellent indicators of process conditions. In addition, differences in the structure and composition of starch fragments have predictive value for downstream process output such as ethanol production from starch. Thus, high-resolution (1)H-(13)C NMR spectroscopic profiles of homooligomeric fragment mixtures in conjunction with chemometric methods provide a useful addition to the analytical chemistry toolbox of biotechnological starch utilization.

  3. $\\gamma$- spectroscopy of n-rich $^{95,96}$Rb nuclei by the incomplete fusion reaction of $^{94}$Kr on $^{7}$Li: Introduction to HIE-ISOLDE studies of n-rich Sb and Tl isotopes with Sn and Hg radioactive beams.

    CERN Document Server

    Fornal, B; Bednarczyk, P; Cieplicka, N; Krolas, W; Maj, A; Leoni, S; Benzoni, G; Blasi, N; Bottoni, S; Bracco, A; Camera, F; Crespi, F; Million, B; Morales, A; Wieland, O; Rusek, K; Lunardi, S; Mengoni, D; Recchia, F; Ur, CA; Valiente-Dobon, J; de France, G; Clement, E; Elseviers, J; Flavigny, F; Huyse, M; Raabe, R; Sambi, S; Van Duppen, P; Sferrazza, M; Simpson, G; Georgiev, G; Sotty, C; Blazhev, A; German, R; Siebeck, B; Seidlitz, M; Reiter, P; Warr, N; Boenig, S; Ilieva, S; Kroell, T; Scheck, M; Thurauf, M; Gernhaeuser, R; Mucher, D; Janssens, R; Carpenter, MP; Zhu, S; Marginean, NM; Balabanski, D; Kowalska, M

    2012-01-01

    $\\gamma$- spectroscopy of n-rich $^{95,96}$Rb nuclei by the incomplete fusion reaction of $^{94}$Kr on $^{7}$Li: Introduction to HIE-ISOLDE studies of n-rich Sb and Tl isotopes with Sn and Hg radioactive beams.

  4. NMR studies of the internal electric field in a single crystal of the quasi-one-dimensional conductor Li0.9Mo6O17

    Science.gov (United States)

    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.

  5. Human in vivo phosphate metabolite imaging with 31P NMR.

    Science.gov (United States)

    Bottomley, P A; Charles, H C; Roemer, P B; Flamig, D; Engeseth, H; Edelstein, W A; Mueller, O M

    1988-07-01

    Phosphorus (31P) spectroscopic images showing the distribution of high-energy phosphate metabolites in the human brain have been obtained at 1.5 T in scan times of 8.5 to 34 min at 27 and 64 cm3 spatial resolution using pulsed phase-encoding gradient magnetic fields and three-dimensional Fourier transform (3DFT) techniques. Data were acquired as free induction decays with a quadrature volume NMR detection coil of a truncated geometry designed to optimize the signal-to-noise ratio on the coil axis on the assumption that the sample noise represents the dominant noise source, and self-shielded magnetic field gradient coils to minimize eddy-current effects. The images permit comparison of metabolic data acquired simultaneously from different locations in the brain, as well as metabolite quantification by inclusion of a vial containing a standard of known 31P concentration in the image array. Values for the NMR visible adenosine triphosphate in three individuals were about 3 mM of tissue. The ratio of NMR detectable phosphocreatine to ATP in brain was 1.15 +/- 0.17 SD in these experiments. Potential sources of random and systematic error in these and other 31P measurements are identified.

  6. 1H-13C NMR-based profiling of biotechnological starch utilization

    DEFF Research Database (Denmark)

    Sundekilde, Ulrik K.; Meier, Sebastian

    2016-01-01

    Starch is used in food-and non-food applications as a renewable and degradable source of carbon and energy. Insight into the chemical detail of starch degradation remains challenging as the starch constituents amylose and amylopectin are homopolymers. We show that considerable molecular detail......-resolution 1H-13C NMR spectroscopic profiles of homooligomeric fragment mixtures in conjunction with chemometric methods provide a useful addition to the analytical chemistry toolbox of biotechnologi-cal starch utilization....

  7. Spectroscopic study of molecular structure, antioxidant activity and biological effects of metal hydroxyflavonol complexes

    Science.gov (United States)

    Samsonowicz, Mariola; Regulska, Ewa

    2017-02-01

    Flavonols with varied hydroxyl substitution can act as strong antioxidants. Thanks to their ability to chelate metals as well as to donate hydrogen atoms they have capacity to scavenge free radicals. Their metal complexes are often more active in comparison with free ligands. They exhibit interesting biological properties, e.g. anticancer, antiphlogistic and antibacterial. The relationship between molecular structure and their biological properties was intensively studied using spectroscopic methods (UV-Vis, IR, Raman, NMR, ESI-MS). The aim of this paper is review on spectroscopic analyses of molecular structure and biological activity of hydroxyflavonol metal complexes.

  8. A Critical Evaluation of the Quality of Published (13)C NMR Data in Natural Product Chemistry.

    Science.gov (United States)

    Robien, Wolfgang

    2017-01-01

    Nuclear Magnetic Resonance spectroscopy contributes very efficiently to the structure elucidation process in organic chemistry. Carbon-13 NMR spectroscopy allows direct insight into the skeleton of organic compounds and therefore plays a central role in the structural assignment of natural products. Despite this important contribution, there is no established and well-accepted workflow protocol utilized during the first steps of interpreting spectroscopic data and converting them into structural fragments and then combining them, by considering the given spectroscopic constraints, into a final proposal of structure. The so-called "combinatorial explosion" in the process of structure generation allows in many cases the generation of reasonable alternatives, which are usually ignored during manual interpretation of the measured data leading ultimately to a large number of structural revisions. Furthermore, even when the determined structure is correct, problems may exist such as assignment errors, ignoring chemical shift values, or assigning lines of impurities to the compound under consideration. An extremely large heterogeneity in the presentation of carbon NMR data can be observed, but, as a result of the efficiency and precision of spectrum prediction, the published data can be analyzed in substantial detail.This contribution presents a comprehensive analysis of frequently occurring errors with respect to (13)C NMR spectroscopic data and proposes a straightforward protocol to eliminate a high percentage of the most obvious errors. The procedure discussed can be integrated readily into the processes of submission and peer-reviewing of manuscripts.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-01-15

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

  10. Systematic comparison of crystal and NMR protein structures deposited in the protein data bank.

    Science.gov (United States)

    Sikic, Kresimir; Tomic, Sanja; Carugo, Oliviero

    2010-09-03

    Nearly all the macromolecular three-dimensional structures deposited in Protein Data Bank were determined by either crystallographic (X-ray) or Nuclear Magnetic Resonance (NMR) spectroscopic methods. This paper reports a systematic comparison of the crystallographic and NMR results deposited in the files of the Protein Data Bank, in order to find out to which extent these information can be aggregated in bioinformatics. A non-redundant data set containing 109 NMR - X-ray structure pairs of nearly identical proteins was derived from the Protein Data Bank. A series of comparisons were performed by focusing the attention towards both global features and local details. It was observed that: (1) the RMDS values between NMR and crystal structures range from about 1.5 Å to about 2.5 Å; (2) the correlation between conformational deviations and residue type reveals that hydrophobic amino acids are more similar in crystal and NMR structures than hydrophilic amino acids; (3) the correlation between solvent accessibility of the residues and their conformational variability in solid state and in solution is relatively modest (correlation coefficient = 0.462); (4) beta strands on average match better between NMR and crystal structures than helices and loops; (5) conformational differences between loops are independent of crystal packing interactions in the solid state; (6) very seldom, side chains buried in the protein interior are observed to adopt different orientations in the solid state and in solution.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Matwiyoff, N.A.

    1983-01-01

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

  13. Development of a quasi-monoenergetic neutron field using the 7Li(p,n)7Be reaction in the energy range from 250 to 390 MeV at RCNP.

    Science.gov (United States)

    Taniguchi, S; Nakao, N; Nakamura, T; Yashima, H; Iwamoto, Y; Satoh, D; Nakane, Y; Nakashima, H; Itoga, T; Tamii, A; Hatanaka, K

    2007-01-01

    A quasi-monoenergetic neutron field using the (7)Li(p,n)(7)Be reaction has been developed at the ring cyclotron facility at the Research Center for Nuclear Physics (RCNP), Osaka University. Neutrons were generated from a 10-mm-thick Li target injected by 250, 350 and 392 MeV protons and neutrons produced at 0 degrees were extracted into the time-of-flight (TOF) room of 100-m length through the concrete collimator of 10 x 12 cm aperture and 150 cm thickness. The neutron energy spectra were measured by a 12.7-cm diam x 12.7-cm long NE213 organic liquid scintillator using the TOF method. The peak neutron fluence was 1.94 x 10(10), 1.07 x 10(10) and 1.50 x 10(10) n sr(-1) per muC of 250, 350 and 392 MeV protons, respectively. The neutron spectra generated from various thick (stopping length) targets of carbon, aluminium, iron and lead, bombarded by 250 and 350 MeV protons, were also measured with the TOF method. Although these measurements were performed to obtain thick target neutron yields, they are also used as a continuous energy neutron field. These neutron fields are very useful for characterising neutron detectors, measuring neutron cross sections, testing irradiation effects for various materials and performing neutron shielding experiments.

  14. Density-independent folding analysis of the sup 6 sup , sup 7 Li elastic scattering at intermediate energies 24.10H; 24.50; 25.70; 27.20

    CERN Document Server

    El-Azab-Farid, M

    2000-01-01

    The differential cross sections of sup 6 sup , sup 7 Li elastic scattering from sup 1 sup 2 C, sup 2 sup 8 S, sup 4 sup 0 Ca, sup 5 sup 8 Ni, sup 9 sup 0 Zr and sup 2 sup 0 sup 8 Pb targets at E/A sub P =12.5 -53 MeV / u have been analyzed using density-independent double folding optical potentials. The calculations are built upon a very simple phenomenological nucleon-nucleon effective interaction, which is represented by a single Yukawa term with a complex strength. The complex microscopic potentials have successfully reproduced the elastic scattering data for most of the analyzed sets. However, more success has been obtained when the single Yukawa term was considered for the real part only while the imaginary part was formulated in a phenomenological Woods-Saxon form. The predictions of the calculated potentials are compared with those obtained by the phenomenological and the M3Y double folded optical potentials. The effects of the knock-on exchange contribution, the variation of the range of the interacti...

  15. Physical and electrochemical characterization of 0.3Li2MnO3 x 0.7LiMn0.60Ni0.25Co0.15O2 material for Li secondary battery.

    Science.gov (United States)

    Kim, Jeong-Min; Choi, Man-Soo; Jin, Bong-Soo; Wang, Guoxiu; Kim, Hyun-Soo

    2014-10-01

    The 0.3Li2MnO3 x 0.7LiMn0.60Ni0.25Co0.15O2 cathode materials were synthesized using a coprecipitation method at a various heat-treatment temperature. From XRD pattern analysis, pure layered structure without impurities was confirmed from all samples and the peak intensity of Li2MnO3 was increased as the heat-treatment temperature increased. The primary particle size increased approximately from 100 nm to 500 nm with increasing heat-treatment temperature. The initial discharge capacity of the materials obtained at 950 degrees C was 235 mA h/g at 0.1 C rate, but then decreased down to 228 mA h/g with further increasing heat-treatment temperature. And, in the voltage range of 2.0-4.6 V, the electrode heat-treated at 900 degrees C showed the highest capacity retention of 68% at 5 C rate against to 0.1 C rate.

  16. The use of enriched 6Li and 7Li Lif:Mg,Cu,P glass-rod thermoluminescent dosemeters for linear accelerator out-of-field radiation dose measurements.

    Science.gov (United States)

    Takam, R; Bezak, E; Liu, G; Marcu, L

    2012-06-01

    (6)LiF:Mg,Cu,P and (7)LiF:Mg,Cu,P glass-rod thermoluminescent dosemeters (TLDs) were used for measurements of out-of-field photon and neutron doses produced by Varian iX linear accelerator. Both TLDs were calibrated using 18-MV X-ray beam to investigate their dose-response sensitivity and linearity. CR-39 etch-track detectors (Luxel+, Landauer) were employed to provide neutron dose data to calibrate (6)LiF:Mg,Cu,P TLDs at various distances from the isocentre. With cadmium filters employed, slow neutrons (neutrons. The average in-air photon dose equivalents per monitor unit (MU) ranged from 1.5±0.4 to 215.5±94.6 μSv at 100 and 15 cm from the isocentre, respectively. Based on the cross-calibration factors obtained with CR-39 etch-track detectors, the average in-air fast neutron dose equivalents per MU range from 10.6±3.8 to 59.1±49.9 μSv at 100 and 15 cm from the isocentre, respectively. Contribution of thermal neutrons to total neutron dose equivalent was small: 3.1±7.2 μSv per MU at 15 cm from the isocentre.

  17. NMR Dynamic Studies in Living Systems

    Institute of Scientific and Technical Information of China (English)

    闫永彬; 范明杰; 罗雪春; 张日清

    2002-01-01

    Nuclear magnetic resonance (NMR) can noninvasively monitor the intracellular concentrations and kinetic properties of numerous inorganic and organic compounds. These characteristics have made NMR a useful tool for dynamic studies of living systems. Applications of NMR to living systems have successfully extended to many areas, including studies of metabolic regulation, ion transport, and intracellular reaction rates in vivo. The major purpose of this review is to summarize the results that can be obtained by modern NMR techniques in living systems. With the advances of new techniques, NMR measurements of various nuclides have been performed for specific physiological purposes. Although some technical problems still remain and there are still discrepancies between NMR and traditional biochemical results, the abundant and unique information obtained from NMR spectra suggests that NMR will be more extensively applied in future studies of living systems. The fast development of these new techniques is providing many new NMR applications in living systems, as well as in structural biology.

  18. 113Cd solid-state NMR for probing the coordination sphere in metal-organic frameworks.

    Science.gov (United States)

    Kuttatheyil, Anusree Viswanath; Handke, Marcel; Bergmann, Jens; Lässig, Daniel; Lincke, Jörg; Haase, Jürgen; Bertmer, Marko; Krautscheid, Harald

    2015-01-12

    Spectroscopic techniques are a powerful tool for structure determination, especially if single-crystal material is unavailable. (113)Cd solid-state NMR is easy to measure and is a highly sensitive probe because the coordination number, the nature of coordinating groups, and the geometry around the metal ion is reflected by the isotropic chemical shift and the chemical-shift anisotropy. Here, a detailed investigation of a series of 27 cadmium coordination polymers by (113)Cd solid-state NMR is reported. The results obtained demonstrate that (113)Cd NMR is a very sensitive tool to characterize the cadmium environment, also in non-single-crystal materials. Furthermore, this method allows the observation of guest-induced phase transitions supporting understanding of the structural flexibility of coordination frameworks.

  19. NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

    Energy Technology Data Exchange (ETDEWEB)

    Richards, T.

    1984-09-01

    NMR imaging, NMR spectroscopic, and histopathologic techniques were used to study the proton relaxation time and related biochemical changes in the central nervous system after helium beam in vivo irradiation of the rodent brain. The spectroscopic observations reported in this dissertation were made possible by development of methods for measuring the NMR parameters of the rodent brain in vivo and in vitro. The methods include (1) depth selective spectroscopy using an optimization of rf pulse energy based on a priori knowledge of N-acetyl aspartate and lipid spectra of the normal brain, (2) phase-encoded proton spectroscopy of the living rodent using a surface coil, and (3) dual aqueous and organic tissue extraction technique for spectroscopy. Radiation induced increases were observed in lipid and p-choline peaks of the proton spectrum, in vivo. Proton NMR spectroscopy measurements on brain extracts (aqueous and organic solvents) were made to observe chemical changes that could not be seen in vivo. Radiation-induced changes were observed in lactate, GABA, glutamate, and p-choline peak areas of the aqueous fraction spectra. In the organic fraction, decreases were observed in peak area ratios of the terminal-methyl peaks, the N-methyl groups of choline, and at a peak at 2.84 ppM (phosphatidyl ethanolamine and phosphatidyl serine resonances) relative to TMS. With histology and Evans blue injections, blood-brain barrier alternations were seen as early as 4 days after irradiation. 83 references, 53 figures.

  20. Synthesis, Mesogenic and Spectroscopic Properties of 2,5-Disubstituted Thiophene Derivatives

    Institute of Scientific and Technical Information of China (English)

    HAN Jie; WANG Yan-Mei; WANG Xiao-Guang

    2006-01-01

    Two series of 2,5-disubstituted thiophene derivatives (series 1: 2,5-bis(p-alkoxyphenylethynyl)thiophene and series 2: 2,5-bis[p-(p-alkoxyphenylethynyl)(phenylethynyl)]thiophene) were synthesized and characterized by 1H NMR, 13C NMR, HRMS and elemental analysis. The relationship between the structure and the mesogenic and spectroscopic properties has been discussed. The results show thatcompounds 1a-1f all exhibited an enantiotropic nematic mesophase, which was confirmed by the polarized optical microscopy (POM), differential scanning calorimeter (DSC) and variable temperature powder X-ray diffraction (PXRD). In contrast, the extended onjugatedanalogues 2a-2b had no liquid crystal properties. As for the spectroscopic properties, ncorporating more phenylethynyl units results in red-shifted absorption and emission spectra, greatly enhanced quantum efficiency.

  1. Synthesis, XRD crystal structure, spectroscopic characterization (FT-IR, 1H and 13C NMR), DFT studies, chemical reactivity and bond dissociation energy studies using molecular dynamics simulations and evaluation of antimicrobial and antioxidant activities of a novel chalcone derivative, (E)-1-(4-bromophenyl)-3-(4-iodophenyl)prop-2-en-1-one

    Science.gov (United States)

    Zainuri, D. Alwani; Arshad, Suhana; Khalib, N. Che; Razak, I. Abdul; Pillai, Renjith Raveendran; Sulaiman, S. Fariza; Hashim, N. Shafiqah; Ooi, K. Leong; Armaković, Stevan; Armaković, Sanja J.; Panicker, C. Yohannan; Van Alsenoy, C.

    2017-01-01

    In the present study, the title compound named as (E)-1-(4-bromophenyl)-3-(4-iodophenyl)prop-2-en-1-one was synthesized and structurally characterized by single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system with P21/c space group with the unit cell parameters of a = 16.147 (2) Å, b = 14.270 (2) Å, c = 5.9058 (9) Å, β = 92.577 (3)° and Z = 4. The molecular geometry obtained from X-Ray structure determination was optimized by Density Functional Theory (DFT) using B3LYP/6-31G+(d, p)/Lanl2dz(f) method in the ground state. The IR spectrum was recorded and interpreted in details with the aid of Density Functional Theory (DFT) calculations and Potential Energy Distribution (PED) analysis. In order to investigate local reactivity properties of the title molecule, we have conducted DFT calculations of average local ionization energy surface and Fukui functions which were mapped to the electron density surface. In order to predict the open air stability and possible degradation properties, within DFT approach, we have also calculated bond dissociation energies. 1H and 13C NMR spectra were recorded and chemical shifts were calculated theoretically and compared with the experimental values. In addition, in vitro antimicrobial results show that the title compound has great potential of antibacterial activity against Staphylococcus aureus, Staphylococcus epidermidis and Micrococcus luteus bacteria and antifungal activity against Candida albicans in comparison to some reported chalcone derivatives. Antioxidant studies revealed the highest metal chelating activity of this compound.

  2. Experimental and theoretical (FT-IR, FT-Raman, UV-vis, NMR) spectroscopic analysis and first order hyperpolarizability studies of non-linear optical material: (2E)-3-[4-(methylsulfanyl) phenyl]-1-(4-nitrophenyl) prop-2-en-1-one using density functional theory.

    Science.gov (United States)

    Kumar, Amit; Deval, Vipin; Tandon, Poonam; Gupta, Archana; Deepak D'silva, E

    2014-09-15

    A combined experimental and theoretical investigation on FT-IR, FT-Raman, NMR, UV-vis spectra of a chalcone derivative (2E)-3-[4-(methylsulfanyl) phenyl]-1-(4-nitrophenyl) prop-2-en-1-one (4N4MSP) has been reported. 4N4MSP has two planar rings connected through conjugated double bond and it provides a necessary configuration to show non-linear optical (NLO) response. The molecular structure, fundamental vibrational frequencies and intensity of the vibrational bands are interpreted with the aid of structure optimizations and normal coordinate force field calculations based on density functional theory (DFT) with B3LYP functional and 6-311++G(d,p) basis set combination. The analysis of the fundamental modes was made with the help of potential energy distribution (PED). Molecular electrostatic potential (MEP) surface was plotted over the geometry primarily for predicting sites and relative reactivities towards electrophilic and nucleophilic attack. The delocalization of electron density of various constituents of the molecule has been discussed with the aid of NBO analysis. The electronic properties, such as excitation energies, oscillator strength, wavelengths, HOMO and LUMO energies, were calculated by time-dependent density functional theory (TD-DFT) and the results complement the experimental findings. The recorded and calculated 1H chemical shifts in gas phase and MeOD solution are gathered for reliable calculations of magnetic properties. Thermodynamic properties like heat capacity (C°p,m), entropy (S°m), enthalpy (H°m) have been calculated for the molecule at the different temperatures. Based on the finite-field approach, the non-linear optical (NLO) parameters such as dipole moment, mean polarizability, anisotropy of polarizability and first order hyperpolarizability of 4N4MSP molecule are calculated. The predicted first hyperpolarizability shows that the molecule has a reasonably good nonlinear optical (NLO) behavior.

  3. NMR studies of actinide dioxides

    Energy Technology Data Exchange (ETDEWEB)

    Tokunaga, Y. [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan)], E-mail: tokunaga.yo@jaea.go.jp; Sakai, H.; Fujimoto, T.; Kambe, S.; Walstedt, R.E.; Ikushima, K.; Yasuoka, H. [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Aoki, D.; Homma, Y. [Institute for Materials Research, Tohoku University, Oarai, Ibaraki 311-1313 (Japan); Haga, Y.; Matsuda, T.D.; Ikeda, S.; Yamamoto, E.; Nakamura, A. [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Shiokawa, Y. [Institute for Materials Research, Tohoku University, Oarai, Ibaraki 311-1313 (Japan); Nakajima, K.; Arai, Y. [Department of Nuclear Energy System, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Onuki, Y. [Advanced Science Research Center, Japan Atomic Energy Agency, Tokai, Ibaraki 319-1195 (Japan); Department of Physics, Osaka University, Toyonaka, Osaka 560-0043 (Japan)

    2007-10-11

    {sup 17}O NMR measurements have been performed on a series of the actinide dioxides, UO{sub 2}, NpO{sub 2} and PuO{sub 2}. Although the {sup 17}O NMR spectra in these materials are similar at higher temperatures, the low-temperature spectra present are significantly different. In UO{sub 2} we have observed a wide spectrum, forming a rectangular shape below T{sub N}=30 K. In NpO{sub 2}, on the other hand, the spectra broaden rather gradually and exhibit a two-peak structure below T{sub 0}=26 K. In PuO{sub 2}, neither spectrum broadening nor splitting has been observed. We show that these NMR spectra clearly indicate the different nature of the low-temperature magnetic ground states in these actinide compounds.

  4. NMR and dynamics of biopolymers

    Energy Technology Data Exchange (ETDEWEB)

    Lian, L.Y.; Barsukov, I.L. [Leicester Univ. (United Kingdom)

    1994-12-31

    Several basic experimental analytical NMR techniques that are frequently used for the qualitative and quantitative analysis of dynamic and exchange processes, focusing on proteins systems, are described: chemical exchange (slow exchange, fast exchange, intermediate exchange), heteronuclear relaxation measurements (relaxation parameters, strategy of relaxation data analysis, experimental results and examples, motional model interpretation of relaxation data, homonuclear relaxation); slow large-scale exchange and hydrogen-deuterium exchange are also studied: mechanisms of hydrogen exchange in a native protein, methods for measuring amide exchange rates by NMR, interpretation of amide exchange rates. 9 fig., 3 tab., 56 ref.

  5. Spectral Estimation of NMR Relaxation

    Science.gov (United States)

    Naugler, David G.; Cushley, Robert J.

    2000-08-01

    In this paper, spectral estimation of NMR relaxation is constructed as an extension of Fourier Transform (FT) theory as it is practiced in NMR or MRI, where multidimensional FT theory is used. nD NMR strives to separate overlapping resonances, so the treatment given here deals primarily with monoexponential decay. In the domain of real error, it is shown how optimal estimation based on prior knowledge can be derived. Assuming small Gaussian error, the estimation variance and bias are derived. Minimum bias and minimum variance are shown to be contradictory experimental design objectives. The analytical continuation of spectral estimation is constructed in an optimal manner. An important property of spectral estimation is that it is phase invariant. Hence, hypercomplex data storage is unnecessary. It is shown that, under reasonable assumptions, spectral estimation is unbiased in the context of complex error and its variance is reduced because the modulus of the whole signal is used. Because of phase invariance, the labor of phasing and any error due to imperfect phase can be avoided. A comparison of spectral estimation with nonlinear least squares (NLS) estimation is made analytically and with numerical examples. Compared to conventional sampling for NLS estimation, spectral estimation would typically provide estimation values of comparable precision in one-quarter to one-tenth of the spectrometer time when S/N is high. When S/N is low, the time saved can be used for signal averaging at the sampled points to give better precision. NLS typically provides one estimate at a time, whereas spectral estimation is inherently parallel. The frequency dimensions of conventional nD FT NMR may be denoted D1, D2, etc. As an extension of nD FT NMR, one can view spectral estimation of NMR relaxation as an extension into the zeroth dimension. In nD NMR, the information content of a spectrum can be extracted as a set of n-tuples (ω1, … ωn), corresponding to the peak maxima

  6. Seleno-auranofin (Et3PAuSe-tagl): synthesis, spectroscopic (EXAFS, 197Au Mössbauer, 31P, 1H, 13C, and 77Se NMR, ESI-MS) characterization, biological activity, and rapid serum albumin-induced triethylphosphine oxide generation.

    Science.gov (United States)

    Hill, David T; Isab, Anvarhusein A; Griswold, Don E; DiMartino, Michael J; Matz, Elizabeth D; Figueroa, Angel L; Wawro, Joyce E; DeBrosse, Charles; Reiff, William M; Elder, Richard C; Jones, Benjamin; Webb, James W; Shaw, C Frank

    2010-09-06

    Seleno-auranofin (SeAF), an analogue of auranofin (AF), the orally active antiarthritic gold drug in clinical use, was synthesized and has been characterized by an array of physical techniques and biological assays. The Mössbauer and extended X-ray absorption fine structure (EXAFS) parameters of the solid compound demonstrate a linear P-Au-Se coordination environment at a gold(I) center, analogous to the structure of auranofin. The (31)P, (13)C, and (1)H NMR spectra of SeAF in chloroform solution closely resemble those of auranofin. The (77)Se spectrum consists of a singlet at 481 ppm, consistent with a metal-bound selenolate ligand. The absence of (2)J(PSe) coupling in the (31)P and (77)Se spectra may arise from dynamic processes occurring in solution or because the (2)J(PSe) coupling constants are smaller than the observed bandwidths. Electrospray ionization mass spectrometry (ESI-MS) spectra of SeAF in 50:50 methanol-water exhibited strong signals for [(Et(3)P)(2)Au](+), [(Et(3)PAu)(2)-mu-Se-tagl](+), and [Au(Se-tagl)(2)](-), which arise from ligand scrambling reactions. Three assays of the anti-inflammatory activity of SeAF allowed comparison to AF. SeAF exhibited comparable activity in the topically administered murine arachadonic acid-induced and phorbol ester-induced anti-inflammatory assays but was inactive in the orally administered carrageenan-induced assay in rats. However, in vivo serum gold levels were comparable in the rat, suggesting that differences between the in vivo metabolism of the two compounds, leading to differences in transport to the inflamed site, may account for the differential activity in the carrageenan-induced assay. Reactions of serum albumin, the principal transport protein of gold in the serum, demonstrated formation of AlbSAuPEt(3) at cysteine 34 and provided evidence for facile reduction of disulfide bonds at cysteine 34 and very rapid formation of Et(3)P=O, a known metabolite of auranofin.

  7. Solid state NMR investigation of a novel Li ion ceramic electrolyte. Li doped BPO sub 4

    CERN Document Server

    Dodd, A J

    2002-01-01

    Over the last decade lithium ion conducting batteries have emerged as the leading technology in battery materials. Their performance, however, is limited to applications below around 50 deg C by the liquid nature of the electrolytes used. In the quest for a solid state electrolyte for use in high temperature applications the nano-crystalline ceramic lithium doped boron phosphate material was developed. Solid state nuclear magnetic resonance (NMR) has been employed to investigate some of the fundamental properties of this material including ionic mobility, defect structure, sample purity and ionic distribution. The findings of this work show that when synthesised at a reaction temperature above 600 deg C the loss of boron from the structure results in the incorporation of vacancy sites about which the Li ions gather in small clusters. Multiple-pulse multiple-quantum spin counting techniques are employed in an effort to count the number of quadrupolar sup 7 Li nuclei interacting in a cluster though it is ultima...

  8. "Solvent Effects" in 1H NMR Spectroscopy.

    Science.gov (United States)

    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)

  9. Simple preparation of new N-aryl-N-(3-indolmethyl acetamides and their spectroscopic analysis

    Directory of Open Access Journals (Sweden)

    José A. Henao

    2009-12-01

    Full Text Available To prepare new indolic molecules and characterize them by spectroscopic methods. Materials and methods: All reagentswere purchased from Aldrich, commercial grade. The purity of the products and the composition of the reaction mixtures were monitoredby thin layer chromatography over Silufol UV254 0.25 mm-thick chromatoplates. Product isolation and purification were performed bycolumn chromatography (SiO2, using ethyl acetate-petroleum ether mixtures as eluents. Results. The synthesis of new N-aryl-N-(3-indolmethyl acetamides based on first step iminization reaction of indol-3-carbaldehyde is accomplished. The structures of the C-3substituted indoles were confirmed by 1H-NMR and 13C-NMR studies supported by inverse-detected 2D NMR experiments and alsothrough monocrystal X-ray diffraction. Conclusions. An efficient, economic, and fast synthetic route was designed to the construction ofthe N-aryl-N-(3-indolmethyl acetamides, structural analogues of some alkaloids.

  10. High resolution NMR theory and chemical applications

    CERN Document Server

    Becker, Edwin D

    1969-01-01

    High Resolution NMR: Theory and Chemical Applications focuses on the applications of nuclear magnetic resonance (NMR), as well as chemical shifts, lattices, and couplings. The book first offers information on the theory of NMR, including nuclear spin and magnetic moment, spin lattice relaxation, line widths, saturation, quantum mechanical description of NMR, and ringing. The text then ponders on instrumentation and techniques and chemical shifts. Discussions focus on the origin of chemical shifts, reference compounds, empirical correlations of chemical shifts, modulation and phase detection,

  11. Impact of heat treatment on surface chemistry of Al-coated Eurofer for application as anti-corrosion and T-permeation barriers in a flowing Pb-15.7Li environment

    Energy Technology Data Exchange (ETDEWEB)

    Konys, J., E-mail: juergen.konys@kit.edu [Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1 76344 Eggenstein-Leopoldshafen (Germany); Krauss, W.; Holstein, N.; Lorenz, J.; Wulf, S. [Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1 76344 Eggenstein-Leopoldshafen (Germany); Bhanumurthy, K. [Scientific Information Resource Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India)

    2012-08-15

    Highlights: Black-Right-Pointing-Pointer Electro-chemical Al deposition is industrially relevant for barrier formation. Black-Right-Pointing-Pointer Al scales have to be converted into protective layers by heat treatments. Black-Right-Pointing-Pointer Morphology of scales depend on deposition parameters. Black-Right-Pointing-Pointer Solid state diffusion step at 640 Degree-Sign C avoids critical Al melting and activates steel surface. Black-Right-Pointing-Pointer Al{sub 2}O{sub 3} protective scales detected. - Abstract: The compatibility testing of Eurofer steel in flowing Pb-15.7Li has shown that corrosion attack is a serious concern at least under view of precipitate formation from dissolved steel components in cooler system sections, leading to a high risk of tube blockages. Additionally, the T-permeation from the liquid breeder through the steel structure into the He-cooling system is an important safety issue. Both topics may be reduced by the application of barriers. Hot dip aluminization (HDA) showed that Al scales exhibit such ability but claimed also the development of improved coating technologies. Thus, two electro-chemically-based deposition processes, which exhibit industrial relevance and adjustable layer thickness of deposited Al, were developed, tested and characterized. Both are working with water-free electrolytes of toluene or ionic liquid (IL) base near room temperature (RT). The successfully deposited homogeneous layers need a heat treatment to establish the required protective/functional properties. During this stage, the Al reacts with the steel and forms an Al-enriched zone with a thin protective Al{sub 2}O{sub 3} surface scale. However, the topology is rough and pores are visible. Thus, for optimization of surface structure and scale quality, investigations concerning the required heat treatment were performed including effects coming from the applied coating technology.

  12. Characterization of high-energy quasi-monoenergetic neutron energy spectra and ambient dose equivalents of 80-389 MeV 7Li(p,n) reactions using a time-of-flight method

    Science.gov (United States)

    Iwamoto, Yosuke; Hagiwara, Masayuki; Satoh, Daiki; Araki, Shouhei; Yashima, Hiroshi; Sato, Tatsuhiko; Masuda, Akihiko; Matsumoto, Tetsuro; Nakao, Noriaki; Shima, Tatsushi; Kin, Tadahiro; Watanabe, Yukinobu; Iwase, Hiroshi; Nakamura, Takashi

    2015-12-01

    We completed a series of measurements on mono-energetic neutron energy spectra of the 7Li(p,n) reaction with 80-389-MeV protons in the 100-m time-of-flight (TOF) tunnel at the Research Center for Nuclear Physics cyclotron facility. For that purpose, we measured neutron energy spectra of the 80-, 100- and 296-MeV proton incident reactions, which had not been investigated in our previous studies. The neutron peak intensity was 0.9-1.1×1010 neutrons/sr/μC in the incident proton energy region of 80-389 MeV, and it was almost independent of the incident proton energy. The contribution of peak intensity of the spectrum to the total intensity integrated with energies above 3 MeV varied between 0.38 and 0.48 in the incident proton energy range of 80-389 MeV. To consider the correction required to derive a response in the peak region from the measured total responses of neutron monitors in the 100-m TOF tunnel, we proposed the subtraction method using energy spectra between 0° and 25°. The normalizing factor k against 25° neutron fluence to equalize it to 0° neutron fluence in the continuum region ranges from 0.74 to 1.02 depending on the incident proton energy and angle measured. Even without the TOF method, the subtraction method with the k factor almost decreases the response in the continuum region of a neutron spectrum against the total response of neutron monitors.

  13. Time domain NMR applied to food products

    NARCIS (Netherlands)

    Duynhoven, van J.P.M.; Voda, A.; Witek, M.M.; As, van H.

    2010-01-01

    Time-domain NMR is being used throughout all areas of food science and technology. A wide range of one- and two-dimensional relaxometric and diffusometric applications have been implemented on cost-effective, robust and easy-to-use benchtop NMR equipment. Time-domain NMR applications do not only

  14. Molecular characterization and quantification using state of the art solid-state adiabatic TOBSY NMR in burn trauma.

    Science.gov (United States)

    Righi, Valeria; Andronesi, Ovidiu; Mintzopoulos, Dionyssios; Tzika, A Aria

    2009-12-01

    We describe a novel solid-state nuclear magnetic resonance (NMR) method that maximizes the advantages of high-resolution magic-angle-spinning (HRMAS), relative conventional liquid-state NMR approaches, when applied to intact biopsies of skeletal muscle specimens collected from burn trauma patients. This novel method, termed optimized adiabatic TOtal through Bond correlation SpectroscopY (TOBSY) solid-state NMR pulse sequence for two-dimensional (2D) 1H-1H homonuclear scalar-coupling longitudinal isotropic mixing, was demonstrated to provide a 40-60% improvement in signal-to-noise ratio (SNR) relative to its liquid-state analogue TOCSY (TOtal Correlation SpectroscopY). Using 1- and 2-dimensional HRMAS NMR experiments, we identified several metabolites in burned tissues. Quantification of metabolites in burned tissues showed increased levels of lipid compounds, intracellular metabolites (e.g., taurine and phosphocreatine) and substantially decreased water-soluble metabolites (e.g., glutathione, carnosine, glucose, glutamine/glutamate and alanine). These findings demonstrate that HRMAS NMR Spectroscopy using TOBSY is a feasible technique that reveals new insights into the pathophysiology of burn trauma. Moreover, this method has applications that facilitate the development of novel therapeutic strategies.

  15. The measurement of in situ stress using NQR/NMR

    Science.gov (United States)

    Schempp, E.; Murdoch, J. B.; Klainer, S. M.

    1982-09-01

    The measurement of stress in rocks underground is a difficult but very important problem in mining engineering and in the design of underground waste repositories. The structural stability of any excavation is critically dependent on the stress distribution in the surrounding rock and its capability to bear the stress, which can build up to hundreds of atmospheres in deep mines. Because existing methods for the determination of stress have limitations, Lawrence Berkeley Laboratory (LBL) has been investigating the use of spectroscopic techniques - nuclear quadrupole resonance (NQR) and nuclear magnetic resonance (NMR) - for rapid in situ measurements of three-dimensional stress in both salt and hard rock. Efforts in the past year have been directed toward computer simulation of boreholes stress patterns and NQR lineshapes, laboratory measurements on salt and aluminosilicates, and construction of a state-of-the-art pulsed NQR spectrometer.

  16. ELISE NMR: Experimental liquid sealing of NMR samples

    Science.gov (United States)

    Wieruszeski, Jean-Michel; Landrieu, Isabelle; Hanoulle, Xavier; Lippens, Guy

    2006-08-01

    We present a simple, generally applicable approach to prevent sample evaporation when working at elevated temperatures in high resolution NMR. It consists of experimentally sealing the NMR sample by a second liquid (Experimental Liquid Sealing, ELISE). For aqueous samples, we identified the mineral oil commonly used in PCR application as the best candidate, because it contains only a very limited amount of water-soluble contaminants, is stable over time and heat resistant. The procedure does not interfere with shim settings, and is compatible with a wide variety of samples, including oligosaccharides and proteins. For chloroform samples, a simple drop of water allows to efficiently seal the sample, avoiding solvent evaporation even over lengthy time periods.

  17. 27 Al MAS NMR Studies of HBEA Zeolite at Low to High Magnetic Fields

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Jian Zhi; Wan, Chuan; Vjunov, Aleksei; Wang, Meng; Zhao, Zhenchao; Hu, Mary Y.; Camaioni, Donald M.; Lercher, Johannes A.

    2017-06-01

    27Al single pulse (SP) MAS NMR spectra of HBEA zeolites with high Si/Al ratios of 71 and 75 were obtained at three magnetic field strengths of 7.05, 11.75 and 19.97 T. High field 27Al MAS NMR spectra acquired at 19.97 T show significantly improved spectral resolution, resulting in at least two well-resolved tetrahedral-Al NMR peaks. Based on the results obtained from 27Al MAS and MQMAS NMR acquired at 19.97 T, four different quadrupole peaks are used to deconvolute the 27Al SP MAS spectra acquired at vari-ous fields by using the same set of quadrupole coupling constants, asymmetric parameters and relative integrated peak intensities for the tetrahedral Al peaks. The line shapes of individual peaks change from typical quadrupole line shape at low field to essentially symmetrical line shapes at high field. We demonstrate that for fully hydrated HBEA zeolites the effect of second order quadrupole interaction can be ignored and quantitative spectral analysis can be performed by directly fitting the high field spectra using mixed Gaussian/Lorentzian line shapes. Also, the analytical steps described in our work allow direct assignment of spectral intensity to individual Al tetrahedral sites (T-sites) of zeolite HBEA. Finally, the proposed concept is suggested generally applicable to other zeo-lite framework types, thus, allowing a direct probing of Al distributions by NMR spectroscopic methods in zeolites with high confi-dence.

  18. 1H and 13C resonance designation of antimycin A1 by two-dimensional NMR spectroscopy

    Science.gov (United States)

    Abidi, S.L.; Adams, B.R.

    1987-01-01

    Complete 1H and 13C resonance assignments of antimycin A1 were accomplished by two-dimensional NMR techniques, viz. 1H homonuclear COSY correlation, heteronuclear 13C-1H chemical shift correlation and long-range heteronuclear 13C-1H COLOC correlation. Antimycin A1 was found to consist of two isomeric components in a 2:1 ratio based on NMR spectroscopic evidence. The structure of the major component was newly assigned as the 8-isopentanoic acid ester. The spectra of the minor component were consistent with the known structure of antimycin A1.

  19. What Is the True Color of Fresh Meat? A Biophysical Undergraduate Laboratory Experiment Investigating the Effects of Ligand Binding on Myoglobin Using Optical, EPR, and NMR Spectroscopy

    Science.gov (United States)

    Linenberger, Kimberly; Bretz, Stacey Lowery; Crowder, Michael W.; McCarrick, Robert; Lorigan, Gary A.; Tierney, David L.

    2011-01-01

    With an increased focus on integrated upper-level laboratories, we present an experiment integrating concepts from inorganic, biological, and physical chemistry content areas. Students investigate the effects of ligand strength on the spectroscopic properties of the heme center in myoglobin using UV-vis, [superscript 1]H NMR, and EPR…

  20. γ‐ and δ-Lactams through Palladium-Catalyzed Intramolecular Allylic Alkylation: Enantioselective Synthesis, NMR Investigation, and DFT Rationalization

    DEFF Research Database (Denmark)

    Bantreil, Xavier; Prestat, Guillaume; Moreno, Aitor;

    2011-01-01

    the cyclization reactions to take place in up to 94:6 enantiomeric ratio. A model Pd-allyl complex has been prepared and studied through NMR spectroscopic analysis, which provided insight into the processes responsible for the observed enantiomeric ratios. DFT studies were used to characterize the diastereomeric...

  1. What Is the True Color of Fresh Meat? A Biophysical Undergraduate Laboratory Experiment Investigating the Effects of Ligand Binding on Myoglobin Using Optical, EPR, and NMR Spectroscopy

    Science.gov (United States)

    Linenberger, Kimberly; Bretz, Stacey Lowery; Crowder, Michael W.; McCarrick, Robert; Lorigan, Gary A.; Tierney, David L.

    2011-01-01

    With an increased focus on integrated upper-level laboratories, we present an experiment integrating concepts from inorganic, biological, and physical chemistry content areas. Students investigate the effects of ligand strength on the spectroscopic properties of the heme center in myoglobin using UV-vis, [superscript 1]H NMR, and EPR…

  2. Potential of NMR Spectroscopy in the Characterization of Nonconventional Oils

    Directory of Open Access Journals (Sweden)

    Abdul Majid

    2014-01-01

    Full Text Available NMR spectroscopy was applied for the characterization of two biomass based pyrolysis oil samples. The samples were extracted in various solvents and the extracts were investigated by both 1H and 13C NMR spectroscopy. Subsequent evaluation of the integrated analytical data revealed chemical information regarding semiquantitative estimation of various functional groups. This information could not have been obtained readily from the individual spectroscopic techniques. Semiquantitative estimation of the various functional groups allowed a comparison of the extraction efficiency of these groups in various solvents. The method is based on the premise that although the number of individual molecular species in pyrolysis oil liquid is large, most of these species are composed of a limited number of functional groups. The methodology provided information on the concentration of chemical functionalities that are potentially useful for synthetic modifications and may help to guide the use of pyrolysis oil as a chemical feedstock. The approach described is expected to be generally applicable to complex mixture of hydrocarbon oils such as bio-oils, oil sands bitumen, and coal pyrolysis oils.

  3. RECENT PROGRESS IN BIOMOLECULAR NMR

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    @@ Structural genomics and proteomics were born from the understanding that functions of a protein are dictated by its 3D structure and dynamics. To understand protein functions on a genomic scale, we must know protein structures on a genomic scale. High resolution NMR can be used for this purpose. Traditional multidimensional NMR structure determination protocols become ineffective for structural genomics since to obtain a structure of a small protein of 15kD requires many months of painstaking spectral analysis and modeling. Recent advances in magnet and probe technology and in experimental methods have expanded the range of proteins amenable to structure determination and make the large scale structure determination possible. These advances are (1) effective expression systems for protein production, (2) introduction of cryoprobe, (3) structure determination with the use of the minimal amount of structural restraints obtained from the chemical shifts, residual dipolar couplings, NOEs, and computer modeling. In this talk,Iwill briefly outline these developments and related works done in our NMR lab.

  4. NMR-Based Milk Metabolomics

    Directory of Open Access Journals (Sweden)

    Hanne C. Bertram

    2013-04-01

    Full Text Available Milk is a key component in infant nutrition worldwide and, in the Western parts of the world, also in adult nutrition. Milk of bovine origin is both consumed fresh and processed into a variety of dairy products including cheese, fermented milk products, and infant formula. The nutritional quality and processing capabilities of bovine milk is closely associated to milk composition. Metabolomics is ideal in the study of the low-molecular-weight compounds in milk, and this review focuses on the recent nuclear magnetic resonance (NMR-based metabolomics trends in milk research, including applications linking the milk metabolite profiling with nutritional aspects, and applications which aim to link the milk metabolite profile to various technological qualities of milk. The metabolite profiling studies encompass the identification of novel metabolites, which potentially can be used as biomarkers or as bioactive compounds. Furthermore, metabolomics applications elucidating how the differential regulated genes affects milk composition are also reported. This review will highlight the recent advances in NMR-based metabolomics on milk, as well as give a brief summary of when NMR spectroscopy can be useful for gaining a better understanding of how milk composition is linked to nutritional or quality traits.

  5. Hyperpolarized 131Xe NMR spectroscopy

    Science.gov (United States)

    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.

  6. Spectroscopic analysis of optoelectronic semiconductors

    CERN Document Server

    Jimenez, Juan

    2016-01-01

    This book deals with standard spectroscopic techniques which can be used to analyze semiconductor samples or devices, in both, bulk, micrometer and submicrometer scale. The book aims helping experimental physicists and engineers to choose the right analytical spectroscopic technique in order to get specific information about their specific demands. For this purpose, the techniques including technical details such as apparatus and probed sample region are described. More important, also the expected outcome from experiments is provided. This involves also the link to theory, that is not subject of this book, and the link to current experimental results in the literature which are presented in a review-like style. Many special spectroscopic techniques are introduced and their relationship to the standard techniques is revealed. Thus the book works also as a type of guide or reference book for people researching in optical spectroscopy of semiconductors.

  7. A DVD Spectroscope: A Simple, High-Resolution Classroom Spectroscope

    Science.gov (United States)

    Wakabayashi, Fumitaka; Hamada, Kiyohito

    2006-01-01

    Digital versatile disks (DVDs) have successfully made up an inexpensive but high-resolution spectroscope suitable for classroom experiments that can easily be made with common material and gives clear and fine spectra of various light sources and colored material. The observed spectra can be photographed with a digital camera, and such images can…

  8. Time Domain Reflectometric and spectroscopic studies on toluene + butyronitrile solution

    Science.gov (United States)

    Karthick, N. K.; Arivazhagan, G.; Kumbharkhane, A. C.; Joshi, Y. S.; Kannan, P. P.

    2016-03-01

    The dielectric parameters of toluene + butyronitrile solution have been obtained by time domain reflectometry (TDR) technique in the frequency range from 10 MHz to 30 GHz at 298 K. Spectroscopic (FTIR and 13C NMR) studies have also been carried out on the solution and the results of the studies show that neat butyronitrile is self-associative through C-H⋯N contacts and weak intermolecular forces of C-H⋯N and C-H⋯π type are operative in the solution. The obtained dielectric parameters such as Kirkwood correlation factor g, relaxation time τ etc. have been analyzed in view of these weak intermolecular forces. The weak non-covalent interactions between heteromolecules appear to have no influence on the ideality of ɛm vs X2 curve of the solution. Heteromolecular entities with weak intermolecular forces experience larger hindrance leading to longer relaxation time τ.

  9. Dual Spectroscopic Responses of Pyridinium Hemicyanine Dyes to Anions%Dual Spectroscopic Responses of Pyridinium Hemicyanine Dyes to Anions

    Institute of Scientific and Technical Information of China (English)

    Xie, Puhui; Guo, Fengqi; Zhang, Dasheng; Zhang, Lei

    2011-01-01

    The absorption and fluorescence spectroscopic responses of three pyridinium hemicyanine dyes to anions F , Cl , Br , I-, H2P02, HS04 and OAc- were investigated. At lower concentrations of OAc- (less than 1 equiv.), both the absorption and the fluorescence intensities of 1--3 were more effectively changed than F at iden- tical concentrations. At higher concentrations of OAc (more than 1 equiv.), the interaction was opposite for each compound. 1H NMR results indicated the interaction between 1, 2 or 3 and F- proceeded through hydrogen bonding. The results showed that these dyes are promising to develop dual fluorescence and chromogenic chemo- sensors toward F- and OAc- according to the subtle difference in the affinity of F and OAc .

  10. Dynamic pulsed-field-gradient NMR

    CERN Document Server

    Sørland, Geir Humborstad

    2014-01-01

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

  11. Applications of NMR in Dairy Research

    Directory of Open Access Journals (Sweden)

    Anthony D. Maher

    2014-03-01

    Full Text Available NMR is a robust analytical technique that has been employed to investigate the properties of many substances of agricultural relevance. NMR was first used to investigate the properties of milk in the 1950s and has since been employed in a wide range of studies; including properties analysis of specific milk proteins to metabolomics techniques used to monitor the health of dairy cows. In this brief review, we highlight the different uses of NMR in the dairy industry.

  12. Fourier Analysis and Structure Determination. Part II: Pulse NMR and NMR Imaging.

    Science.gov (United States)

    Chesick, John P.

    1989-01-01

    Uses simple pulse NMR experiments to discuss Fourier transforms. Studies the generation of spin echoes used in the imaging procedure. Shows that pulse NMR experiments give signals that are additions of sinusoids of differing amplitudes, frequencies, and phases. (MVL)

  13. NMR studies of isotopically labeled RNA

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-12-01

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

  14. NMR exposure sensitizes tumor cells to apoptosis.

    Science.gov (United States)

    Ghibelli, L; Cerella, C; Cordisco, S; Clavarino, G; Marazzi, S; De Nicola, M; Nuccitelli, S; D'Alessio, M; Magrini, A; Bergamaschi, A; Guerrisi, V; Porfiri, L M

    2006-03-01

    NMR technology has dramatically contributed to the revolution of image diagnostic. NMR apparatuses use combinations of microwaves over a homogeneous strong (1 Tesla) static magnetic field. We had previously shown that low intensity (0.3-66 mT) static magnetic fields deeply affect apoptosis in a Ca2+ dependent fashion (Fanelli et al., 1999 FASEBJ., 13;95-102). The rationale of the present study is to examine whether exposure to the static magnetic fields of NMR can affect apoptosis induced on reporter tumor cells of haematopoietic origin. The impressive result was the strong increase (1.8-2.5 fold) of damage-induced apoptosis by NMR. This potentiation is due to cytosolic Ca2+ overload consequent to NMR-promoted Ca2+ influx, since it is prevented by intracellular (BAPTA-AM) and extracellular (EGTA) Ca2+ chelation or by inhibition of plasma membrane L-type Ca2+ channels. Three-days follow up of treated cultures shows that NMR decrease long term cell survival, thus increasing the efficiency of cytocidal treatments. Importantly, mononuclear white blood cells are not sensitised to apoptosis by NMR, showing that NMR may increase the differential cytotoxicity of antitumor drugs on tumor vs normal cells. This strong, differential potentiating effect of NMR on tumor cell apoptosis may have important implications, being in fact a possible adjuvant for antitumor therapies.

  15. Spin-Exchange Pumped NMR Gyros

    CERN Document Server

    Walker, Thad G

    2016-01-01

    We present the basic theory governing spin-exchange pumped NMR gyros. We review the basic physics of spin-exchange collisions and relaxation as they pertain to precision NMR. We present a simple model of operation as an NMR oscillator and use it to analyze the dynamic response and noise properties of the oscillator. We discuss the primary systematic errors (differential alkali fields, quadrupole shifts, and offset drifts) that limit the bias stability, and discuss methods to minimize them. We give with a brief overview of a practical implementation and performance of an NMR gyro built by Northrop-Grumman Corporation, and conclude with some comments about future prospects.

  16. Solid-state NMR and Membrane Proteins

    Science.gov (United States)

    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

  17. Solid state NMR and pair distribution function studies of silicon electrodes for lithium-ion batteries

    Science.gov (United States)

    Key, Baris

    The universally used negative electrode material in a LIB is carbon, because of its moderate capacity (372 mAhg-1 for graphite), cyclability and high rate capability. However, new, low cost, safe electrode materials with higher capacities are still urgently required for both portable and transportation applications. Silicon anodes are particularly attractive alternatives to carbon with extremely high gravimetric energy densities (3572 mAhg-1). Compared to graphite, silicon has a massive volumetric capacity of 8322 mAhcm-3 (calculated based on the original volume of silicon) which is approximately ten times that graphite. At room temperature, upon electrochemical lithiation, silicon undergoes a crystalline to amorphous phase transition forming a lithiated amorphous silicide phase. Unfortunately, due to the amorphous nature of the lithiated silicides, it is not possible to monitor all the structural changes that occur during lithium insertion/removal with conventional methods such as diffraction. The short range order of the amorphous materials remains unknown, preventing attempts to optimize performance based on electrochemical-structure correlations. In this work, a combination of local structure probes, ex-situ 7Li nuclear magnetic resonance (NMR) studies and pair distribution function (PDF) analysis of X-ray data was applied to investigate the changes in short range order that occur during the initial charge and discharge cycles. The distinct electrochemical profiles observed subsequent to the 1 st discharge have been shown to be associated with the formation of distinct amorphous lithiated silicide structures. A (de)lithiation model consisting of four different mechanisms, each being valid for regions of the charge or discharge process is proposed to explain the hysteresis and the steps in the electrochemical profile observed during lithiation and delithiation of Si. A spontaneous reaction of the fully lithiated lithium silicide with the electrolyte is directly

  18. Investigation of the binding of roxatidine acetate hydrochloride with cyclomaltoheptaose (β-cyclodextrin) using IR and NMR spectroscopy.

    Science.gov (United States)

    Maheshwari, Arti; Sharma, Manisha; Sharma, Deepak

    2011-09-27

    NMR chemical shift changes of the cyclomaltoheptaose (β-cyclodextrin, β-CD) cavity protons as well as roxatidine acetate hydrochloride aromatic ring protons revealed the formation of a RAH-β-CD inclusion complex. Detailed FTIR and NMR spectroscopic ((1)H NMR, COSY, NOESY, ROESY) studies have been done. The stoichiometry of the complex was determined to be 1:1, and the overall binding constant was also determined by Scott's method. The NOESY spectrum confirmed the selective penetration of the aromatic ring of RAH into the β-CD cavity in comparison to that of the piperidine ring. The mode of penetration of the guest into the CD cavity and structure of the complex has been established.

  19. Factor analysis of 27Al MAS NMR spectra for identifying nanocrystalline phases in amorphous geopolymers.

    Science.gov (United States)

    Urbanova, Martina; Kobera, Libor; Brus, Jiri

    2013-11-01

    Nanostructured materials offer enhanced physicochemical properties because of the large interfacial area. Typically, geopolymers with specifically synthesized nanosized zeolites are a promising material for the sorption of pollutants. The structural characterization of these aluminosilicates, however, continues to be a challenge. To circumvent complications resulting from the amorphous character of the aluminosilicate matrix and from the low concentrations of nanosized crystallites, we have proposed a procedure based on factor analysis of (27)Al MAS NMR spectra. The capability of the proposed method was tested on geopolymers that exhibited various tendencies to crystallize (i) completely amorphous systems, (ii) X-ray amorphous systems with nanocrystalline phases, and (iii) highly crystalline systems. Although the recorded (27)Al MAS NMR spectra did not show visible differences between the amorphous systems (i) and the geopolymers with the nanocrystalline phase (ii), the applied factor analysis unambiguously distinguished these materials. The samples were separated into the well-defined clusters, and the systems with the evolving crystalline phase were identified even before any crystalline fraction was detected by X-ray powder diffraction. Reliability of the proposed procedure was verified by comparing it with (29)Si MAS NMR spectra. Factor analysis of (27)Al MAS NMR spectra thus has the ability to reveal spectroscopic features corresponding to the nanocrystalline phases. Because the measurement time of (27)Al MAS NMR spectra is significantly shorter than that of (29)Si MAS NMR data, the proposed procedure is particularly suitable for the analysis of large sets of specifically synthesized geopolymers in which the formation of the limited fractions of nanocrystalline phases is desired. Copyright © 2013 John Wiley & Sons, Ltd.

  20. Perspectives in enzymology of membrane proteins by solid-state NMR.

    Science.gov (United States)

    Ullrich, Sandra J; Glaubitz, Clemens

    2013-09-17

    Membrane proteins catalyze reactions at the cell membrane and facilitate thetransport of molecules or signals across the membrane. Recently researchers have made great progress in understanding the structural biology of membrane proteins, mainly based on X-ray crystallography. In addition, the application of complementary spectroscopic techniques has allowed researchers to develop a functional understanding of these proteins. Solid-state NMR has become an indispensable tool for the structure-function analysis of insoluble proteins and protein complexes. It offers the possibility of investigating membrane proteins directly in their environment, which provides essential information about the intrinsic coupling of protein structure and functional dynamics within the lipid bilayer. However, to date, researchers have hardly explored the enzymology of mem-brane proteins. In this Account, we review the perspectives for investigating membrane-bound enzymes by solid-state NMR. Understanding enzyme mechanisms requires access to kinetic parameters, structural analysis of the catalytic center, knowledge of the 3D structure and methods to follow the structural dynamics of the enzyme during the catalytic cycle. In principle, solid-state NMR can address all of these issues. Researchers can characterize the enzyme kinetics by observing substrate turnover within the membrane or at the membrane interphase in a time-resolved fashion as shown for diacylglycerol kinase. Solid-state NMR has also provided a mechanistic understanding of soluble enzymes including triosephosphate isomerase (TIM) and different metal-binding proteins, which demonstrates a promising perspective also for membrane proteins. The increasing availability of high magnetic fields and the development of new experimental schemes and computational protocols have made it easier to determine 3D structure using solid-state NMR. Dynamic nuclear polarization, a key technique to boost sensitivity of solid-state NMR at low

  1. NMR-based metabonomic study on the subacute toxicity of aristolochic acid in rats.

    Science.gov (United States)

    Zhang, Xiaoyu; Wu, Huifeng; Liao, Peiqiu; Li, Xiaojing; Ni, Jiazuan; Pei, Fengkui

    2006-07-01

    The subacute toxicity of aristolochic acid (AA) was investigated by (1)H NMR spectroscopic and pattern recognition (PR)-based metabonomic methods. Model toxins were used to enable comparisons of the urinary profiles from rats treated with known toxicants and AA at various time intervals. Urinary (1)H NMR spectra were data-processed and analyzed by pattern recognition method. The result of visual comparison of the spectra showed that AA caused a renal proximal tubular and papillary lesion and a slight hepatic impair. Pattern recognition analysis indicated that the renal proximal tubule lesion was the main damage induced by AA, and the renal toxicity induced by AA was a progressive course with the accumulation of dosage by monitoring the toxicological processes from onset, development and part-recovery. These results were also supported by the conventional clinical biochemical parameters.

  2. Design and application of robust rf pulses for toroid cavity NMR spectroscopy

    CERN Document Server

    Skinner, Thomas E; Woelk, Klaus; Gershenzon, Naum I; Glaser, Steffen J

    2010-01-01

    We present robust radio frequency (rf) pulses that tolerate a factor of six inhomogeneity in the B1 field, significantly enhancing the potential of toroid cavity resonators for NMR spectroscopic applications. Both point-to-point (PP) and unitary rotation (UR) pulses were optimized for excitation, inversion, and refocusing using the gradient ascent pulse engineering (GRAPE) algorithm based on optimal control theory. In addition, the optimized parameterization (OP) algorithm applied to the adiabatic BIR-4 UR pulse scheme enabled ultra-short (50 microsec) pulses with acceptable performance compared to standard implementations. OP also discovered a new class of non-adiabatic pulse shapes with improved performance within the BIR-4 framework. However, none of the OP-BIR4 pulses are competitive with the more generally optimized UR pulses. The advantages of the new pulses are demonstrated in simulations and experiments. In particular, the DQF COSY result presented here represents the first implementation of 2D NMR sp...

  3. Gold(III)pentafluorophenylarylazoimidazole: Synthesis and spectral (H, C, COSY, HMQC NMR) characterisation

    Indian Academy of Sciences (India)

    Prithwiraj Byabartta; Mariano Laguna

    2006-09-01

    Reaction of [AuIII(C6F5)3(tht)] with RaaiR' in dichloromethane medium leads to [AuIII(C6F5)3 (RaaiR')] [RaaiR' = -R-C6H4-N=N-C3H2-NN-1-R', (1-3), R = H (a), Me (b), Cl (c) and R' = Me (1), CH2CH3 (2), CH2Ph (3), tht is tetrahydrothiophen]. The nine new complexes are characterised by ES/MS as well as FAB, IR and multinuclear NMR (1H, 13C, 19F) spectroscopic studies. In addition to dimensional NMR studies as 1H, 1H COSY and 1H 13C HMQC permit complete assignment of the complexes in the solution phase.

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

    Science.gov (United States)

    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.

  5. Access to NMR Spectroscopy for Two-Year College Students: The NMR Site at Trinity University

    Science.gov (United States)

    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…

  6. Echo-Planar Imaging-Based, J-Resolved Spectroscopic Imaging for Improved Metabolite Detection in Prostate Cancer

    Science.gov (United States)

    2015-10-01

    16 July 2015, Accepted: 17 July 2015, Published online in Wiley Online Library : 7 September 2015 (wileyonlinelibrary.com) DOI: 10.1002/nbm.3373 NMR...published online at www.rsna2014.rsna.org, Abstract LL-PHE118, 2014. Accelerated echo planar J-resolved spectroscopic imaging in prostate cancer: a...than 13 min and we were able to detect and quantify several metabolites. Copyright © 2015 John Wiley & Sons, Ltd. Keywords: MRS; prostate cancer; 4D

  7. Enzyme dynamics from NMR spectroscopy.

    Science.gov (United States)

    Palmer, Arthur G

    2015-02-17

    CONSPECTUS: Biological activities of enzymes, including regulation or coordination of mechanistic stages preceding or following the chemical step, may depend upon kinetic or equilibrium changes in protein conformations. Exchange of more open or flexible conformational states with more closed or constrained states can influence inhibition, allosteric regulation, substrate recognition, formation of the Michaelis complex, side reactions, and product release. NMR spectroscopy has long been applied to the study of conformational dynamic processes in enzymes because these phenomena can be characterized over multiple time scales with atomic site resolution. Laboratory-frame spin-relaxation measurements, sensitive to reorientational motions on picosecond-nanosecond time scales, and rotating-frame relaxation-dispersion measurements, sensitive to chemical exchange processes on microsecond-millisecond time scales, provide information on both conformational distributions and kinetics. This Account reviews NMR spin relaxation studies of the enzymes ribonuclease HI from mesophilic (Escherichia coli) and thermophilic (Thermus thermophilus) bacteria, E. coli AlkB, and Saccharomyces cerevisiae triosephosphate isomerase to illustrate the contributions of conformational flexibility and dynamics to diverse steps in enzyme mechanism. Spin relaxation measurements and molecular dynamics (MD) simulations of the bacterial ribonuclease H enzymes show that the handle region, one of three loop regions that interact with substrates, interconverts between two conformations. Comparison of these conformations with the structure of the complex between Homo sapiens ribonuclease H and a DNA:RNA substrate suggests that the more closed state is inhibitory to binding. The large population of the closed conformation in T. thermophilus ribonuclease H contributes to the increased Michaelis constant compared with the E. coli enzyme. NMR spin relaxation and fluorescence spectroscopy have characterized a

  8. NMR characterization of hydrocarbon adsorption on calcite surfaces: A first principles study

    Energy Technology Data Exchange (ETDEWEB)

    Bevilaqua, Rochele C. A.; Miranda, Caetano R. [Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, UFABC, Santo André, SP (Brazil); Rigo, Vagner A. [Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, UFABC, Santo André, SP (Brazil); Universidade Tecnológica Federal do Paraná, UTFPR, Cornélio Procópio, PR (Brazil); Veríssimo-Alves, Marcos [Centro de Ciências Naturais e Humanas, Universidade Federal do ABC, UFABC, Santo André, SP (Brazil); Departamento de Física, ICEx, Universidade Federal Fluminense, UFF, Volta Redonda, RJ (Brazil)

    2014-11-28

    The electronic and coordination environment of minerals surfaces, as calcite, are very difficult to characterize experimentally. This is mainly due to the fact that there are relatively few spectroscopic techniques able to detect Ca{sup 2+}. Since calcite is a major constituent of sedimentary rocks in oil reservoir, a more detailed characterization of the interaction between hydrocarbon molecules and mineral surfaces is highly desirable. Here we perform a first principles study on the adsorption of hydrocarbon molecules on calcite surface (CaCO{sub 3} (101{sup ¯}4)). The simulations were based on Density Functional Theory with Solid State Nuclear Magnetic Resonance (SS-NMR) calculations. The Gauge-Including Projector Augmented Wave method was used to compute mainly SS-NMR parameters for {sup 43}Ca, {sup 13}C, and {sup 17}O in calcite surface. It was possible to assign the peaks in the theoretical NMR spectra for all structures studied. Besides showing different chemical shifts for atoms located on different environments (bulk and surface) for calcite, the results also display changes on the chemical shift, mainly for Ca sites, when the hydrocarbon molecules are present. Even though the interaction of the benzene molecule with the calcite surface is weak, there is a clearly distinguishable displacement of the signal of the Ca sites over which the hydrocarbon molecule is located. A similar effect is also observed for hexane adsorption. Through NMR spectroscopy, we show that aromatic and alkane hydrocarbon molecules adsorbed on carbonate surfaces can be differentiated.

  9. Structural investigation of aluminium doped ZnO nanoparticles by solid-state NMR spectroscopy.

    Science.gov (United States)

    Avadhut, Yamini S; Weber, Johannes; Hammarberg, Elin; Feldmann, Claus; Schmedt auf der Günne, Jörn

    2012-09-07

    The electrical conductivity of aluminium doped zinc oxide (AZO, ZnO:Al) materials depends on doping induced defects and grain structure. This study aims at relating macroscopic electrical conductivity of AZO nanoparticles with their atomic structure, which is non-trivial because the derived materials are heavily disordered and heterogeneous in nature. For this purpose we synthesized AZO nanoparticles with different doping levels and narrow size distribution by a microwave assisted polyol method followed by drying and a reductive treatment with forming gas. From these particles electrically conductive, optically transparent films were obtained by spin-coating. Characterization involved energy-dispersive X-ray analysis, wet chemical analysis, X-ray diffraction, electron microscopy and dynamic light scattering, which provided a basis for a detailed structural solid-state NMR study. A multinuclear ((27)Al, (13)C, (1)H) spectroscopic investigation required a number of 1D MAS NMR and 2D MAS NMR techniques (T(1)-measurements, (27)Al-MQMAS, (27)Al-(1)H 2D-PRESTO-III heteronuclear correlation spectroscopy), which were corroborated by quantum chemical calculations with an embedded cluster method (EEIM) at the DFT level. From the combined data we conclude that only a small part of the provided Al is incorporated into the ZnO structure by substitution of Zn. The related (27)Al NMR signal undergoes a Knight shift when the material is subjected to a reductive treatment with forming gas. At higher (formal) doping levels Al forms insulating (Al, H and C containing) side-phases, which cover the surface of the ZnO:Al particles and increase the sheet resistivity of spin-coated material. Moreover, calculated (27)Al quadrupole coupling constants serve as a spectroscopic fingerprint by which previously suggested point-defects can be identified and in their great majority be ruled out.

  10. The 1997 spectroscopic GEISA databank.

    Science.gov (United States)

    Jacquinet-Husson, N.; Arie, E.; Ballard, J.; Barbe, A.; Bjoraker, G.; Bonnet, B.; Brown, L. R.; Camy-Peyret, C.; Champion, J. P.; Chedin, A.; Chursin, A.; Clerbaux, C.; Duxbury, G.; Flaud, J.-M.; Fourrie, N.; Fayt, A.; Graner, G.; Gamache, R.; Goldman, A.; Golovko, V.; Guelachvili, G.; Hartmann, J. M.; Hilico, J. C.; Hillman, J.; Lefevre, G.; Lellouch, E.; Mikhailenko, S. N.; Naumenko, O. V.; Nemtchinov, V.; Newnham, D. A.; Nikitin, A.; Orphal, J.; Perrin, A.; Reuter, D. C.; Rinsland, C. P.; Rosenmann, L.; Rothman, L. S.; Scott, N. A.; Selby, J.; Sinitsa, L. N.; Sirota, J. M.; Smith, A. M.; Smith, K. M.; Tyuterev, V. G.; Tipping, R. H.; Urban, S.; Varanasi, P.; Weber, M.

    1999-05-01

    The current version GEISA-97 of the computer-accessible database system GEISA (Gestion et Etude des Informations Spectroscopiques Atmospheriques: Management and Study of Atmospheric Spectroscopic Information) is described. This catalogue contains 1,346,266 entries. These are the spectroscopic parameters required to describe adequately the individual spectral lines belonging to 42 molecules (96 isotopic species) and located between 0 and 22656 cm-1. The featured molecules are of interest in studies of the terrestrial as well as the other planetary atmospheres, especially those of the giant planets. GEISA-97 contains also a catalog of absorption cross-sections of molecules such as chlorofluorocarbons which exhibit unresolvable spectra. The modifications and improvements made to the earlier edition (GEISA-92) and the data management software are described.

  11. Single nanoparticle tracking spectroscopic microscope

    Science.gov (United States)

    Yang, Haw [Moraga, CA; Cang, Hu [Berkeley, CA; Xu, Cangshan [Berkeley, CA; Wong, Chung M [San Gabriel, CA

    2011-07-19

    A system that can maintain and track the position of a single nanoparticle in three dimensions for a prolonged period has been disclosed. The system allows for continuously imaging the particle to observe any interactions it may have. The system also enables the acquisition of real-time sequential spectroscopic information from the particle. The apparatus holds great promise in performing single molecule spectroscopy and imaging on a non-stationary target.

  12. NMR Spectroscopy and Its Value: A Primer

    Science.gov (United States)

    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…

  13. Using Cloud Storage for NMR Data Distribution

    Science.gov (United States)

    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…

  14. Planar microcoil-based microfluidic NMR probes.

    NARCIS (Netherlands)

    Massin, C.; Vincent, F.; Homsy, A.; Ehrmann, K.; Boero, G.; Besse, P-A; Daridon, A.; Verpoorte, E.; de Rooij, N.F.; Popovic, R.S.

    2003-01-01

    Microfabricated small-volume NMR probes consisting of electroplated planar microcoils integrated on a glass substrate with etched microfluidic channels are fabricated and tested. 1H NMR spectra are acquired at 300 MHz with three different probes having observed sample volumes of respectively 30, 120

  15. Using Cloud Storage for NMR Data Distribution

    Science.gov (United States)

    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…

  16. An Inversion Recovery NMR Kinetics Experiment

    Science.gov (United States)

    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…

  17. NMR Spectroscopy and Its Value: A Primer

    Science.gov (United States)

    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…

  18. Planar microcoil-based microfluidic NMR probes.

    NARCIS (Netherlands)

    Massin, C.; Vincent, F.; Homsy, A.; Ehrmann, K.; Boero, G.; Besse, P-A; Daridon, A.; Verpoorte, E.; de Rooij, N.F.; Popovic, R.S.

    2003-01-01

    Microfabricated small-volume NMR probes consisting of electroplated planar microcoils integrated on a glass substrate with etched microfluidic channels are fabricated and tested. 1H NMR spectra are acquired at 300 MHz with three different probes having observed sample volumes of respectively 30, 120

  19. A Guided Inquiry Approach to NMR Spectroscopy

    Science.gov (United States)

    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.

  20. Multi-pass spectroscopic ellipsometry

    Energy Technology Data Exchange (ETDEWEB)

    Stehle, Jean-Louis [Sopralab, 7 rue du Moulin des Bruyeres, 92400 Courbevoie (France); Samartzis, Peter C., E-mail: sama@iesl.forth.gr [Institute of Electronic Structure and Laser, Foundation of Research and Technology-Hellas, Vassilika Vouton 71110, Heraklion Crete (Greece); Stamataki, Katerina [Institute of Electronic Structure and Laser, Foundation of Research and Technology-Hellas, Vassilika Vouton 71110, Heraklion Crete (Greece); Department of Chemistry, University of Crete, Voutes, 71003, Heraklion (Greece); Piel, Jean-Philippe [Sopralab, 7 rue du Moulin des Bruyeres, 92400 Courbevoie (France); Katsoprinakis, George E.; Papadakis, Vassilis [Institute of Electronic Structure and Laser, Foundation of Research and Technology-Hellas, Vassilika Vouton 71110, Heraklion Crete (Greece); Schimowski, Xavier [Sopralab, 7 rue du Moulin des Bruyeres, 92400 Courbevoie (France); Rakitzis, T. Peter [Institute of Electronic Structure and Laser, Foundation of Research and Technology-Hellas, Vassilika Vouton 71110, Heraklion Crete (Greece); Department of Physics, University of Crete, Voutes, 71003, Heraklion (Greece); Loppinet, Benoit [Institute of Electronic Structure and Laser, Foundation of Research and Technology-Hellas, Vassilika Vouton 71110, Heraklion Crete (Greece)

    2014-03-31

    Spectroscopic ellipsometry is an established technique, particularly useful for thickness measurements of thin films. It measures polarization rotation after a single reflection of a beam of light on the measured substrate at a given incidence angle. In this paper, we report the development of multi-pass spectroscopic ellipsometry where the light beam reflects multiple times on the sample. We have investigated both theoretically and experimentally the effect of sample reflectivity, number of reflections (passes), angles of incidence and detector dynamic range on ellipsometric observables tanΨ and cosΔ. The multiple pass approach provides increased sensitivity to small changes in Ψ and Δ, opening the way for single measurement determination of optical thickness T, refractive index n and absorption coefficient k of thin films, a significant improvement over the existing techniques. Based on our results, we discuss the strengths, the weaknesses and possible applications of this technique. - Highlights: • We present multi-pass spectroscopic ellipsometry (MPSE), a multi-pass approach to ellipsometry. • Different detectors, samples, angles of incidence and number of passes were tested. • N passes improve polarization ratio sensitivity to the power of N. • N reflections improve phase shift sensitivity by a factor of N. • MPSE can significantly improve thickness measurements in thin films.

  1. Characterization of Fen-Daqu Through Multivariate Statistical Analysis of H-1 NMR Spectroscopic Data

    NARCIS (Netherlands)

    Van-Diep, L.; Zheng, X.; Ma, K.; Chen, J.Y.; Han, B.Z.; Nout, M.J.R.

    2011-01-01

    J. Inst. Brew. 117(4), 516-522, 2011 Fen liquor is typical of Chinese light-flavour liquor (alcoholic spirit), which is fermented from sorghum with Fen-Daqu powder. Fen-Daqu is a saccharifying agent and fermentation starter in this fermentation process and in Fen traditional vinegar. To investigate

  2. Paraffin molecule mobility in channel clathrates of urea on spectroscopic NMR relaxation data

    CERN Document Server

    Kriger, Y G; Chekhova, G N

    2001-01-01

    The temperature dependences of the protons spin-lattice relaxation time (T sub I) in the channel clathrates of urea with paraffins are measured. The data on the T sub I are interpreted within the frames of the model of the paraffins molecules and their fragments orientation in the clathrate channels. The dynamics peculiarities are connected with the disproportion effects of these compounds

  3. Perturbed Angular Correlation (PAC)/NMR spectroscopic properties and dynamics of compounds containing metal ions

    DEFF Research Database (Denmark)

    Arcisauskaité, Vaida

    computationally demanding Coupled Cluster results. We also determined to what degree the computationally cheaper approximate relativistic methods ZORA(-4) and SR-ZORA-4 at the DFT level can reproduce fully-relativistic results. As a result, we proposed reliable computational methods applicable to Hg binding sites...... compounds in terms of the atomic constituents. The analysis provided a chemophysical interpretation of changes in Vzz upon structural distortions and ligand exchange. The gained insights can be useful when predicting and understanding changes in Q values for Hg binding sites in proteins. One of the first...

  4. Purification and H-1 NMR spectroscopic characterization of phase II metabolites of tolfenamic acid

    DEFF Research Database (Denmark)

    Sidelmann, U. G.; Christiansen, E.; Krogh, L.

    1997-01-01

    )-anthranilic acid (T), N-(2-hydroxymethyl-3-chlorophenyl)-anthranilic acid (1), N-(2-hydroxymethyl-3-chloro-4-hydroxyphenyl)-anthranilic acid (2), N-(2-formyl-3-chlorophenyl) anthranilic acid (3), N-(2-methyl-3-chloro-4-hydroxyphenyl)-anthranilic acid (4), N-(2-methyl-3-chloro-5-hydroxyphenyl)-anthranilic acid (5...

  5. NMR spectroscopic investigations on copper-catalyzed reactions and zintl anions

    OpenAIRE

    Koch, Carina

    2016-01-01

    The copper-catalyzed asymmetric conjugated 1,4-addition reaction of organozinc reagents to a,b-unsaturated compounds is a very effective and widely used method for the enantioselective carbon-carbon bond formation. By the use of phosphoramidite ligands it is possible to reach ee-values and conversion up to > 99 %. Furthermore, this outstanding reaction provides lower costs in comparison to other transition-metal catalyzed reactions and compatibility to many functional groups. Despite the grea...

  6. Characterization of Fen-Daqu Through Multivariate Statistical Analysis of H-1 NMR Spectroscopic Data

    NARCIS (Netherlands)

    Van-Diep, L.; Zheng, X.; Ma, K.; Chen, J.Y.; Han, B.Z.; Nout, M.J.R.

    2011-01-01

    J. Inst. Brew. 117(4), 516-522, 2011 Fen liquor is typical of Chinese light-flavour liquor (alcoholic spirit), which is fermented from sorghum with Fen-Daqu powder. Fen-Daqu is a saccharifying agent and fermentation starter in this fermentation process and in Fen traditional vinegar. To investigate

  7. NMR spectroscopic and analytical ultracentrifuge analysis of membrane protein detergent complexes

    OpenAIRE

    Choe Senyon; Riek Roland; Johnson Casey; Kefala Georgia; Maslennikov Innokentiy; Kwiatkowski Witek

    2007-01-01

    Abstract Background Structural studies of integral membrane proteins (IMPs) are hampered by inherent difficulties in their heterologous expression and in the purification of solubilized protein-detergent complexes (PDCs). The choice and concentrations of detergents used in an IMP preparation play a critical role in protein homogeneity and are thus important for successful crystallization. Results Seeking an effective and standardized means applicable to genomic approaches for the characteriza...

  8. Conformational study of acyclic alcohols by NMR spectroscopic analysis, molecular force field and Ab initio calculations

    Energy Technology Data Exchange (ETDEWEB)

    Abe, K.; Ito, K.; Suezawa, H.; Hirota, M.; Nishio, M.

    1986-10-01

    Conformations of a series of acyclic alcohols (CH/sub 3/CH(R)CH(OH)CH/sub 3/, CH/sub 3/CH(R)CH(OH)CH(R')CH/sub 3/, and CH/sub 3/CH(R)CH(OH)Bu/sup t/) were studied (1) by measuring vicinal H-H coupling constants (/sup 3/JH-H), (2) by lanthanoid-induced shift (LIS) analysis, (3) by molecular mechanics calculations (MM2), and (4) by ab initio (STO-3G, 4-31G geometry optimization) calculations. In the case of conformationally flexible alcohols as exemplified by 2-butanol and 3-pentanol, population of conformers determined by the LIS method do not agree with those determined by the /sup 3/JH-H, MM2, and ab initio methods. The discrepancy comes from the fact that the LIS measurement gives the most stable conformation of the alcohol in the LSR-alcohol complex and not of the free alcohol. In some flexible molecules, the most stable conformer in the complex can be different from that of the free molecule. In general, the conformational equilibrium is shifted by coordination of the shift reagent to the conformer whose alkyl chain stretches opposite to the direction of the coordination site of the shift reagent. 21 references, 1 figure, 6 tables.

  9. Challenges and perspectives in quantitative NMR.

    Science.gov (United States)

    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. Copyright © 2016 John Wiley & Sons, Ltd.

  10. NMR and MRI apparatus and method

    Science.gov (United States)

    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.

  11. Carbon-13 NMR spectroscopy of biological systems

    CERN Document Server

    Beckmann, Nicolau

    1995-01-01

    This book is intended to provide an in-depth understanding of 13C NMR as a tool in biological research. 13C NMR has provided unique information concerning complex biological systems, from proteins and nucleic acids to animals and humans. The subjects addressed include multidimensional heteronuclear techniques for structural studies of molecules in the liquid and solid states, the investigation of interactions in model membranes, the elucidation of metabolic pathwaysin vitro and in vivo on animals, and noninvasive metabolic studies performed on humans. The book is a unique mix of NMR methods and biological applications which makes it a convenient reference for those interested in research in this interdisciplinary area of physics, chemistry, biology, and medicine.Key Features* An interdisciplinary text with emphasis on both 13C NMR methodology and the relevant biological and biomedical issues* State-of-the-art 13C NMR techniques are described; Whenever possible, their advantages over other approaches are empha...

  12. Robust, integrated computational control of NMR experiments to achieve optimal assignment by ADAPT-NMR.

    Science.gov (United States)

    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.

  13. Robust, integrated computational control of NMR experiments to achieve optimal assignment by ADAPT-NMR.

    Directory of Open Access Journals (Sweden)

    Arash Bahrami

    Full Text Available 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.

  14. NMR-based milk metabolomics

    DEFF Research Database (Denmark)

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

    2013-01-01

    Milk is a key component in infant nutrition worldwide and, in the Western parts of the world, also in adult nutrition. Milk of bovine origin is both consumed fresh and processed into a variety of dairy products including cheese, fermented milk products, and infant formula. The nutritional quality...... and processing capabilities of bovine milk is closely associated to milk composition. Metabolomics is ideal in the study of the low-molecular-weight compounds in milk, and this review focuses on the recent nuclear magnetic resonance (NMR)-based metabolomics trends in milk research, including applications linking...... the milk metabolite profiling with nutritional aspects, and applications which aim to link the milk metabolite profile to various technological qualities of milk. The metabolite profiling studies encompass the identification of novel metabolites, which potentially can be used as biomarkers or as bioactive...

  15. Preprocessing of NMR metabolomics data.

    Science.gov (United States)

    Euceda, Leslie R; Giskeødegård, Guro F; Bathen, Tone F

    2015-05-01

    Metabolomics involves the large scale analysis of metabolites and thus, provides information regarding cellular processes in a biological sample. Independently of the analytical technique used, a vast amount of data is always acquired when carrying out metabolomics studies; this results in complex datasets with large amounts of variables. This type of data requires multivariate statistical analysis for its proper biological interpretation. Prior to multivariate analysis, preprocessing of the data must be carried out to remove unwanted variation such as instrumental or experimental artifacts. This review aims to outline the steps in the preprocessing of NMR metabolomics data and describe some of the methods to perform these. Since using different preprocessing methods may produce different results, it is important that an appropriate pipeline exists for the selection of the optimal combination of methods in the preprocessing workflow.

  16. NMR Hyperpolarization Techniques of Gases.

    Science.gov (United States)

    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.

  17. Applications of NMR spectroscopy to systems biochemistry.

    Science.gov (United States)

    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.

  18. Synthesis, GC-EIMS, ~1H NMR, ~(13)C NMR, Mechanistic and Thermal Studies of o-Xylylene-α,α'-bis(triphenylphosphinebromide)

    Institute of Scientific and Technical Information of China (English)

    Muddasir Hanif; LU Ping; XU Hai; TIAN Zhi-cheng; YANG Bing; WANG Zhi-ming; TIAN Lei-lei; XU Yuan-ze; XIE Zeng-qi; MA Yu-guang

    2009-01-01

    Organophosphorous compounds containing phosphorus as an integral part have been widely used in industry, organic synthesis and optoelectronics. o-Xylylene-α,α'-bis(triphenylphosphinebromide)(OXBTPPB) is a facile reagent to convert o-quinones(e.g., 9,10-phenanthrenequinone) into polycyclic aromatic hydrocarbons(PAHs). Herein lies an improved synthetic route to OXBTPPB. The resultant was carefully characterized with GC-EIMS, ~1H NMR, ~(13)C NMR, spectroscopic techniques. The EIMS shows characteristic peaks at m/z=262.4, 183.3, 108.2, 77.1 attributed to the [C_(18)H_(15)P]~+, [C_(18)H_8P]~+, [C_6H_5P]~+, [C_6H_5]~+ ions, respectively. The 1H and ~(13)C NMR spectrum shows well resolved peaks and all the hydrogens and carbons were well-assigned via a combined study of ~1H-~1H COSY, HMBC, and HMQC experiments. The mechanism for the formation of OXBTPPB was proposed based on literature and obtained experimental data. Meanwhile, the thermal stability of OXBTPPB was evaluated with TGA analysis, and an onset decomposition temperature(T_d) was recorded at 323.6℃.

  19. Spectroscopic study and structure of ( E)-2-[(2-chlorobenzylimino)methyl]methoxyphenol

    Science.gov (United States)

    Ünver, Hüseyin; Yıldız, Mustafa; Özay, Hava; Durlu, Tahsin Nuri

    2009-12-01

    ( E)-2-[(2-Chlorobenzylimino)methyl]methoxyphenol has been synthesized from the reaction of 2-hydroxy-3-methoxy-1-benzaldehyde( o-vanillin) with 2-chlorobenzylamine. The title compound has been characterized by using elemental analysis, FT-IR, 1H NMR, 13C NMR and UV-vis spectroscopic techniques. The crystal structure of the title compound has also been examined cyrstallographically. It crystallizes in the orthorhombic space group Pbca with unit cell parameters: a = 7.208(1) Å, b = 13.726(2) Å, c = 27.858(4) Å, V = 2756.0(1) Å 3, Dc = 1.18 g cm -3 and Z = 8. The crystal structure was solved by direct methods and refined by full-matrix least squares to a find R = 0.046 for 2773 observed reflections.

  20. Thermomorphic phase separation in ionic liquid-organic liquid systems--conductivity and spectroscopic characterization.

    Science.gov (United States)

    Riisager, Anders; Fehrmann, Rasmus; Berg, Rolf W; van Hal, Roy; Wasserscheid, Peter

    2005-08-21

    Electrical conductivity, FT-Raman and NMR measurements are demonstrated as useful tools to probe and determine phase behavior of thermomorphic ionic liquid-organic liquid systems. To illustrate the methods, consecutive conductivity measurements of a thermomorphic methoxyethoxyethyl-imidazolium ionic liquid/1-hexanol system are performed in the temperature interval 25-80 degrees C using a specially constructed double-electrode cell. In addition, FT-Raman and 1H-NMR spectroscopic studies performed on the phase-separable system in the same temperature interval confirm the mutual solubility of the components in the system, the liquid-liquid equilibrium phase diagram of the binary mixture, and signify the importance of hydrogen bonding between the ionic liquid and the hydroxyl group of the alcohol.

  1. Spectroscopic and Crystal Field Consequences of Fluoride Binding by [Yb⋅DTMA]3+ in Aqueous Solution

    Science.gov (United States)

    Blackburn, Octavia A; Chilton, Nicholas F; Keller, Katharina; Tait, Claudia E; Myers, William K; McInnes, Eric J L; Kenwright, Alan M; Beer, Paul D; Timmel, Christiane R; Faulkner, Stephen

    2015-01-01

    Yb⋅DTMA forms a ternary complex with fluoride in aqueous solution by displacement of a bound solvent molecule from the lanthanide ion. [Yb⋅DTMA⋅F]2+ and [Yb⋅DTMA⋅OH2]3+ are in slow exchange on the relevant NMR timescale (<2000 s−1), and profound differences are observed in their respective NMR and EPR spectra of these species. The observed differences can be explained by drastic modification of the ligand field states due to the fluoride binding. This changes the magnetic anisotropy of the YbIII ground state from easy-axis to easy-plane type, and this change is easily detected in the observed magnetic anisotropy despite thermal population of more than just the ground state. The spectroscopic consequences of such drastic changes to the ligand field represent important new opportunities in developing fluoride-responsive complexes and contrast agents. PMID:26223970

  2. Efficient ultrasound-assisted synthesis, spectroscopic, crystallographic and biological investigations of pyrazole-appended quinolinyl chalcones

    Science.gov (United States)

    Prasath, R.; Bhavana, P.; Sarveswari, S.; Ng, Seik Weng; Tiekink, Edward R. T.

    2015-02-01

    Two series of new quinolinyl chalcones containing a pyrazole group, 3a-f and 4a-r, have been synthesized by Claisen-Schmidt condensation of the derivatives of 2-methyl-3-acetylquinoline with either substituted 1,3-diphenyl-1H-pyrazole-4-carbaldehyde or 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carbaldehyde in 76-93% yield under ultrasonic method. The compounds were characterized using IR, 1H NMR and ESI-MS spectroscopic methods and, for representative compounds, by X-ray crystallography. An E-configuration about the Cdbnd C ethylene bond has been established via 1H NMR spectroscopy and X-ray crystallography. These compounds show promising anti-microbial properties, with 4a and 3e being the most potent against bacterial and fungal strains, respectively and the methoxy substituted compounds showed moderate anti-oxidant activity.

  3. Spectroscopic studies of the interactions between β-lactoglobulin and bovine submaxillary mucin

    DEFF Research Database (Denmark)

    Celebioglu, Hilal Yilmaz; Guðjónsdóttir, María; Meier, Sebastian

    2015-01-01

    The structural changes occurring during the interaction between β-lactoglobulin (BLG), the major whey protein, and bovine submaxillary mucin (BSM), a major salivary protein, were studied using high and low field Nuclear Magnetic Resonance (NMR), Dynamic Light Scattering (DLS), and Circular...... Dichroism (CD) spectroscopy. The zeta potentials of the proteins were also measured to provide information on the role of electrostatic forces in the interaction. The ratio between BLG and BSM was 1:1, and pH was adjusted to 3.0, 5.0 and 7.4 at room temperature. These spectroscopic results suggested...... between the two proteins can thus be concluded to be mostly of hydrophilic origin. Moreover, low field NMR measurements showed a decrease in transverse relaxation times in the mixture compared to the pure BLG and buffer solutions. This is possibly connected to fewer hydrophilic binding sites available...

  4. 13C Solid State Nuclear Magnetic Resonance and µ-Raman Spectroscopic Characterization of Sicilian Amber.

    Science.gov (United States)

    Barone, Germana; Capitani, Donatella; Mazzoleni, Paolo; Proietti, Noemi; Raneri, Simona; Longobardo, Ugo; Di Tullio, Valeria

    2016-08-01

    (13)C cross-polarization magic angle spinning (CPMAS) nuclear magnetic resonance (NMR) and µ-Raman spectroscopy were applied to characterize Sicilian amber samples. The main goal of this work was to supply a complete study of simetite, highlighting discriminating criteria useful to distinguish Sicilian amber from fossil resins from other regions and laying the foundations for building a spectroscopic database of Sicilian amber. With this aim, a private collection of unrefined simetite samples and fossil resins from the Baltic region and Dominican Republic was analyzed. Overall, the obtained spectra permitted simetite to be distinguished from the other resins. In addition, principal component analysis (PCA) was applied to the spectroscopic data, allowing the clustering of simetite samples with respect to the Baltic and Dominican samples and to group the simetite samples in two sets, depending on their maturity. Finally, the analysis of loadings allowed for a better understanding of the spectral features that mainly influenced the discriminating characteristics of the investigated ambers.

  5. REDOR NMR of stable-isotope-labeled protein binding sites

    Energy Technology Data Exchange (ETDEWEB)

    Schaefer, J. [Washington Univ., St. Louis, MO (United States)

    1994-12-01

    Rotational-echo, double resonance (REDOR) NMR, a new analytical spectroscopic technique for solids spinning at the magic angle, has been developed over the last 5 years. REDOR provides a direct measure of heteronuclear dipolar coupling between isolated pairs of labeled nuclei. In a solid with a {sup 13}C-{sup 15}N labeled pair, for example, the {sup 13}C rotational echoes that form each rotor period following a{sup 1}H-{sup 13}C cross-polarization transfer can be prevented from reaching full intensity by insertion of a {sup 15}N {pi} pulse each half rotor period. The REDOR difference (the difference between a {sup 13}C NMR spectrum obtained under these conditions and one obtained with no {sup 15}N {pi} pulses) has a strong dependence on the {sup 13}C-{sup 15}N dipolar coupling, and hence, the {sup 13}C-{sup 15}N internuclear distance. REDOR is described as double-resonance even though three radio frequencies (typically {sup 1}H, {sup 13}C, and {sup 15}N) are used because the protons are removed from the important evolution part of the experiment by resonant decoupling. The dephasing of magnetization in REDOR arises from a local dipolar {sup 13}C-{sup 15}N field gradient and involves no polarization transfer. REDOR has no dependence on {sup 13}C or {sup 15}N chemical-shift tensors and does not require resolution of a {sup 13}C-{sup 15}N coupling in the chemical-shift dimension.

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

    Directory of Open Access Journals (Sweden)

    E. Finessi

    2012-01-01

    terpenes photo-oxidation. The second NMR factor associated with western air masses was linked to biogenic marine sources, and was enriched in low-molecular weight aliphatic amines. Such findings provide evidence of at least two independent sources originating biogenic organic aerosols in Hyytiälä by oxidation and condensation mechanisms: reactive terpenes emitted by the boreal forest and compounds of marine origin, with the latter relatively more important when predominantly polar air masses reach the site.

    This study is an example of how spectroscopic techniques, such as proton NMR, can add functional group specificity for certain chemical features (like aromatics of OA with respect to AMS. They can therefore be profitably exploited to complement aerosol mass spectrometric measurements in organic source apportionment studies.

  7. Facile synthesis and spectroscopic elucidation of 4,11-bis(dehydroxy)-bipolaroamide

    Science.gov (United States)

    Jainta, Manuel; Nieger, Martin; Bräse, Stefan

    2009-03-01

    A new diketopiperazine was formed by facile condensation of the artificial 2-indoline carboxylic acid. This highly crystalline compound was characterized by NMR-spectroscopy as well as X-ray crystallography. Spectroscopic data of the new pentacyclic diketopiperazine revealed further evidence that the phosphite-promoted coupling used is free of racemization or inversion. These stereochemical results are important for this advanced reaction and may lead to a key step in the total synthesis of many natural products. The dimerized 2-indoline carboxylic acid described herein was chosen to be a model system for structure and reaction studies on route to the favored rostratines.

  8. Chemical and spectroscopic characterization of a vegetable oil used as dielectric coolant in distribution transformers

    Energy Technology Data Exchange (ETDEWEB)

    Gomez, Neffer A.; Abonia, Rodrigo, E-mail: rodrigo.abonia@correounivalle.edu.co [Departamento de Quimica, Escuela de Ingenieria Electrica, Universidad del Valle, Cali (Colombia); Cadavid, Hector [Grupo GRALTA, Escuela de Ingenieria Electrica, Universidad del Valle, Cali (Colombia); Vargas, Ines H. [Area de Ingenieria de Distribucion, Empresas Publicas de Medellin (EPM), Medellin (Colombia)

    2011-09-15

    In this work, a complete UV-Vis, IR and (1H, 13C and DEPT) NMR spectroscopic analysis was performed for a FR3 vegetable oil sample used as dielectric coolant in an experimental distribution transformer. The same spectroscopic analysis was performed for three used FR3 oil samples (i.e., 4 months in use, 8 months in use and 7 years in use), removed from several operating distribution transformers. Comparison of the data indicated that no significant spectroscopic changes, and hence, no structural changes occurred to the oils by the use. Chemical transformations like catalytic hydrogenation (hardening) and hydrolysis were performed to the FR3 oil sample and the obtained products were analyzed by spectroscopic methods in order to collect further structural information about the FR3 oil. Accelerated aging tests in laboratory were also performed for three FR3 oil samples affording interesting information about the structure of the degradation products. These findings would be valuable to search for a spectroscopy-based technique for monitoring the lifetime and performance of this insulating vegetable oil. (author)

  9. Structural Dynamics and Conformational Equilibria of SERCA Regulatory Proteins in Membranes by Solid-State NMR Restrained Simulations

    Science.gov (United States)

    De Simone, Alfonso; Mote, Kaustubh R.; Veglia, Gianluigi

    2014-01-01

    Solid-state NMR spectroscopy is emerging as a powerful approach to determine structure, topology, and conformational dynamics of membrane proteins at the atomic level. Conformational dynamics are often inferred and quantified from the motional averaging of the NMR parameters. However, the nature of these motions is difficult to envision based only on spectroscopic data. Here, we utilized restrained molecular dynamics simulations to probe the structural dynamics, topology and conformational transitions of regulatory membrane proteins of the calcium ATPase SERCA, namely sarcolipin and phospholamban, in explicit lipid bilayers. Specifically, we employed oriented solid-state NMR data, such as dipolar couplings and chemical shift anisotropy measured in lipid bicelles, to refine the conformational ensemble of these proteins in lipid membranes. The samplings accurately reproduced the orientations of transmembrane helices and showed a significant degree of convergence with all of the NMR parameters. Unlike the unrestrained simulations, the resulting sarcolipin structures are in agreement with distances and angles for hydrogen bonds in ideal helices. In the case of phospholamban, the restrained ensemble sampled the conformational interconversion between T (helical) and R (unfolded) states for the cytoplasmic region that could not be observed using standard structural refinements with the same experimental data set. This study underscores the importance of implementing NMR data in molecular dynamics protocols to better describe the conformational landscapes of membrane proteins embedded in realistic lipid membranes. PMID:24940774

  10. Bacterial spore detection and analysis using hyperpolarized (129)Xe chemical exchange saturation transfer (Hyper-CEST) NMR.

    Science.gov (United States)

    Bai, Yubin; Wang, Yanfei; Goulian, Mark; Driks, Adam; Dmochowski, Ivan J

    2014-08-01

    Previously, we reported hyperpolarized (129)Xe chemical exchange saturation transfer (Hyper-CEST) NMR techniques for the ultrasensitive (i.e., 1 picomolar) detection of xenon host molecules known as cryptophane. Here, we demonstrate a more general role for Hyper-CEST NMR as a spectroscopic method for probing nanoporous structures, without the requirement for cryptophane or engineered xenon-binding sites. Hyper-CEST (129)Xe NMR spectroscopy was employed to detect Bacillus anthracis and Bacillus subtilis spores in solution, and interrogate the layers that comprise their structures. (129)Xe-spore samples were selectively irradiated with radiofrequency pulses; the depolarized (129)Xe returned to aqueous solution and depleted the (129)Xe-water signal, providing measurable contrast. Removal of the outermost spore layers in B. anthracis and B. subtilis (the exosporium and coat, respectively) enhanced (129)Xe exchange with the spore interior. Notably, the spores were invisible to hyperpolarized (129)Xe NMR direct detection methods, highlighting the lack of high-affinity xenon-binding sites, and the potential for extending Hyper-CEST NMR structural analysis to other biological and synthetic nanoporous structures.

  11. An introduction to biological NMR spectroscopy.

    Science.gov (United States)

    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).

  12. 15N and 1H Solid-State NMR Investigation of a Canonical Low-Barrier Hydrogen-Bond Compound: 1,8-bis(dimethylamino) naphthalene

    OpenAIRE

    White, Paul B.; Hong, Mei

    2015-01-01

    Strong or low-barrier hydrogen bonds have been often proposed in proteins to explain enzyme catalysis and proton transfer reactions. So far 1H chemical shifts and scalar couplings have been used as the main NMR spectroscopic signatures for strong H-bonds. In this work, we report simultaneous measurements of 15N and 1H chemical shifts and N-H bond lengths by solid-state NMR in 15N-labeled 1,8-bis(dimethylamino) naphthalene (DMAN), which contains a well known strong NHN H-bond. We complexed DMA...

  13. Discovery of new natural products by application of X-hitting, a novel algorithm for automated comparison of full UV-spectra, combined with structural determination by NMR spectroscophy

    DEFF Research Database (Denmark)

    Larsen, Thomas Ostenfeld; Petersen, Bent O.; Duus, Jens Øllgaard;

    2005-01-01

    X-hitting, a newly developed algorithm for automated comparison of UV data, has been used for the tracking of two novel spiro-quinazoline metabolites, lapatins A (1)andB(2), in a screening study targeting quinazolines. The structures of 1 and 2 were elucidated by analysis of spectroscopic data, p......, primarily 2D NMR....

  14. MAS NMR of HIV-1 protein assemblies

    Science.gov (United States)

    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.

  15. Scalar operators in solid-state NMR

    Energy Technology Data Exchange (ETDEWEB)

    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.

  16. NMR reaction monitoring in flow synthesis

    Directory of Open Access Journals (Sweden)

    M. Victoria Gomez

    2017-02-01

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

  17. Oriented solid-state NMR spectrosocpy

    DEFF Research Database (Denmark)

    Bertelsen, Kresten

    This thesis is concerned with driving forward oriented solid-state NMR spectroscopy as a viable technique for studying peptides in membrane bilayers. I will show that structural heterogeneity is an intrinsic part of the peptide/lipid system and that NMR can be used to characterize static...... and dynamic structural features of the peptides and its local surroundings. In fact one need to take into account the dynamical features of the system in order to correctly predict the structure from oriented solid-state NMR spectra.      ...

  18. Graphical programming for pulse automated NMR experiments

    Energy Technology Data Exchange (ETDEWEB)

    Belmonte, S.B. [Universidade do Estado, Rio de Janeiro, RJ (Brazil); Oliveira, I.S.; Guimaraes, A.P. [Centro Brasileiro de Pesquisas Fisicas (CBPF), Rio de Janeiro, RJ (Brazil)

    1999-01-01

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

  19. Spectroscopic properties of chlorophyll f.

    Science.gov (United States)

    Li, Yaqiong; Cai, Zheng-Li; Chen, Min

    2013-09-26

    The absorption and fluorescence spectra of chlorophyll f (newly discovered in 2010) have been measured in acetone and methanol at different temperatures. The spectral analysis and assignment are compared with the spectra of chlorophyll a and d under the same experimental conditions. The spectroscopic properties of these chlorophylls have further been studied by the aid of density functional CAM-B3LYP and high-level symmetric adapted coupled-cluster configuration interaction calculations. The main Q and Soret bands and possible sidebands of chlorophylls have been determined. The photophysical properties of chlorophyll f are discussed.

  20. Isovector giant resonances in sup 6 He, sup 1 sup 2 B, sup 9 sup 0 Y, sup 1 sup 2 sup 0 In, and sup 2 sup 0 sup 8 Tl observed in the ( sup 7 Li, sup 7 Be) charge-exchange reaction

    CERN Document Server

    Annakkage, T; Winfield, J S; Berg, G P A; Brown, J A; Crawley, G; Danczyk, S; Fujiwara, M; Mercer, D J; Pham, K; Roberts, D A; Stasko, J T; Yoo, G H

    1999-01-01

    The ( sup 7 Li, sup 7 Be) and ( sup 7 Li, sup 7 Be gamma) reactions have been studied at bombarding energies of 50 A MeV on targets of sup 6 Li, sup 1 sup 2 C, sup 9 sup 0 Zr, sup 1 sup 2 sup 0 Sn, sup 2 sup 0 sup 8 Pb, and polystyrene. The detection of Doppler-shifted gamma-rays from excited sup 7 Be permits the identification of the spinflip and non-spinflip characteristics. Transitions to over 20 discrete states and resonances have been observed. Angular distributions for sup 6 Li and sup 1 sup 2 C are well described by microscopic one-step distorted-waves calculations with shell-model transition amplitudes. The transitions to the ground states of sup 6 He and sup 1 sup 2 C exhibit significant Gamow-Teller strength, but approx 7% and approx 17%, respectively, of the calculated cross sections at theta approx 0 deg. arise from the tensor interaction. A broad resonance at approx 5.6 MeV in the halo nucleus sup 6 He with J suppi = (2 sup + , 1 sup - , 0 sup +) seems to correspond to a structure predicted at th...