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Sample records for 7li nmr spectroscopic

  1. 7Li NMR studies of lithium transport in human erythrocytes

    Lithium transport in human erythrocytes was investigated by 7Li NMR spectroscopy. The intra- and extracellular pools of Li+ were distinguished by the addition to the red cell suspension of a cell-impermeable shift reagent, dysprosium(III) triphosphate. It was found that, for therapeutic levels of lithium used in the US (where the typical plasma (Li+) concentration range is 0.5-1.2 mM), a shift reagent concentration of 3 mM is sufficient to achieve clear chemical shift separation between the two 7Li+ NMR resonances. Despite competition between Li+ and other mono- and divalent cations for the shift reagent, the intra and extracellular 7Li+ NMR signals are clearly separated (approximately 3 ppM) even in the presence of physiologically relevant concentrations of Na+, K+, Mg2+, and Ca2+. Addition of an ionophore, monesin, to a K+-only RBC (red blood cell) suspension induces passive Li+ transport, which can be monitored by following the relative intensities of the two 7Li+ resonances. It is concluded that the 7Li NMR method is suitable for the noninvasive study of Li+ transport in human erythrocytes and that it shows great promise as a tool for the investigation of the bioinorganic chemistry of lithium. 24 references, 3 figures, 1 table

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

    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.

  3. A 7Li and 27Al NMR study of interaction of lithium hydride with aluminium

    Lithium hydride interaction with metal aluminium is studied using 7Li and 27Al NMR method within 100-700 deg C temperature interval. It is detected, that at temperatures exceeding 420 deg C a number of α', α'', β, γ, δ and δ' phases based on intermetallic LiAl9, LiAl3, LiAl, Li3Al2 and Li9Al4 compounds (IC) are produced in LiH-Al system, their concentrations and rates of production being dependent on the molar ratio of initial components r =[LiH]:[Al]. Production of a stable αphase of [Al] and two methastable α' and α''-phases based on LiAl3 and LiAl9, which are decayed at 530 deg C, is detected under minor molar lithium content. Values of 7Li and 27Al NMR shifts in IC are determined. (author)

  4. Host-guest interactions in fluorinated polymer electrolytes: A 7Li-13C NMR study

    Mustarelli, P.; Quartarone, E.; Capiglia, C.; Tomasi, C.; Ferloni, P.; Magistris, A.

    1999-08-01

    Gel-type electrolytes based on fluorinated polymers are of interest for electrochemical devices. We present a 7Li-13C solid-state NMR and modulated differential scanning calorimetry (MDSC) study of gel electrolytes based on a copolymer poly(vinylidene fluoride) (PVdF)-hexafluoropropylene (HFP) activated with a nonaqueous solution ethylene carbonate (EC)-propylene carbonate (PC)-LiN(CF3SO2)2. We show that the narrowing of the Li lineshape is decoupled from the glass transition. The behavior of the longitudinal relaxation times, T1, confirms that the host polymer matrix simply behaves like a quasiinert cage for the solution. These results are confirmed by 13C NMR at the magic angle (MAS) data, which show that the presence of the polymer does not significantly affect the chemical shift changes induced in the EC/PC carbons by the imide salt.

  5. Investigations of Li-containing SiCN(O) ceramics via 7Li MAS NMR.

    Gumann, Sina; Nestle, Nikolaus; Liebau-Kunzmann, Verena; Riedel, Ralf

    2007-04-01

    Lithium-containing silicon (oxy)carbonitride ceramics (SiCN(O):Li) were synthesized via precursor-to-ceramic-transformation of Li-containing (poly)silazanes. The precursors were obtained by lithiation of 2,4,6-trimethyl-2,4,6-trivinylcyclotrisilazane with n-butyllithium and by reaction of a commercial poly(organosilazane) VL20 with metallic lithium. The annealing treatment was carried out at temperatures between 200 and 1400 degrees C in argon (DeltaT=200 degrees C) and yielded Li-containing silicon (oxy)carbonitride. X-ray powder diffraction revealed that the resulting SiCN(O):Li ceramics were basically amorphous up to temperatures of 1000 degrees C and formed LiSi(2)N(3), graphite and silicon carbide as crystalline phases at higher temperatures. (7)Li MAS NMR spectroscopy was carried out to investigate the structure of the Li-containing phases and to study the reaction path of metallic Li with polysilazane. Based on the NMR spectra, there is almost no difference found in the chemical shift of the SiCN(O):Li ceramics obtained at different temperatures. Accordingly, Li is assigned to be mainly coordinated to N and O present as contaminant element. Relaxation time measurements showed that the most mobile Li(+) species seems to be present in the product obtained in the pyrolysis temperature range between 600 and 1000 degrees C. PMID:17418540

  6. Localization of vacancies and mobility of lithium ions in Li{sub 2}ZrO{sub 3} as obtained by {sup 6,7}Li NMR

    Baklanova, Ya. V., E-mail: baklanovay@ihim.uran.ru [Institute of Solid State Chemistry, Ural Branch of the Russian Academy of Sciences, 91 Pervomaiskaya str., 620990 Ekaterinburg (Russian Federation); Arapova, I. Yu.; Buzlukov, A.L.; Gerashenko, A.P.; Verkhovskii, S.V.; Mikhalev, K.N. [Institute of Metal Physics, Ural Branch of the Russian Academy of Sciences, 18 Kovalevskaya str., 620990 Ekaterinburg (Russian Federation); Denisova, T.A.; Shein, I.R.; Maksimova, L.G. [Institute of Solid State Chemistry, Ural Branch of the Russian Academy of Sciences, 91 Pervomaiskaya str., 620990 Ekaterinburg (Russian Federation)

    2013-12-15

    The {sup 6,7}Li NMR spectra and the {sup 7}Li spin–lattice relaxation rate were measured on polycrystalline samples of Li{sub 2}ZrO{sub 3}, synthesized at 1050 K and 1300 K. The {sup 7}Li NMR lines were attributed to corresponding structural positions of lithium Li1 and Li2 by comparing the EFG components with those obtained in the first-principles calculations of the charge density in Li{sub 2}ZrO{sub 3}. For both samples the line width of the central {sup 7}Li transition and the spin–lattice relaxation time decrease abruptly at the temperature increasing above ∼500 K, whereas the EFG parameters are averaged (〈ν{sub Q}〉=42 (5) kHz) owing to thermally activated diffusion of lithium ions. - Graphical abstract: Path of lithium ion hopping in lithium zirconate Li{sub 2}ZrO{sub 3}. - Highlights: • Polycrystalline samples Li{sub 2}ZrO{sub 3} with monoclinic crystal structure synthesized at different temperatures were investigated by {sup 6,7}Li NMR spectroscopy. • Two {sup 6,7}Li NMR lines were attributed to the specific structural positions Li1 and Li2. • The distribution of vacancies was clarified for both lithium sites. • The activation energy and pathways of lithium diffusion in Li{sub 2}ZrO{sub 3} were defined.

  7. Structural nature of 7Li and 11B sites in the nonlinear optical material LiB3O5 using static NMR and MAS NMR

    The structural nature of the nonlinear optical properties of LiB3O5 is analyzed using single-crystal nuclear magnetic resonance (NMR) and magic angle spinning (MAS) NMR. The 3-coordinated trigonal [B(1) and B(2)] and 4-coordinated tetragonal [B(3)] sites are distinguished using the spectrum and the spin-lattice relaxation time in rotating frame T1ρ, which was obtained from the 11B MAS NMR. Moreover, the T1 and T1ρ values for 7Li and 11B are compared, and the activation energies were obtained. The T1ρ values of the boron nuclei in LiB3O5 show no significant changes. These results may be closely related to the largest second-order nonlinear optical coefficient. - Highlights: • The structural nature of the nonlinear optical properties of LiB3O5. • Single-crystal NMR and MAS NMR. • The 3-coordnated trigonal and 4-coordinated tetragonal. • The spin-lattice relaxation time in rotating frame T1ρ

  8. 1H and 7Li NMR in li2-xhxmo3 (m = Ti, Zr)

    Baklanova, Ya

    2008-01-01

    Nuclear magnetic resonance (NMR), Raman spectroscopy and thermogravimetric methods were used to study the peculiarities of lithium ion replacement by protons in lithium metallates Li2MO3 (M=Ti, Zr). In this article we show that almost all protons in the final substitution products H2MO3 enter into the crystal structure. All protons in zirconium hydroxide belong to hydrogen-bonded OH-groups. Contrary, titanium hydroxide contains both hydrogen-bonded and isolated OH-groups. Protons in H2ZrO3 fo...

  9. Identification of Li-Ion Battery SEI Compounds through (7)Li and (13)C Solid-State MAS NMR Spectroscopy and MALDI-TOF Mass Spectrometry.

    Huff, Laura A; Tavassol, Hadi; Esbenshade, Jennifer L; Xing, Wenting; Chiang, Yet-Ming; Gewirth, Andrew A

    2016-01-13

    Solid-state (7)Li and (13)C MAS NMR spectra of cycled graphitic Li-ion anodes demonstrate SEI compound formation upon lithiation that is followed by changes in the SEI upon delithiation. Solid-state (13)C DPMAS NMR shows changes in peaks associated with organic solvent compounds (ethylene carbonate and dimethyl carbonate, EC/DMC) upon electrochemical cycling due to the formation of and subsequent changes in the SEI compounds. Solid-state (13)C NMR spin-lattice (T1) relaxation time measurements of lithiated Li-ion anodes and reference poly(ethylene oxide) (PEO) powders, along with MALDI-TOF mass spectrometry results, indicate that large-molecular-weight polymers are formed in the SEI layers of the discharged anodes. MALDI-TOF MS and NMR spectroscopy results additionally indicate that delithiated anodes exhibit a larger number of SEI products than is found in lithiated anodes. PMID:26653886

  10. Li mobility in Nasicon-type materials LiM2(PO4)3, M = Ge, Ti, Sn, Zr and Hf, followed by 7Li NMR spectroscopy.

    Arbi, K; París, M A; Sanz, J

    2011-10-21

    Lithium mobility in LiM(2)(PO(4))(3) compounds, M = Ge and Sn, has been investigated by (7)Li Nuclear Magnetic Resonance (NMR) spectroscopy, and deduced information compared with that reported previously in Ti, Zr and Hf members of the series in the temperature range 100-500 K. From the analysis of (7)Li NMR quadrupole interactions (C(Q) and η parameters), spin-spin T(2)(-1) and spin-lattice T(1)(-1) relaxation rates, structural sites occupancy and mobility of lithium have been deduced. Below 250 K, Li ions are preferentially located at M(1) sites in rhombohedral phases, but occupy intermediate M(12) sites between M(1) and M(2) sites in triclinic ones. In high-temperature rhombohedral phases, a superionic state is achieved when residence times at M(1) and M(12) sites become similar and correlation effects on Li motion decrease. This state can be obtained by large order-disorder transformations in rhombohedral phases or by sharp first order transitions in triclinic ones. The presence of two relaxation mechanisms in T(1)(-1) plots of rhombohedral phases has been associated with departures of conductivity from the Arrhenius behavior. Long term mobility of lithium is discussed in terms of the cation vacancy distribution along conduction paths. PMID:21897945

  11. Solid 7Li-NMR and in situ XRD studies of the insertion reaction of lithium with tin oxide and tin-based amorphous composite oxide

    The lithium insertion reactions with tin (II) oxide (SnO) and tin-based composite oxide (abbreviated as TBCO) are studied by solid 7Li-NMR Knight shift, T1 and T1ρ relaxation rate, TEM and in situ XRD methods. By the insertion reaction for SnO, the lithium oxide and β-tin are produced first at Li/Sn = 2; at Li/Sn = 3 to 6 the products are not simple and a mixture of LiSn2, LiSn, Li5Sn2 and Li7Sn2 alloys is detected during the insertion. For the TBCO, which is revealed as amorphous, mainly constituted by randomly distributed very short-range (order of 10-9 m) regions by TEM observation, it is found that electrochemically inserted lithium forms Li2O and produces metallic tin (Sn) in the first step (Li/Sn 7Sn2 (and Li7Si2), are produced in the second step (Li/Sn >2). During the second step, the Li/Sn ratio of formed lithium-tin alloy is kept at almost 4. By the analyses of 7Li NMR Knight shifts, line shape and in situ XRD, the lithium-inserted TBCOs are characterized as almost amorphous and mixtures of highly ionic components. (author)

  12. [sup 7]Li-NMR determination of stability constants as a function of temperature for lithium-crown ether complexes in a molten salt mixtures

    Gerhard, A. (Univ. of Utah, Salt Lake City, UT (United States) Univ. of Witten/Herdecke (Germany)); Cobranchi, D.P.; Garland, B.A.; Highley, A.M.; Huang, Y.H.; Konya, G.; Eyring, E.M. (Univ. of Utah, Salt Lake City, UT (United States)); Zahl, A.; Eldik, R. van (Univ. of Witten/Herdecke (Germany)); Petrucci, S. (Polytechnic Univ., Farmingdale, NY (United States))

    1994-08-11

    The stability constants of several crown ethers with lithium ion were determined by [sup 7]Li-NMR measurements. A room temperature, basic molten salt of the composition of 55/45 mol % 1-methyl-3-ethyl-imidazolium chloride to aluminum (III) chloride was used as solvent. On the basis of a 1:1 complex formation the following order was found for the stability constants of the investigated crown ethers: 18-crown-6 < 12-crown-4 < benzo-15-crown-5 < 15-crown-5. A temperature dependence study for 12-crown-4, benzo-15-crown-5, and 15-crown-5 was undertaken for the range 5-84[degree]C. Values of [Delta]H and [Delta]S were calculated. At 5.5[degree]C the splitting of the single, fast exchange peak into two separate signals was observed for benzo-15-crown-5, providing further evidence for the formation of the 1:1 complex. 34 refs., 4 figs., 5 tabs.

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

    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.

  14. 通过在线7Li-NMR谱对负离子聚合见解的进一步验证%FURTHER CONFIRMATION OF THE ANIONIC POLYMERIZATION INSIGHT THROUGH in situ 7Li-NMR SPECTRUM

    胡迪航; 吴尚翰; 李天一; 郑安呐; 管涌

    2013-01-01

    通过对正丁基锂(n-BuLi)/四氢呋喃(THF)引发α-甲基苯乙烯(mSt)负离子本体聚合,验证了n-BuLi缔合体可以引发聚合,形成超分子团聚体,然后在进一步聚合过程中超分子解离.证实了先前提出的负离子聚合的引发机理.通过7 Li-NMR对聚合过程的在线检测,进一步证实了mSt在氘代苯为溶剂,THF为调节剂下的负离子聚合以及异戊二烯在非极性条件下的溶液聚合都存在引发剂多元缔合体向二元缔合体转变.研究还发现,少量THF可能使n-BuLi的六元缔合结构2~3个进一步串联起来,但先于六元缔合结构解离.此外,THF与n-BuLi作用,随着n-BuLi/THF的摩尔比从1∶1到1∶5的变化,可以使n-BuLi的巨大缔合体解离并向六元缔合体转变.

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

    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. Heterocyclic Analogs of Thioflavones: Synthesis and NMR Spectroscopic Investigations

    Wolfgang Holzer

    2009-09-01

    Full Text Available The synthesis of several hitherto unknown heterocyclic ring systems derived from thioflavone is described. Coupling of various o-haloheteroarenecarbonyl chlorides with phenylacetylene gives 1-(o-haloheteroaryl-3-phenylprop-2-yn-1-ones, which were treated with NaSH in refluxing ethanol to yield the corresponding bi- and tricyclic annelated 2-phenylthiopyran-4-ones. Detailed NMR spectroscopic investigations of the ring systems and their precursors are presented.

  17. Electric dipolarizability of 7Li

    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.

  18. NMR spectroscopic study of organic phosphate esters coprecipitated with calcite

    Phillips, Brian L.; Zhang, Zelong; Kubista, Laura; Frisia, Silvia; Borsato, Andrea

    2016-06-01

    Organic phosphorus incorporated in calcite during laboratory precipitation experiments and in natural cave deposits was investigated by solid-state NMR spectroscopy. For calcite precipitated in the presence of organic phosphoesters of varying size and functionality, solid-state 31P{1H} CP/MAS NMR shows that the phosphoesters were incorporated intact into the solid. Systematic changes in the 31P NMR chemical shift of the phosphate group were observed between the solid phosphoester and that incorporated in the solid precipitate, yielding 31P NMR chemical shifts of the coprecipitates in the range of +1.8 to -2.2 ppm. These chemical shifts are distinct from that of similarly prepared calcite coprecipitated with inorganic phosphate, 3.5 ppm. Only minor changes were noted in the phosphoester 31P chemical shift anisotropy (CSA) which suggests no significant change in the local structure of the phosphate group, which is dominated by C-O-P bonding. Close spatial proximity of the organic phosphate group to calcite structural components was revealed by 31P/13C rotational echo double resonance (REDOR) experiments for coprecipitates prepared with 13C-labeled carbonate. All coprecipitates showed significant 31P dephasing effects upon 13C-irradiation, signaling atomic-scale proximity to carbonate carbon. The dephasing rate for smaller organophosphate molecules is similar to that observed for inorganic phosphate, whereas much slower dephasing was observed for larger molecules having long and/or bulky side-chains. This result suggests that small organic molecules can be tightly enclosed within the calcite structure, whereas significant structural disruption required to accommodate the larger organic molecules leads to longer phosphate-carbonate distances. Comparison of 31P NMR spectroscopic data from the synthetic coprecipitates with those from calcite moonmilk speleothems indicates that phosphorus occurs mainly as inorganic orthophosphate in the natural deposits, although small

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

    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.

  20. NMR Spectroscopic Investigations of Catalyzed Reactions. Mechanisms, Kinetics & Unexpected Intermediates

    Leutzsch, Markus

    2015-01-01

    This thesis describes mechanistic studies by NMR spectroscopy in different areas of homogenous catalysis. Over the last years a wide range of organocatalysts were developed enabling highly diverse transformations with high enantioselectivities and excellent yields. In contrast to the high amount of publications on this field, a mechanistic understanding based on experimental evidences is often underinvestigated. Therefore the first two chapters of this thesis are focused on various (NMR-)...

  1. NMR spectroscopic study of the Murex trunculus dyeing process.

    Hoffman, Rina C; Zilber, Reut C; Hoffman, Roy E

    2010-11-01

    It is widely accepted that indigo dyes derived from Murex trunculus were used to produce the biblical dyes tekhelet and argaman. We describe a method of following the debromination of natural leucoindigos and their binding to wool using NMR spectroscopy. Debromination is observed prior to reaction with the wool and prior to oxidation. Binding to the wool is shown to occur prior to oxidation. NMR allows the dyeing process to be followed. This, in principle, could be used to correct problems during dyeing that would increase the reliability of the process. PMID:20882520

  2. 1H NMR spectroscopic identification of a glue sniffing biomarker.

    Kwon, Bobae; Kim, Siwon; Kim, Sosun; Lee, Dong-Kye; Park, Yu-Jin; Kim, Myung-Duck; Lee, Jae-Shin; Kim, Suhkmann

    2011-06-15

    Organic solvent abuse typically involves sniffing organic solvents to experience the mind-altering conditions they induce. In Republic of Korea, organic solvent abuse is a serious social problem, especially among teenagers. Several studies have addressed the effects of organic solvent abuse on mind and body, but there are no simple methods by which such abuse can be positively identified. In this report, we describe a method for analyzing toluene metabolites (toluene is the main ingredient of glue) in glue-sniffers' urine using (1)H NMR spectroscopy. Toluene is a commonly used solvent in the rubber, paint, plastics, leather, printing, and chemical industries. Inhaled toluene is metabolized to hippuric acid in the liver and excreted in the urine. Hippuric acid is known as a good biomarker for biological monitoring of toluene exposure. We have scanned hippuric acid and other toluene metabolites by NMR spectroscopy and performed statistical multivariate analysis of the data. Based on this analysis, we sought to determine parameters by which glue-sniffing (toluene inhalation) behavior may be verified. We also demonstrate the use of a pattern recognition method for accurate and efficient analysis of NMR data. In comparison to conventional methods, such as mass spectroscopy coupled with liquid chromatography or gas chromatography, nuclear magnetic resonance spectroscopy has several advantages, including simple sample preparation, non-destructive sampling, accuracy, short acquisition time, and reproducibility in the determination of urinary hippuric acid. PMID:21316881

  3. Investigation of 7Li(n, γ)8Li reaction by law energy

    The wave functions and main spectroscopic characteristics of the 8Li nucleus as well as the interaction potential in the 7Li+n channel are calculated within the frames of the three-body αtn-potential cluster model. The complete cross sections and reaction velocities of the 7Li(n, γ)8Li are determined along with the above values in the area of the energy up to 1 MeV

  4. 1H NMR spectroscopic determination of deterioration marker compounds in fats and oils

    Skiera, Christina

    2013-01-01

    In food and pharmaceutical analysis, the classical indices peroxide value (PV), acid value (AV) and p-anisidine value (ANV) still play an important role as quality and authenticity control parameters of fats and oils. These indices are sum parameters for certain deterioration products (PV for hydroperoxides, AV for free fatty acids, ANV for aldehydes) and are obtained using volumetric or UV/VIS spectroscopic analytical approaches. 1H NMR spectroscopy provides a fast and simple alternative to ...

  5. Complexation of enalapril maleate with β-cyclodextrin: NMR spectroscopic study in solution

    A detailed NMR (1H , COSY, ROESY) spectroscopic study of complexation of enalapril maleate with β-cyclodextrin was carried out. The 1H NMR spectrum of enalapril maleate confirmed the existence of cis-trans equilibrium in solution, possibly due to hindered rotation along the amide bond. The cis-trans ratio remained almost the same in the presence of β-cyclodextrin but in one case it was found significantly different which suggests a catalytic role of β-cyclodextrin in the isomerization. 1H NMR titration studies confirmed the formation of an enalapril-β-cyclodextrin inclusion complex as evidenced by chemical shift variations in the proton resonances of both the host and the guest. The stoichiometry of the complex was determined to be 2:1 (guest: host). The mode of penetration of the guest into the β-cyclodextrin cavity as well as the structure of the complex were established using ROESY spectroscopy. (author)

  6. Layered structure of room-temperature ionic liquids in microemulsions by multinuclear NMR spectroscopic studies.

    Falcone, R Dario; Baruah, Bharat; Gaidamauskas, Ernestas; Rithner, Christopher D; Correa, N Mariano; Silber, Juana J; Crans, Debbie C; Levinger, Nancy E

    2011-06-01

    Microemulsions form in mixtures of polar, nonpolar, and amphiphilic molecules. Typical microemulsions employ water as the polar phase. However, microemulsions can form with a polar phase other than water, which hold promise to diversify the range of properties, and hence utility, of microemulsions. Here microemulsions formed by using a room-temperature ionic liquid (RTIL) as the polar phase were created and characterized by using multinuclear NMR spectroscopy. (1)H, (11)B, and (19)F NMR spectroscopy was applied to explore differences between microemulsions formed by using 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim][BF(4)]) as the polar phase with a cationic surfactant, benzylhexadecyldimethylammonium chloride (BHDC), and a nonionic surfactant, Triton X-100 (TX-100). NMR spectroscopy showed distinct differences in the behavior of the RTIL as the charge of the surfactant head group varies in the different microemulsion environments. Minor changes in the chemical shifts were observed for [bmim](+) and [BF(4)](-) in the presence of TX-100 suggesting that the surfactant and the ionic liquid are separated in the microemulsion. The large changes in spectroscopic parameters observed are consistent with microstructure formation with layering of [bmim](+) and [BF(4)](-) and migration of Cl(-) within the BHDC microemulsions. Comparisons with NMR results for related ionic compounds in organic and aqueous environments as well as literature studies assisted the development of a simple organizational model for these microstructures. PMID:21547960

  7. In vivo 31P NMR spectroscopic studies on brain metabolic deterioration

    A custom-built 31P NMR spectrometer with 5.6 Tesla, horizontal magnet was used to determine the changes of in vivo phosphorus metabolism of the rat brain in various pathological conditions. 31P NMR spectroscopy readily demonstrated cerebral metabolic deterioration and/or recovery in vivo, in terms of the changes in relative concentrations of phosphate metabolites such as adenosine triphosphate (ATP), phosphocreatine (PCr) and inorganic phosphate (Pi), and the alterations of intracellular pH (pHi) calculated from the chemical shift of the Pi peak relative to the PCr peak, following different kinds of brain insults. 25-minute hypoxia caused the decrease in PCr and the increase in Pi with ATP's unchanged. After 15-minute global ischemia, PCr and ATP peaks completely disappeared, which recovered after the restoration of cerebral blood flow. 31P NMR spectroscopy clearly showed metabolic deterioration associated with focal cerebral infarction in the rat with middle cerebral artery occluded 24 hours previously. Severe impact trauma provoked progressive deterioration of cerebral phosphorus metabolism. This alteration was notified even at the first five-minute spectrum. The author has demonstrated that in vivo 31P NMR spectroscopic measurement would be useful and fascinating to evaluate in vivo phosphorus metabolism at various pathological states repeatedly and noninvasively. (author)

  8. 1H NMR spectroscopic studies establish that heparanase is a retaining glycosidase

    Highlights: •1H and 13C NMR chemical shifts of fondaparinux were fully assigned by 1D and 2D NMR techniques. •Hydrolysis of fondaparinux by heparanase was monitored by 1H 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 1H 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

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

    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.

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

    Arcisauskaité, Vaida

    -Parrinello molecular dynamics approach(CPMD) and showed that the 1st coordination sphere of Zn(II) comprises six water molecules in agreement with the experimental results. Secondly, we performed Direct CPMD metadynamics simulations on the equilibrated structure by introducing an additional bias potential acting...... cases more than in others. These results suggest that the calculations on the Hg binding sites in proteins should include the immediate chemical environment. In addition, for the first time in Paper 2 we conducted the projection analysis of molecular orbital contributions to Vzz in some small Hg......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...

  11. A new mass value for 7Li

    Nagy, Sz; Suhonen, M; Schuch, R; Blaum, K; Björkhage, M; Bergström, I; 10.1103/PhysRevLett.96.163004

    2012-01-01

    A high-accuracy mass measurement of 7Li was performed with the Smiletrap Penning trap mass spectrometer via a cyclotron frequency comparison of Li3+ and H2+. A new atomic mass value of 7Li has been determined to be 7.016,003,425,6,(45)u with a relative uncertainty of 0.63 ppb. It has uncovered a discrepancy as large as 14 sigma (1.1 micro u) deviation relative to the literature value given in the Atomic-Mass Evaluation AME 2003. The importance of the improved and revised 7Li mass value, for calibration purposes in nuclear-charge radii and atomic mass measurements of the neutron halos 9Li and 11Li, is discussed.

  12. Low temperature FTIR, Raman, NMR spectroscopic and theoretical study of hydroxyethylammonium picrate

    Sudharsana, N.; Sharma, A.; Kuş, N.; Fausto, R.; Luísa Ramos, M.; Krishnakumar, V.; Pal, R.; Guru Row, T. N.; Nagalakshmi, R.

    2016-01-01

    A combined experimental (infrared, Raman and NMR) and theoretical quantum chemical study is performed on the charge-transfer complex hydroxyethylammonium picrate (HEAP). The infrared (IR) spectra for HEAP were recorded at various temperatures, ranging from 16 K to 299 K, and the Raman spectrum was recorded at room temperature. A comparison of the experimental IR and Raman spectra with the corresponding calculated spectra was done, in order to facilitate interpretation of the experimental data. Formation of the HEAP complex is evidenced by the presence of the most prominent characteristic bands of the constituting groups of the charge-transfer complex [e.g., NH3+, CO- and NO2]. Vibrational spectroscopic analysis, together with natural bond orbital (NBO) and theoretical charge density analysis in the crystalline phase, was used to shed light on relevant structural details of HEAP resulting from deprotonation of picric acid followed by formation of a hydrogen bond of the N-H⋯OC type between the hydroxyethylammonium cation and the picrate. 13C and 1H NMR spectroscopic analysis are also presented for the DMSO-d6 solution of the compound revealing that in that medium the HEAP crystal dissolves forming the free picrate and hydroxyethylammonium ions. Finally, the electron excitation analysis of HEAP was performed in an attempt to determine the nature of the most important excited states responsible for the NLO properties exhibited by the compound.

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

    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)

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

    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 13C 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 13C NMR were used to obtain information about SOM structures and their interactions with residual paramagnetic metal ion. The signal of the residual metallic oxycation, VO2+ correlated positively with uronic acid-type hydrophilic organic structures, determined from the 13C 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. Reaction mechanism study of 7Li(7Li, 6He) reaction at above Coulomb barrier energies

    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.

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

    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.

  17. Raman and 31P MAS NMR spectroscopic studies of lead phosphate glasses containing thorium oxide

    (PbO)0.5(P2O5)0.5 glasses in which part of the PbO/ P2O5 was replaced by ThO2 up to 10 mol% have been prepared by conventional melt quench method and characterized by Raman and 31P MAS NMR spectroscopic studies. Raman studies of these samples clearly revealed the existence of PO4 structural units having two non bridging oxygen atoms attached to phosphorus (PO22-). The 31P MAS NMR studies indicated the presence of two types of phosphorus structural units in both PbO -P2O5 and PbO-P2O5-ThO2 glasses, namely Q2 and Q1 (PO4 structural units with 2 and 1 bridging oxygen atoms respectively). Increase in the concentration of ThO2 at the expense of both PbO/P2O5 has been found to result in the increased amount of Q1 structural units of phosphorus, indicating that ThO2 acts as only a network modifier. ThO2 has been found to form the glassy phase with PbO-P2O5 system only up to 10 mol%. (author)

  18. $^{7}$Li abundances in halo stars testing stellar evolution models and the primordial $^{7}$Li abundance

    Chaboyer, B; Brian Chaboyer

    1994-01-01

    A large number of stellar evolution models with [Fe/H] = -2.3 and -3.3 have been calculated in order to determine the primordial .sup(7)Li abundance and to test current stellar evolution models by a comparison to the extensive database of Li abundances in extremely metal poor halo stars observed by Thorburn (1994). Standard models do a good job of fitting the observed Li abundances in stars hotter than 5600 K. They predict a primordial ^7Li abundance of log N(Li) = 2.24\\pm 0.03. Models which include microscopic diffusion predict a downward curvature in the .sup(7)Li destruction isochrones at hot temperatures which is not present in the observations. Thus, the observations clearly rule out models which include uninhibited microscopic diffusion of .sup(7)Li from the surface of the star. The [Fe/H] = -2.3 stellar models which include both diffusion and rotational mixing provide an excellent match to the observations. Both the plateau stars and the heavily depleted cool stars are well fit by these models. The rot...

  19. Angular correlations and decay branching ratio for excited state of 7Li*(7,45 MeV) in reactions 7Li(alpha, alpha)7Li*

    Measurements of differential cross-sections of alpha-particle inelastic scattering by 7Li nuclei and 7Li(alpha, alpha 6Li)n, 7Li(alpha, alpha alpha)t reactions have been performed at the energy Ea = 27,2 MeV. Probability of 7Li*(7,45 MeV) decay into 6Li + n channel has been determined from the ratio of cross-sections measured in kinematically complete and incomplete experiments. The large discrepancy of this value (P 0,49 ± 0,06) and of those obtained at the study of 7Li*(7,45 MeV) decay in binary reactions can be explained by the influence of Coulomb field of accompanied alpha-particle on the decay of near-threshold resonances in three-particle reactions

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

    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.

  1. Line shapes of prompt γ-ray from 7*Li produced in 10B(n,α)7*Li reaction

    Prompt γ-ray spectra of recoil 7*Li produced in the 10B(n,α)7*Li reaction were measured using neutron beam. The observed Doppler broadening energy spectra were satisfactorily reproduced by a simulation where the velocity degradation of 7*Li within its lifetime of 1.05x10-13 s was estimated using the LSS theory. Our successful line-shape analysis was applied to non-destructive state analysis of trace amounts of boron. (author)

  2. Energy levels in (7Li) nucleus

    The energies of the normal-parity states and positive parity states in (7Li) nucleus are calculated, using many-particle nuclear shell-model, and the harmonic oscillator-wave-functions, over the residual interaction of the Gaussian from the Serber force. Spin-orbit interactions are neglected. The kinetic energy is introduced as a variant quantity, through the variation of the harmonic oscillator parameter (r0) (r02=h/mw). Finally, we separate the ''spurious'' states (one quantum excitations of the center of mass of the nucleus) by the effect of the operator (R-i), for the coordinate of the center of mass on the different wave-functions of the ground state-configurations. The calculations show that the energy of the positive-parity states, separated into two groups; the first in the energy region (10-20 Mev) and described by the symmetries (43), (421); and the second group in the energy region (26-46 Mev) and described by the symmetries (31), (3211). 9 tabs.; 3 figs.; 64 refs

  3. Reactions 7Li(e,6He) pe' and 7Li(e,6Li) ne' at intermediate excitation energies

    The reactions 7Li(e,6He) pe' and 7Li(e,6Li) ne' have been studied at intermediate excitation energies. Angular distributions as well as energy distributions are presented. The experimental cross sections are compared to the results obtained from a simple model

  4. Chemical and physical properties of the normal and aging lens: spectroscopic (UV, fluorescence, phosphorescence, and NMR) analyses

    In vitro [UV absorption, fluorescence, phosphorescence, and nuclear magnetic resonance (NMR)] spectroscopic studies on the normal human lens demonstrate age-related changes which can be correlated with biochemical and photobiologic mechanisms occurring during our lifetime. Chronic cumulative UV exposure results in an age-related increase of photochemically induced chromophores and in color of the lens nucleus. This enables the lens to filter the incident UV radiation, thereby protecting the underlying aging retina from UV photodamage. We have measured the age-related increase in lens fluorescence in vivo on more than 300 normal subjects (1st to 9th decade) by UV slitlamp densitography. These data show a good correlation with the in vitro lens fluorescence studies reported previously and demonstrate that molecular photodamage can be monitored in the lens. In vitro NMR (human and animal lenses) and in vivo experiments currently in progress are rapidly elucidating the physicochemical basis for transparency and the development of light scattering areas. Surface scanning NMR can monitor organophosphate metabolism in the ocular lens in vivo as well as in vitro. These studies demonstrate the feasibility of using biophysical methods (optical spectroscopy and NMR analyses) to delineate age-related parameters in the lens, in vivo as well as in vitro. 46 references

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

    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.

  6. Static and dynamic moments of the 7Li nucleus

    The data of Weller et al. (1985) on the tensor analysing powers for elastic and inelastic Coulomb scattering of aligned 7Li ions have been reanalyzed in order to obtain information on the values of the four 7Li moments Q, B(E2)↑, τ11 and τ12. It is shown that a single set of values, chosen primarily to be consistent with the value of Q measured by molecular techniques and the values of B(E2)↑ and τ12. required to fit unpolarized 7Li data, and also with the theoretical constraint τ11≅-[τ12], gives a good fit to the aligned 7Li data. 19 refs., 6 figs

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

    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...... endogenous polar compounds that are present in the urine. The individual metabolites were purified by preparative high performance liquid chromatography (HPLC) and then identified using H-1 NMR, Both one- and two-dimensional NMR experiments were performed to identify the phase II metabolites of tolfenamic......), and N-(2-methyl-4-hydroxyphenyl)-anthranilic acid (11) were identified. The phase II metabolites (5-11) had not previously been identified in urine from humans administered tolfenamic acid. The phase I metabolites of the glucuronides 7, 8, 10, and 11 were identified here for the first time. An HPLC...

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

    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.

  9. Electronic structure and solvatochromism of merocyanines NMR spectroscopic point of view.

    Kulinich, Andrii V; Ishchenko, Alexander A; Groth, Ulrich M

    2007-09-01

    (1)H and (13)C NMR spectra of two series of malononitrile-based merocyanines, which possess positive and negative solvatochromism have been in detail investigated in low polar chloroform and polar dimethyl sulfoxide (DMSO). Careful attribution of signals in spectra has been made with the help of two-dimensional NMR experiments (COSY, NOESY, HMBC, and HMQC). Hence, the dependence of merocyanines electronic structure on their chemical structure and solvent nature has been studied by this powerful method. It has been shown that there exists a good correlation between the calculated charges on carbon atoms of a polymethine chain and their chemical shifts in (13)C NMR spectra. The influence of solvent polarity on bond orders for dyes with positive and negative solvatochromism is also observed. The comparison of (13)C NMR spectra of merocyanines and corresponding parent ionic dyes allows to determine their sign of solvatochromism irrespectively of electronic spectra, and also to find the key atoms of chromophore whose signals in (13)C NMR spectra are most informative. PMID:17188560

  10. NMR spectroscopic studies on metallo-base-pair in DNA duplex

    Tanaka, Y.; Okamoto, I.; Furuita, K.; Šebera, Jakub; Kondo, J.; Torigoe, H.; Urata, H.; Dairaku, T.; Ono, A.; Kojima, C.; Sychrovský, Vladimír

    2014-01-01

    Roč. 19, Suppl 2 (2014), S732-S733. ISSN 0949-8257. [European Biological Inorganic Chemistry Conference /12./. 24.08.2014-28.08.2014, Zurich] Institutional support: RVO:61388963 Keywords : NMR * DNA * mercury * thymine Subject RIV: CF - Physical ; Theoretical Chemistry

  11. Ionic conductivity of chemically lithiated YBa2Cu3O7: NMR and impedance spectroscopic studies

    High-Tc superconducting YBa2Cu3O7 ceramic samples are lithiated by the reaction with n-butyllithium. For lithium nominal contents less than unity per formula the presence of '123' and '124' phases are deduced from X-ray diffraction and high-resolution electron microscopy experiments. NMR and impedance spectroscopy techniques have been conducted in a sample with a nominal Li content of 0.9 per formula. Spin-lattice relaxation times and electrical conductivity relaxation (ECR) are measured as a function of temperature. NMR and ECR data are interpreted in terms of a stretched exponential decay function in the time domain. Microscopic activation energies for lithium motion of 0.49 eV (NMR measurements) and of 0.41 eV (ECR) are deduced for short range motion. Activation energies for long range motion of 0.98 eV (NMR) and 1.03 eV (ECR) are also deduced. (author)

  12. (6)Li, (7)Li Nuclear Magnetic Resonance Investigation of Lithium Coordination in Binary Phosphate Glasses

    Alam, T.M.; Boyle, T.J.; Brow, R.K.; Conzone, S.

    1999-02-08

    {sup 6}Li and {sup 7}Li solid state magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectroscopy has been used to investigate the local coordination environment of lithium in a series of xLi{sub 2}O {center_dot} (1-x)P{sub 2}O{sub 5} glasses, where 0.05 {le} x {le} 0.55. Both the {sup 6}Li and {sup 7}Li show chemical shift variations with changes in the Li{sub 2}O concentration, but the observed {sup 6}Li NMR chemical shifts closely approximate the true isotropic chemical shift and can provide a measure of the lithium bonding environment. The {sup 6}Li NMR results indicate that in this series of lithium phosphate glasses the Li atoms have an average coordination between four and five. The results for the metaphosphate glass agree with the coordination number and range of chemical shifts observed for crystalline LiPO{sub 3}. An increase in the {sup 6}Li NMR chemical shift with increasing Li{sub 2}O content was observed for the entire concentration range investigated, correlating with increased cross-linking of the phosphate tetrahedral network by O-Li-O bridges. The {sup 6}Li chemical shifts were also observed to vary monotonically through the anomalous glass transition temperature (T{sub g}) minimum. This continuous chemical shift variation shows that abrupt changes in the Li coordination environment do not occur as the Li{sub 2}O concentration is increased, and such abrupt changes can not be used to explain the T{sub g} minimum.

  13. A newly synthesized thiazole derivative as a fluoride ion chemosensor: Naked-eye, spectroscopic, electrochemical and NMR studies

    Sarıgüney, Ahmet Burak; Saf, Ahmet Özgür; Coşkun, Ahmet

    2014-07-01

    2,3-Indoledione 3-thiosemicarbazone (TSCI) and a novel compound 3-(2-(4-(4-phenoxyphenyl)thiazol-2-yl)hydrazono)indolin-2-one (FTHI) were synthesized with high yield and characterized by spectroscopic techniques. The complexation behaviors of TSCI and FTHI for various anionic species (F-, Cl-, Br-, I-, NO2-, NO3-, BzO-, HSO4-, ClO4-) in CH3CN were investigated and compared by UV-vis spectroscopy, cyclic voltammetry and 1H NMR titration techniques. FTHI showed high degree of selectivity for fluoride over other anions. This selectivity could be easily observed by the naked eye, indicating that FTHI is potential colorimetric sensor for fluoride anion.

  14. Photoassociation and ionization spectroscopy of ultracold $^{7}$Li$^{85}$Rb molecules

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

    2014-01-01

    We report spectroscopic studies of ultracold $^{7}$Li$^{85}$Rb molecules using multiphoton ionization detection. With our dual-species Li and Rb MOT apparatus, we create ultracold LiRb molecules via photoassociation (PA), and explore new PA resonances, with binding energies up to ~62 cm^{-1}. Furthermore, we measure the resonantly enhanced multiphoton ionization (REMPI) spectra as a probe of ground and excited state vibrational levels. We identify vibrational levels of the $a^{3}\\Sigma^{+} (v" = 7 - 13)$, $3^{3} \\Pi (v'_{\\Pi} = 0 - 10)$ and $4^{3} \\Sigma^{+} (v'_{\\Sigma} = 0 - 5)$ electronic states. Our line assignments agree well with ab initio calculations. These spectroscopic studies are crucial to discovering transition pathways for transferring ultracold LiRb molecules created via PA to deeply bound rovibrational levels of the electronic ground state.

  15. Operando NMR spectroscopic analysis of proton transfer in heterogeneous photocatalytic reactions.

    Wang, Xue Lu; Liu, Wenqing; Yu, Yan-Yan; Song, Yanhong; Fang, Wen Qi; Wei, Daxiu; Gong, Xue-Qing; Yao, Ye-Feng; Yang, Hua Gui

    2016-01-01

    Proton transfer (PT) processes in solid-liquid phases play central roles throughout chemistry, biology and materials science. Identification of PT routes deep into the realistic catalytic process is experimentally challenging, thus leaving a gap in our understanding. Here we demonstrate an approach using operando nuclear magnetic resonance (NMR) spectroscopy that allows to quantitatively describe the complex species dynamics of generated H2/HD gases and liquid intermediates in pmol resolution during photocatalytic hydrogen evolution reaction (HER). In this system, the effective protons for HER are mainly from H2O, and CH3OH evidently serves as an outstanding sacrificial agent reacting with holes, further supported by our density functional theory calculations. This results rule out controversy about the complicated proton sources for HER. The operando NMR method provides a direct molecular-level insight with the methodology offering exciting possibilities for the quantitative studies of mechanisms of proton-involved catalytic reactions in solid-liquid phases. PMID:27311326

  16. High resolution 1H NMR spectroscopic studies of the metabolism and excretion of ampicillin in rats and amoxycillin in rats and man.

    Connor, S C; Everett, J R; Jennings, K R; Nicholson, J K; Woodnutt, G

    1994-02-01

    High resolution proton nuclear magnetic resonance (1H NMR) spectroscopy has been used to investigate the metabolism and urinary excretion of the aminopenicillins, ampicillin and amoxycillin, in rats and of amoxycillin in man. 1H NMR resonances of the aminopenicillins, together with those for their 5R, 6R and 5S, 6R penicilloic acids and diketopiperazine metabolites were detected, assigned and quantified in urine samples with the aid of spin-echo NMR techniques. The dimer of amoxycillin was detected in rat urine for the first time together with novel drug-related resonances assigned to amoxycillin carbamate. Quantitative 1H NMR spectroscopic results were consistent with HPLC and microbiological data considering that only single measurements were recorded. Due to the short analysis time and simple sample preparation, NMR was particularly useful for studying the metabolism of the aminopenicillins for which sample degradation poses analytical problems. The non-invasive character of 1H NMR spectroscopic analysis of urine also provided unique information on a reversible reaction between amoxycillin and bicarbonate, an endogenous urinary metabolite. PMID:8021801

  17. The 7Li(γ,N) and 7Li(e,N) reactions at intermediate photon energies

    Cross sections for single-photonucleon emissions from 7Li have been measured for photon energies in the range 60-120 MeV by detecting the recoiling residual nuclei following excitation with bremsstrahlung radiation of end-point energies 140 and 155 MeV. Measurements of the 7Li(e,6Li)e'p and 7Li(e,6He)e'n cross sections were also made at the same electron energies. A significant difference between the ratio of electron- and bremsstrahlung-induced yields for proton and neutron emission is observed. The results are compared to a modified quasi-deuteron model and a simple direct-knockout model in which recoil terms are included. (orig.)

  18. Computational and Experimental Evidence of Through-Space NMR Spectroscopic J Coupling of Hydrogen Atoms

    Dračínský, Martin; Jansa, Petr; Bouř, Petr

    2012-01-01

    Roč. 18, č. 3 (2012), s. 981-986. ISSN 0947-6539 R&D Projects: GA AV ČR KJB400550903; GA MŠk(CZ) LH11033; GA ČR GAP208/11/0105 Grant ostatní: AV ČR(CZ) M200550902 Institutional research plan: CEZ:AV0Z40550506 Keywords : conformations * density functional calculations * NMR spectroscopy * through-space coupling * weak interactions Subject RIV: CC - Organic Chemistry Impact factor: 5.831, year: 2012

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

    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. PMID:25127577

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

    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.

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

    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.

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

    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.

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

    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.

  4. The structural environments of cations adsorbed onto clays: A 133CsMAS NMR spectroscopic study

    Chapter One investigates the local structural environment of adsorbed cations on the mineral hectorite using 133Ca Variable-Temperature Magic-Angle-Spinning Nuclear Magnetic Resonance (VT-MAS NMR) spectroscopy. The results show that Cs on hectorite occurs in several distinctly different chemical environments, and that motional averaging of Ca between some of these sites occurs above ∼-40 degree C if water is present in the interlayer. Above ∼-10 degree C, spectra for slurries of hectorite in CsCl solutions yield two peaks, one due to Cs in solution, and the other due to Cs motionally-averaged on the clay. Below ∼-60 degree C, motional averaging of the adsorbed Cs slows sufficiently to allow resolution of two peaks representing different Cs-environments on the clay. The Stern-Gouy model is employed to explain these peaks and assign one to Cs in the Stern layer (relatively tightly bound to the basal oxygens), and the other to Cs in the Gouy diffuse layer. Between ∼-60 and ∼-10 degree C peaks for these two sites and a motionally-averaged peak are present. Cs-exchanged hectorite dehydrated at 500 degree C yields peaks for two different sites on the clay, interpreted to be highly coordinated site (probably 12), and a less coordinated site (possibly 9), both in the interlayer. Chapter II discusses 133Cs MAS NMR results for a number of other Cs-exchanged clays and the relationship of chemical and structural parameters to the 133Cs chemical shift. Increased rotational distortions of the basal oxygen sheet, total layer charge and tetrahedral Al3+ for Si4+ substitution correlate with increased deshielding of the 133Cs chemical shifts for both hydrated slurry and anhydrous samples. Correlations for the slurries are poorer because of the distances between the clay silicate and the CO in solution

  5. Synthesis of Radiation Curable Palm Oil–Based Epoxy Acrylate: NMR and FTIR Spectroscopic Investigations

    Ashraf M. Salih

    2015-08-01

    Full Text Available Over the past few decades, there has been an increasing demand for bio-based polymers and resins in industrial applications, due to their potential lower cost and environmental impact compared with petroleum-based counterparts. The present research concerns the synthesis of epoxidized palm oil acrylate (EPOLA from an epoxidized palm oil product (EPOP as environmentally friendly material. EPOP was acrylated by acrylic acid via a ring opening reaction. The kinetics of the acrylation reaction were monitored throughout the reaction course and the acid value of the reaction mixture reached 10 mg KOH/g after 16 h, indicating the consumption of the acrylic acid. The obtained epoxy acrylate was investigated intensively by means of FTIR and NMR spectroscopy, and the results revealed that the ring opening reaction was completed successfully with an acrylation yield about 82%. The UV free radical polymerization of EPOLA was carried out using two types of photoinitiators. The radiation curing behavior was determined by following the conversion of the acrylate groups. The cross-linking density and the hardness of the cured EPOLA films were measured to evaluate the effect of the photoinitiator on the solid film characteristics, besides, the thermal and mechanical properties were also evaluated.

  6. a Combined Molecular Dynamics and NMR Spectroscopic Protocol for the Conformational Analysis of Oligosaccharides.

    Varma, Vikram

    A combined experimental and theoretical protocol for the conformational analysis of oligosaccharides is presented. Three disaccharides, methyl alpha - scD-mannopyranosyl-(1 to 3)-alpha- scD-mannopyranoside, methyl beta- scD-galactopyranosyl-(1 to 4)-beta- scD-glucopyranoside, and propyl beta- scD-2-acetamido -2-deoxy glucopyranosyl-(1 to 3)- alpha- scL-rhamnopyranoside, are used to evaluate a protocol for conformational analysis that makes use of molecular dynamics calculations with the CHARMM force field. Dynamics trajectories computed in vacuo and in water are used to calculate time-averaged NMR parameters such as spin-lattice relaxation times (T_1 ), Nuclear Overhauser Enhancements (NOE), and heteronuclear spin-spin coupling constants (^3J _{rm CH}). The calculated NMR parameters are then compared to experimental values and used to evaluate the computational procedure. The energetically accessible conformations are effectively sampled by the simulations. The method has been extended to the conformational analysis of higher-order oligosaccharides corresponding to the cell-wall polysaccharide of the Streptococcus Group A, and the Shigella flexneri Y O-antigen. The Streptococcus Group A cell-wall polysaccharide is comprised of a backbone of rhamnopyranosyl units connected by alternating alpha- scL-(1 to 3) and alpha- scL -(1 to 2) linkages, to which are attached N-acetyl-beta- scD-glucosamine ( beta- scD-GlcpNAc) residues at the 3 positions of the rhamnose backbone.rm A&rm B^'qquad A^'& rm Bqquad Acr[{-alpha}{-}L{-}Rha {it p}{-}(1to2){-alpha }{-}L{-}Rha{it p} {-}(1to3){-alpha}{ -}L{-}Rha{it p}-(1to2) -alpha-L-Rha{it p}{-}(1 to3){-alpha}{-}L{- }Rha{it p}{-}cr&uparrow(1 to3)&uparrow(1to3)crbeta {-}D{-}&rm Glc{it p }NAcqquadbeta{-}D{-}& rm Glc{it p}NAccr&rm C ^'&rm C] A branched trisaccharide (A^' -(C)B), a tetrasaccharide (A^' -(C)B-A), a pentasaccharide (C^' -B^'-A ^'-(C)B), and two hexasaccharides (C^'-B^ '-A^' -(C)B-A) and (A-(C^')B ^'-A^' -(C)B), have been chosen

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

    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.

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

    Highlights: • 1H NMR profilings of 718 wines were fused with stable isotope analysis data (SNIF-NMR, 18O, 13C). • 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 1H NMR to 99% for the fused data). • Independent component analysis was used as an alternative chemometric tool for classification. - Abstract: It is known that 1H 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 1H NMR profiles are fused with stable isotope (SNIF-NMR, 18O, 13C) data. Variable selection based on clustering of latent variables was performed on 1H 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 1H 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 1H NMR data alone in 82–89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for 1H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of 1H 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

  9. Spectroscopic effects in {sup 1}H and {sup 13}C NMR spectra of 4,4`-di-substituted 3,3`-diquinolines sulfides; Efekty spektroskopowe w widmach {sup 1}H i {sup 13}C NMR 4,4`-dwupodstawionych sulfidow 3,3` dichinolinylowych

    Pluta, K. [Katedra i Zaklad Chemii Organicznej, Slaska Akademia Medyczna, Sosnowiec (Poland)

    1994-12-31

    The {sup 1}H and {sup 13}C NMR spectra of 4,4`-disubstituted sulfides of 3,3`-quinolines have been studied in CDCl{sub 3} solutions. The observed spectroscopic effects have been interpreted in terms of molecule structure and configuration. The factors being responsible for the value of spectroscopic effects have been discussed. 11 refs, 3 tabs.

  10. 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

    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.

  11. A comparative study of selected disperse azo dye derivatives based on spectroscopic (FT-IR, NMR and UV-Vis) and nonlinear optical behaviors

    Cinar, Mehmet; Coruh, Ali; Karabacak, Mehmet

    2014-03-01

    In the present work, a combined experimental and quantum chemical study on ground state equilibrium structure, spectroscopic and nonlinear optical properties of selected disperse azo dye molecules are reported. The vibrational transitions were identified based on the recorded FT-IR spectra in the range of 4000-400 cm-1 for solid state, simulated IR spectra and total energy distribution (TED) of vibrational modes. The chemical shifts were determined from the results of observed 1H and 13C NMR spectra in chloroform and dimethylsulfoxide solution. The DFT/gauge-invariant atomic orbital (GIAO) methodology was applied to predict the magnetic properties. Electronic properties were carried out by UV-Vis spectroscopy and TD-DFT/CIS approach. The nonlinear optical (NLO) features were addressed theoretically. A detailed description of spectroscopic and NLO behaviors of studied disperse azo dyes was reported with the help of comparison of experimental measurements and theoretical calculations.

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

    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...

  13. Detection of the inverse pion electroproduction on 7Li nuclei

    The inverse pion electroproduction process on 7Li nucleus, π++7Li→e++e-+X, at the pion kinetic energy of 380 MeV has been detected. The missing mass distribution of the process events is described well assuming that approximately one half of the detected events belongs to the reaction channel producing 7Be nucleus either in the ground state (7Be) or in the excited state (7Be*): π++7Li→e++e-+7Be(7Be*). For this reaction the differential cross section for the electron and positron energies above 70 MeV, for the particles emitted under an angle of about 65 deg in l. s., is d2σ/dΩ2=(1.3+-0.3)x10-32 cm2/sr2

  14. Fission fragment mass and angular distribution in 6,7Li+235,238U reactions

    Fission fragment (FF) angular distributions for 6,7Li+235,238U reactions and mass distributions for 6,7Li+ 238U reactions have been measured at energies near and above the Coulomb barrier. The angle integrated fission cross sections for 6Li induced reactions at sub-barrier energies are found to be higher than 7Li induced reactions possibly due to larger contribution of breakup induced fission in case of the former compared to the latter. The FF anisotropy for 6,7Li+235U was found to be smaller than 6,7Li+238U, manifesting the effect of target ground state spin. The statistical saddle point (SSP) model predictions were found to be consistent with the measured FF anisotropy for 6,7Li+235U, however they were under-estimated for 6,7Li+238U particularly at lower energies. Observation of larger FWHM of FF folding angle distribution and sharp increase in peak to valley ratio for FF mass distribution with the decrease in bombarding energy in 6,7Li+238U reactions confirms the presence of breakup induced fission. (authors)

  15. Fission fragment mass and angular distribution in 6,7Li+235,238U reactions

    Santra S.

    2013-12-01

    Full Text Available Fission fragment (FF angular distributions for 6,7Li+235,238U reactions and mass distributions for 6,7Li+238U reactions have been measured at energies near and above the Coulomb barrier. The angle integrated fission cross sections for 6Li induced reactions at sub-barrier energies are found to be higher than 7Li induced reactions possibly due to larger contribution of breakup induced fission in case of the former compared to the latter. The FF anisotropy for 6,7Li+235U was found to be smaller than 6,7Li+238U, manifesting the effect of target ground state spin. The statistical saddle point (SSP model predictions were found to be consistent with the measured FF anisotropy for 6,7Li+235U, however they were under-estimated for 6,7Li+238U particularly at lower energies. Observation of larger FWHM of FF folding angle distribution and sharp increase in peak to valley ratio for FF mass distribution with the decrease in bombarding energy in 6,7Li+238U reactions confirms the presence of breakup induced fission.

  16. Use of 7Li(p,n) reaction as a neutron source in a PGNAA setup.

    Naqvi, A A; Nagadi, M M

    2005-03-01

    The performance of a 7Li(p,n) reaction-based Prompt Gamma Ray Neutron Activation Analysis (PGNAA) setup has been determined for analysis of Portland cement samples using Monte Carlo study. The calculations were carried out for a 7Li(p,n) reaction-based PGNAA setup with an external moderator similar to the one used in a previous 2.8 MeV neutrons-based PGNAA setup. The optimum values of geometry parameters of the 7Li(p,n) reaction-based setup are different from those of the 2.8 MeV neutrons-based setup resulting in better performance of the 7Li(p,n) reaction-based setup. The prompt gamma-ray yield from the 7Li(p,n) reaction-based setup is 60-70% higher than that from the 2.8 MeV neutrons-based setup. Although the performances of the 7Li(p,n) reaction-based setup is comparable with that of a previously studied 3H(p,n) reaction-based setup, yet performance of the 7Li(p,n) reaction-based setup is superior to that of the 3H(p,n) reaction-based setup because it has less radiation hazard due to utilization of non-radioactive neutron producing target. This study has provided a theoretical base for experimental test of a 7Li(p,n) reaction-based PGNAA setup. PMID:15607917

  17. Use of 7Li(p,n) reaction as a neutron source in a PGNAA setup

    The performance of a 7Li(p,n) reaction-based Prompt Gamma Ray Neutron Activation Analysis (PGNAA) setup has been determined for analysis of Portland cement samples using Monte Carlo study. The calculations were carried out for a 7Li(p,n) reaction-based PGNAA setup with an external moderator similar to the one used in a previous 2.8 MeV neutrons-based PGNAA setup. The optimum values of geometry parameters of the 7Li(p,n) reaction-based setup are different from those of the 2.8 MeV neutrons-based setup resulting in better performance of the 7Li(p,n) reaction-based setup. The prompt γ-ray yield from the 7Li(p,n) reaction-based setup is 60-70% higher than that from the 2.8 MeV neutrons-based setup. Although the performances of the 7Li(p,n) reaction-based setup is comparable with that of a previously studied 3H(p,n) reaction-based setup, yet performance of the 7Li(p,n) reaction-based setup is superior to that of the 3H(p,n) reaction-based setup because it has less radiation hazard due to utilization of non-radioactive neutron producing target. This study has provided a theoretical base for experimental test of a 7Li(p,n) reaction-based PGNAA setup

  18. Prospects of lithium enrichment on 7Li isotope by method of controlled ions electro-migration

    Martoyan, G. A.; Kalugin, M. M.; Gabrielyan, A. V.; Martoyan, A. G.

    2016-01-01

    This paper deals with a new electro-membrane method of enrichment of 7Li isotope. The data are presented on the importance and application fields regarding the use of 7Li isotopes. Existing methods and criteria of separation of lithium isotopes are discussed. The principle of new technology, regimes of enrichment experiments, and analysis details of obtained products are briefly described.

  19. Study of fusion barrier distribution from quasielastic scattering for 6,7Li + 197Au systems

    Earlier we have reported breakup and fusion excitation function measurements in 6,7Li + 197Au systems. In this paper we present the fusion barrier distribution from QEL at backward angles for the same systems, namely, 6,7Li + 197Au

  20. Determination of nuclear reduced transition probabilities by 7Li ion induced Coulomb excitation

    Recently the authors observed that the first excited state of 7Li nucleus was excited in 7Li ion-Cu collision in the energy range 4.9 to 11.9 MeV, and the excitation process was via Coulomb excitation. By using the well known B (E2; g.s. 3-/2 - 478 keV, 1-/2) value of 7Li nucleus and the 7Li induced Coulomb excitation yields of both 7Li projectile and targets, the authors determined the reduced transition probabilities for low-lying states of some medium weight nuclei. The reduced transition probabilities determined this way are free from uncertainties due to target thickness and incident particle collection

  1. Excitation and decay of 7Li*(4.63) → α + t in the 7Li(αα1)7Li(4.63) and 9Be(dα1)7Li(4.63) reactions in close kinematic conditions

    Angular correlation function (ACF) of alpha particles and tritons from 7Li* (4.63) decay in the d+9Be → α1+7Li*(4.63) → α1+t+α reaction at deuteron energy Ed=13.6 MeV for escape angles Θαlab=45 and 67 deg has been measured. Results of investigation into the α+7Li → α1+7Li*(4.63) → α1+t+d reaction at Eα=27.2 MeV, Θα1lab=30 deg have been used as well. Kinematic conditions for outlet channels of both reactions are identical. An analytical expression for ACF has been derived. The analysis shows that different mechanisms of the first stage of the d+9Be and α+7Li reactions result in differential phase shifts and limits of summing in the formula for ACF and, therefore, in different ACF form

  2. UV-vis, IR and 1H NMR spectroscopic studies and characterization of ionic-pair crystal violet-oxytetracycline

    Orellana, Sandra; Soto, César; Toral, M. Inés

    2010-01-01

    The present study shows the formation and characterization of the ionic-pair between the antibiotic oxytetracycline and the dye crystal violet in ammonia solution pH 9.0 ± 0.2 extracted into chloroform. The characterization was demonstrated using UV-vis spectrophotometry, 1H NMR, measurement of relaxation times T1 and IR spectroscopy, using a comparison between the signals of individual pure compounds with the signals with the mixture CV-OTC in different alkaline media. The formation of ionic-pair was also corroborated by new signals and chemical shifts. (2D) NMR spectroscopy experiments show that the interaction is electrostatic.

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

    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. PMID:26988489

  4. Molecular structure and spectroscopic analysis of homovanillic acid and its sodium salt - NMR, FT-IR and DFT studies

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

    2014-01-01

    The estimation of the electronic charge distribution in metal complex or salt allows to predict what kind of deformation of the electronic system of ligand would undergo during complexation. It also permits to make more precise interpretation of mechanism by which metals affect the biochemical properties of ligands. The influence of sodium cation on the electronic system of homovanillic acid was studied in this paper. Optimized geometrical structures of studied compounds were calculated by B3LYP/6-311++G** method. Mulliken, MK and ChelpG atomic charges were analyzed. The theoretical NMR and IR spectra were obtained. 1H and 13C NMR as well as FT-IR and FT-Raman spectra of studied compounds were also recorded and analyzed. The calculated parameters are compared with experimental characteristics of these molecules.

  5. Gene synthesis, bacterial expression, and 1H NMR spectroscopic studies of the rat outer mitochondrial membrane cytochrome b5.

    Rivera, M; Barillas-Mury, C; Christensen, K A; Little, J W; Wells, M A; Walker, F A

    1992-12-01

    The gene coding for the water-soluble domain of the outer mitochondrial membrane cytochrome b5 (OM cytochrome b5) from rat liver has been synthetized and expressed in Escherichia coli. The DNA sequence was obtained by back-translating the known amino acid sequence [Lederer, F., Ghrir, R., Guiard, B., Cortial, S., & Ito, A. (1983) Eur. J. Biochem. 132, 95-102]. The recombinant OM cytochrome b5 was characterized by UV-visible, EPR, and 1H NMR spectroscopy. The UV-visible and EPR spectra of the OM cytochrome b5 are almost identical to the ones obtained from the overexpressed rat microsomal cytochrome b5 [Bodman, S. B. V., Schyler, M. A., Jollie, D. R., & Sligar, S. G. (1986) Proc. Natl. Acad. Sci. U.S.A. 83, 9443-9447]. The one-dimensional 1H NMR spectrum of the OM cytochrome b5 indicates that the rhombic perturbation of the ferric center is essentially identical to that in the microsomal beef, rabbit, chicken, and rat cytochromes b5. Two-dimensional 1H NMR spectroscopy (NOESY) and one-dimensional NOE difference spectroscopy were used to assign the contact-shifted resonances that correspond to each of the two isomers that result from the rotation of the heme around its alpha-gamma-meso axis. The assignment of the resonances allowed the determination of the heme orientation ratio in the OM cytochrome b5, which was found to be 1.0 +/- 0.1. It is noteworthy that the two cytochromes b5 that have similar populations of the two heme isomers (large heme disorder) originate from the rat liver. PMID:1333795

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

    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.

  7. Importance of the tensor interaction in the (/sup 7/Li, /sup 7/Be) reaction

    Dodd, A.C.; Clarke, N.M.; Coopersmith, J.; Griffiths, R.J.; Pearce, K.I.; Stanley, B.; Cook, J.

    1985-09-01

    Data for the /sup 28/Si(/sup 7/Li, /sup 7/Be)/sup 28/Al reaction at 72 MeV and for the /sup 26/Mg(/sup 7/Li, /sup 7/Be)/sup 26/Na reaction at 88 MeV are presented together with one-step DWBA calculations using microscopic form factors. The tensor interaction is shown to be important to explain the structureless nature of the angular distributions.

  8. The importance of the tensor interaction in the (7Li, 7Be) reaction

    Data for the 28Si(7Li, 7Be)28Al reaction at 72 MeV and for the 26Mg(7Li, 7Be)26Na reaction at 88 MeV are presented together with one-step DWBA calculations using microscopic form factors. The tensor interaction is shown to be important to explain the structureless nature of the angular distributions. (author)

  9. Elastic scattering of vector polarized 7LiON58Ni

    The elastic scattering of vector polarized 7Li on 58Ni at 20.3 MeV exhibits vector analyzing powers of approximate the same size but of opposite sign as the ones observed for elastic 6Li-58Ni scattering. Present versions of the folding model predict that vector analyzing powers for 7Li should have the same much smaller magnitude than for 6Li scattering. The physical reasons of this observed effect are presently not known. (orig.)

  10. Lines in the spectrum of 7LiH (4728--5298 A)

    The emission spectra of the A1Σ+--X1Σ+ bands of 7LiH were photographed in the 4728A - 5298 A region with a 3.4 meter Ebert Spectrograph of theoretical resolution of about 0.07 cm-1. High purity 7LiH crystals were obtained from Oak Ridge National Laboratory. The atomic percent of 7Li in 7LiH and 7LiD was 99.93 percent. The discharge source was a demountable stainless steel hollow cathode lamp. The lithium hydride crystals were packed into the cathode. Pressure in the discharge tube was about 10 to 20 torr of H2. The discharge was run at about 600 volts and 1.25 to 1.75 amperes. Acceptable spectra were obtained with exposure time of 6 hours. A Westinghouse iron hollow cathode was used to produce the iron spectrum for calibration. The plates were measured on the Gaertner photoplate comparator with an encoder system and on-line computer service at Argonne National Laboratory. The measured lines in the spectra of 7LiH are given in this repot 9COO-2326-19). Similar spectra for 6LiH and 6LiD are given in companion reports (COO-2326-17) and (COO-2326-18), respectively. The relative intensities of the lines are applicable only to short regions and do not extend over the whole spectrum

  11. NMR spectroscopic and densimetric study of reaction kinetics of formaldehyde polymer formation in water, deuterium oxide, and methanol

    Hahnenstein, I.; Albert, M.; Hasse, H.; Kreiter, C.G.; Maurer, G. (Univ. Kaiserslautern (Germany))

    1995-02-01

    In industrial processes, formaldehyde is mainly handled in aqueous solutions, which often contain methanol. In these solutions, formaldehyde forms predominantly adducts with the solvents. In aqueous solutions, methylene glycol and poly(oxymethylene) glycols are formed, in methanolic solutions hemiformal and poly(oxymethylene) hemiformals. As both the formation of poly(oxymethylene) glycol and of poly(oxymethylene) hemiformal are slow compared to typical residence times in separation equipment, reliable information on kinetics of these reactions is essential for process design. Two independent methods were applied to obtain this information: NMR spectroscopy and high-resolution densimetry. The experiments were carried out at temperatures between 273 and 334 K and pH between 2 and 9. Both for poly(oxymethylene) glycol formation and poly(oxymethylene) hemiformal formation, the minimal reaction rate occurs between pH 3 and 5. At 293 K, the inverse rate constant 1/k at this minimum is about 6 min for poly(oxymethylene) glycol formation and about 110 h for poly(oxymethylene) hemiformal formation. The rate constants determined with NMR spectroscopy and densimetry generally agree well. Previously reported discrepancies between results from both methods are explained by the fact that rate constants of poly(oxymethylene) glycol formation depend strongly on the solvent water or deuterium oxide. Reaction kinetics of poly(oxymethylene) glycol and poly(oxymethylene) hemiformal formation in the mixed-solvent system with water and methanol predicted from results obtained in the single-solvent systems are in good agreement with experimental data.

  12. The spectroscopic (FT-IR, FT-Raman, dispersive Raman and NMR) study of ethyl-6-chloronicotinate molecule by combined density functional theory

    Karabacak, Mehmet; Calisir, Zuhre; Kurt, Mustafa; Kose, Etem; Atac, Ahmet

    2016-01-01

    In this study, ethyl-6-chloronicotinate (E-6-ClN) molecule is recorded in the region 4000-400 cm- 1 and 3500-100 cm- 1 (FT-IR, FT-Raman and dispersive Raman, respectively) in the solid phase. 1H and 13C nuclear magnetic resonance (NMR) spectra are recorded in DMSO solution. The structural and spectroscopic data of the molecule are obtained for two possible isomers (S1 and S2) from DFT (B3LYP) with 6-311++G(d,p) basis set calculations. The geometry of the molecule is fully optimized, vibrational spectra are calculated and fundamental vibrations are assigned on the basis of the potential energy distribution (PED) of the vibrational modes. 1H and 13C NMR chemical shifts are calculated by using the gauge-invariant atomic orbital (GIAO) method. The electronic properties, such as excitation energies, oscillator strengths, wavelengths, HOMO and LUMO energies, are performed by time-dependent density functional theory (TD-DFT). Total and partial density of state and overlap population density of state diagrams analysis are presented for E-6-ClN molecule. Furthermore, frontier molecular orbitals (FMO), molecular electrostatic potential, and thermodynamic features are performed. In addition to these, reduced density gradient of the molecule is performed and discussed. As a conclusion, the calculated results are compared with the experimental spectra of the title compound. The results of the calculations are applied to simulate the vibrational spectra of the molecule, which show excellent agreement with the observed ones. The theoretical and tentative results will give us a detailed description of the structural and physicochemical properties of the molecule. Natural bond orbital analysis is done to have more information stability of the molecule arising from charge delocalization, and to reveal the information regarding charge transfer within the molecules.

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

    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.

  14. Application of Spectroscopic Techniques (FT-IR, 13C NMR) to the analysis of humic substances in volcanic soils along an environmental gradient (Tenerife, Canary Islands, Spain)

    Rodriguez Rodriguez, Antonio; María Armas Herrera, Cecilia; González Pérez, José Antonio; González-Vila, Francisco Javier; Arbelo Rodríguez, Carmen Dolores; Mora Hernández, Juan Luis; Polvillo Polo, Oliva

    2010-05-01

    Andosols and andic soils are considered as efficient C-sinks in terms of C sequestration. These soils are usually developed from volcanic materials, and are characterized by a predominance of short-range ordered minerals like allophanes, imogolite and other Fe and Al oxyhydroxides. Such materials occur commonly associated with organic compounds, thus generating highly stable organo-mineral complexes and leading to the accumulation of a high amount of organic carbon. Spectroscopic methods like FT-IR and 13C NMR are suitable for the analysis of the chemical structure of soil humic substances, and allow identifying distinct functional groups and protein, lipids, lignin, carbohydrate-derived fragments. In this work we study the structural features of four soils developed on Pleistocene basaltic lavae in Tenerife (Canary Island, Spain), distributed along an altitudinal climatic gradient. The soil sequence comprises soils with different degree of geochemical evolution and andic character, including a mineral ‘Hypersalic Solonchak' (Tabaibal de Rasca), a slightly vitric ‘Luvic Phaeozem' (Los Frailes), a degraded and shallow ‘Endoleptic, fulvic, silandic Andosol' (Siete Lomas), and a well-developed and deep ‘Fulvic, silandic, Andosol' (Ravelo). Samples of the raw soil and humic and fulvic acids isolated from the surface horizons were analyzed. The results show a low content of organic carbon in the mineral soil, the inherited humin predominating, and a very high content of humic and fulvic acids in Andosols. The FT-IR and 13C NMR spectra of the raw soil samples show a low resolution, related to interferences from mineral complexes signals, particularly in soils with lower organic carbon content. 13C NMR shows a predominance of O-alkyl carbon (derived of carbohydrates) in andic soils, whereas O-alkyl and aromatic fractions are most evident in the mineral soil. The humic acids spectra are characterized by a dominance of alkyl and aromatic fractions with a high degree

  15. Spontaneous Lithium Transportation via LiMn2O4/Electrolyte Interface Studied by 6/7Li Solid-State Nuclear Magnetic Resonance

    Highlights: • Spontaneous Li+ exchange between LiMn2O4 and LiPF6-based electrolyte was studied. • 6/7Li solid-state NMR techniques were developed to examine the exchange. • The exchange occurs for stoichiometric LiMn2O4 but not in Li-excess LiMn2O4. • The exchange was approximated by the 1st-order reaction with the rate of 0.024 min-1. • The suppression in Li-excess LiMn2O4 was ascribed to excess amount of Mn4+. - Abstract: Lithium transportation across the interface of LiMn2O4/LiPF6-based electrolyte was studied by 6/7Li solid-state NMR with 6Li-enriched LiPF6. For almost stoichiometric LiMn2O4, we show that exchange of lithium ions occurs across an electrolyte/electrode interface just by immersing LiMn2O4 powder into LiPF6-based electrolyte, while such transportation is suppressed in Li-excess LiMn2O4. The exchange was approximated by the 1st-order reaction, and the rate was estimated from the 6Li/7Li intensities to be 0.024 min−1 at room temperature. The lithium ions penetrated into the surface of a LiMn2O4 particle reach to the core with a time scale of a few hours at room temperature. The suppression of the exchange in Li-excess LiMn2O4 was ascribed to the presence of excess amount of Mn4+

  16. Spectroscopic (FT-IR, FT-Raman, UV and NMR) investigation on 1-phenyl-2-nitropropene by quantum computational calculations.

    Xavier, S; Periandy, S

    2015-10-01

    In this paper, the spectral analysis of 1-phenyl-2-nitropropene is carried out using the FTIR, FT Raman, FT NMR and UV-Vis spectra of the compound with the help of quantum mechanical computations using ab-initio and density functional theories. The FT-IR (4000-400 cm(-1)) and FT-Raman (4000-100 cm(-1)) spectra were recorded in solid phase, the (1)H and (13)C NMR spectra were recorded in CDCl3 solution phase and the UV-Vis (200-800 nm) spectrum was recorded in ethanol solution phase. The different conformers of the compound and their minimum energies are studied using B3LYP functional with 6-311+G(d,p) basis set and two stable conformers with lowest energy were identified and the same was used for further computations. The computed wavenumbers from different methods are scaled so as to agree with the experimental values and the scaling factors are reported. All the modes of vibrations are assigned and the structure the molecule is analyzed in terms of parameters like bond length, bond angle and dihedral angle predicted by both B3LYP and B3PW91 methods with 6-311+G(d,p) and 6-311++G(d,p) basis sets. The values of dipole moment (μ), polarizability (α) and hyperpolarizability (β) of the molecule are reported, using which the non-linear property of the molecule is discussed. The HOMO-LUMO mappings are reported which reveals the different charge transfer possibilities within the molecule. The isotropic chemical shifts predicted for (1)H and (13)C atoms using gauge invariant atomic orbital (GIAO) theory show good agreement with experimental shifts. NBO analysis is carried out to picture the charge transfer between the localized bonds and lone pairs. The local reactivity of the molecule has been studied using the Fukui function. The thermodynamic properties (heat capacity, entropy and enthalpy) at different temperatures are also calculated. PMID:25965169

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

    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.

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

    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)

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

    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.

  20. NMR spectroscopic analysis reveals extensive binding interactions of complex xyloglucan oligosaccharides with the Cellvibrio japonicus glycoside hydrolase family 31 α-xylosidase.

    Silipo, Alba; Larsbrink, Johan; Marchetti, Roberta; Lanzetta, Rosa; Brumer, Harry; Molinaro, Antonio

    2012-10-15

    The study of the interaction of glycoside hydrolases with their substrates is fundamental to diverse applications in medicine, food and feed production, and biomass-resource utilization. Recent molecular modeling of the α-xylosidase CjXyl31A from the soil saprophyte Cellvibrio japonicus, together with protein crystallography and enzyme-kinetic analysis, has suggested that an appended PA14 protein domain, unique among glycoside hydrolase family 31 members, may confer specificity for large oligosaccharide fragments of the ubiquitous plant polysaccharide xyloglucan (J. Larsbrink, A. Izumi, F.M. Ibatullin, A. Nakhai, H.J. Gilbert, G.J. Davies, H. Brumer, Biochem. J. 2011, 436, 567-580). In the present study, a combination of NMR spectroscopic techniques, including saturation transfer difference (STD) and transfer NOE (TR-NOE) spectroscopy, was used to reveal extensive interactions between CjXyl31A active-site variants and xyloglucan hexa- and heptasaccharides. The data specifically indicate that the enzyme recognizes the entire cello-tetraosyl backbone of the substrate and product in positive enzyme subsites and makes further significant interactions with internal pendant α-(1→6)-linked xylosyl units. As such, the present analysis provides an important rationalization of previous kinetic data on CjXyl31A and unique insight into the role of the PA14 domain, which was not otherwise obtainable by protein crystallography. PMID:22961810

  1. Thermally induced rearrangement of hydrogen-bonded helices in solid 4-isopropylphenol as studied by calorimetric, proton NMR, dielectric and near IR spectroscopic methods

    Wójcik, G.; Szostak, M. M.; Misiaszek, T.; Pająk, Z.; Wąsicki, J.; Kołodziej, H. A.; Freundlich, P.

    1999-11-01

    Calorimetric, dielectric and Fourier transform near infrared (IR) spectroscopic methods were used to study molecular dynamics and structural transition in solid 4-isopropylphenol (4IP) above room temperature. Pulse proton nuclear magnetic resonance (NMR) measurements were performed in the 100-340 K temperature range. A phase transition was found at 331.5 K, 1.5 K below the melting point. Energetically inequivalent methyl groups reorientations were observed in differently prepared samples and this suggested that a high-temperature polymorph occurs below the transition point as a metastable phase. Dielectric relaxation measurements showed an electric conductivity similar in value to that in water. This was detected as a pronounced contribution to the imaginary part of dielectric permittivity at temperatures higher than 310 K. Near IR spectra revealed that hydrogen bondings are stronger in the high-temperature phase than in the room-temperature-stable one. We propose that thermally induced molecular rearrangements enable proton transfer in hydrogen bonds (HBs) and this stimulates protonic conduction.

  2. The importance of having different isotopes in NMR/NQR studies

    One of the powers of Nuclear Magnetic Resonance (NMR) as a spectroscopic tool arises from the fact that each stable element of the periodic table (except for Ar and Tc) has at least one isotope that possesses a nuclear magnetic dipole moment and hence can be employed in a NMR experiment. For the benefit of the researcher, 36 elements have even several magnetic isotopes, e.g. H, Li, B, N, Cl, K, Cu, Xe, Ba. Furthermore, there are 62 elements which possess at least one isotope having a nuclear quadrupole moment and thus, in addition to NMR, allow Nuclear Quadrupole Resonance (NQR) experiments. Given this rich supply of isotopes, no wonder that chemical compounds with different isotopes of the same element, for instance H2O and D2O, play an important role in NMR studies. Well known are the structural investigations in liquids by NMR (high-resolution NMR) where, e.g., hydrogen is replaced by deuterium if a certain bond is of special interest. The hydrogen bond studies in ferroelectrics using also deuterium substitution are a typical example from solid-state physics. In our review, we will present less known but representative examples where the NMR study of two isotopes of the same element yields important information on very different characteristic features of the compound (structure, dynamics etc.). We will discuss the following examples: i) Determination of the type of molecular movements of a transient Xe molecule in the gas phase (by using the Xe isotopes 129 Xe and 131 Xe); ii) Classical nature of the isotope effect of the Li diffusion coefficient in Li metal (7 Li and 6 Li in solid Li); iii) Magnetic and electric origin of spin-lattice relaxation and other quantities in cuprate superconductors 63 Cu and 65 Cu); iv) Isotope shift of the temperature of the opening of the spin gap in the superconductor YBa2Cu4O8 (16 O and 18 O exchanged samples). (author)

  3. Genetically unstable CXG repeats are structurally dynamic and have a high propensity for folding. An NMR and UV spectroscopic study.

    Zheng, M; Huang, X; Smith, G K; Yang, X; Gao, X

    1996-11-29

    Recent molecular genetics studies have revealed a correlation between spontaneous, progressive expansion of several DNA trinucleotide repeats and certain hereditary neurodegenerative diseases. Triplet repeat (TR) sequences may be present in structured forms that can mediate the processes interrupting normal cellular replication, transcription, or repair activities, eventually leading to gene mutation. Using high resolution NMR spectroscopy and other biophysical methods, we probed the solution structures and properties of single-stranded TR sequences. These studies have led to the discovery of a new duplex motif (e-motif), present in CCG repeats, and to the elucidation of the structure of the (CTG)3 duplex. In this paper we provide a global picture of the solution behavior of the human disease-related CXG (X = A, C, G, or T) and the comparison GXC (X = A, or T) TR sequences. All six triplet repeats form antiparallel duplexes. The mismatched bases in CAG and CGG repeat duplexes are rather flexible and they do not appear to form stable, paired conformations. By comparison, GAC repeat duplexes and their mismatched A residues are well-structured. Most interestingly, the structures of the disease-related CXG repeats exhibit a propensity for folding at chain lengths as short as 12 residues. Furthermore, the energy barrier for the formation of homo-duplexes from the corresponding complementary hetero-duplexes are much lower for the CXG TR sequences than for the GAC or GTC TR sequences. These results provide insights into the conformation and physiochemical properties of TR sequences. Thus, a basis is provided for further studies of the behavior of long TR sequences in an effort to elucidate the molecular mechanisms of in vivo expansion and function of TR sequences. PMID:8951379

  4. Reactions (d,7Li) and (d,7Be) in 19F nuclei

    Differential cross sections have been measured for the reactions 19F(d,7Li)14N, 19F(d,7Li(/sub 0.478/)14N, 19F(d,7Be)14C, and 19F(d,7Be(/sub 0.429/)14C in a cyclotron beam of deuterons with energy 13.6 MeV. The experimental data were analyzed by the distorted-wave method with inclusion of the finite interaction range and recoil. It is shown that the reactiuns 19F(d,7Li)14N and 19F(d,7Li(/sub 0.478/)14N occur mainly by direct transfer of a 5He cluster from the 4P/sub 1/2/ state of the 19F nucleus to the 1D/sub 3/2/ state of the 7Li nucleus. The differential cross sections for the reactions 19F(d,7Be)14C and 19F(d,7Be(/sub 0.429/)14C could not be explained in terms of the theory of direct transfer of a 5Li cluster

  5. Global optical model potentials for symmetrical lithium systems: 6Li+6Li, 7Li+7Li at Elab = 5-40 MeV

    Angular distributions of 6Li+6Li elastic scattering were measured for Elab=5-40 MeV. An optical model analysis of these data together with older data of 7Li+7Li elastic scattering taken at Elab = 8-17 MeV was performed with the aim to search for a ''global'' OM potential which describes elastic scattering in both Li-Li systems in a broad energy range. Both surface and volume absorbing potentials can be found which fulfill this requirement if a linear energy dependence is assumed of the depths of the real as well as the imaginary potential. These depths, if fitted to individual angular distributions, are found to vary in a correlated manner with the beam energy. This is taken as indication of strong coupling between elastic, inelastic, and reaction channels. This is corroborated by the existence of resonances in reaction channels at these energies where the potential depths are most pronouncedly changing. (orig.)

  6. Space distributions and decay probability for excited state of 7Li*(7,45 MeV) in reaction 7Li(alpha, alpha6Li)n

    Differential cross-sections of excitation and decay of 7Li*(7,45 MeV) resonance into 6Li + n channel in three particle reaction 7Li(alpha, alpha6Li)n at alpha-particle energy of 27,2 MeV have been determined in kinematically complete and incomplete experiments. Usage of position sensitive detector made it possible to obtain the data on space distributions of decay events for full range of possible angles and to determine the total probability of this process, which value essentially differs from the data for binary reactions. This result is agreed with previously obtained [1] and confirms the theoretical calculations [2] of decay branching ratio for short lived near-threshold resonances in three particle reactions

  7. Study on the differential cross sections of the (d, 7Li)-reactions on 13C nuclei

    Differential cross sections of 13C(d, 7Li)8Be and 13C(d, sup(7)Li*sub(0.478))sup(8)Be on 13.6 MeV deuteron cyclotron beam using the ΔExE technique to identify reaction products, in which silicon ΔE detectors, of approximately 5 mk thickness were applied, have been measured. Experimental data have been analyzed according to the Hauser- Feshbach statistical theory and in the approximation of distorted waves with account for finitude of interaction and recoil radius. It is shown that angular distributions of 7Li and sup(7)Li*sub(0.478) ions are described most satisfactorily in the approximation of direct transfer of 5He quasicluster from 2Dsub(1/2) state of 13C nucleus into 2Ssub(3/2) state of 7Li, sup(7)Li*sub(0.478) nuclei

  8. The automatic NMR gaussmeter

    The paper describes the automatic gaussmeter operating according to the principle of nuclear magnetic resonance. There have been discussed the operating principle, the block diagram and operating parameters of the meter. It can be applied to measurements of induction in electromagnets of wide-line radio-spectrometers EPR and NMR and in calibration stands of magnetic induction values. Frequency range of an autodyne oscillator from 0,6 up to 86 MHz for protons is corresponding to the field range from 0.016 up to 2T. Applicaton of other nuclei, such as 7Li and 2D is also foreseen. The induction measurement is carried over automatically, and the NMR signal and value of measured induction are displayed on a monitor screen. (author)

  9. Global optical-model potentials for the elastic scattering of sup(6,7)Li projectiles

    Simultaneous fits have been made to 44 6Li data sets covering the mass range 24-208 and the energy range 13-156 MeV in order to determine an average ('global') optical-model potential for 6Li scattering. A similar study has been made for 25 7Li data sets over the same mass range and an energy range of 28-88 MeV to find an average 7Li potential. With Saxon-Woods factors, constant values may be used for all parameters except for the depth of the imaginary potential which decreases in magnitude with increasing mass. The necessity of energy dependence, Coulomb correction and (for 7Li) a symmetry term is investigated. The variation of the integral properties of the potentials is discussed, and also a comparison is made for the two projectiles. Application of the global potentials is made to inelastic scattering and single-nucleon transfer reactions. (orig.)

  10. 7Li(3He,p)9Be reaction and primordial nucleosynthesis

    The differential cross section for the 7Li(3He, p)9Be reaction has been measured in 50 keV intervals at 8 angles (15deg-160deg) in the energy range from Ec.m.=0.5 to 2.0 MeV, and total cross sections were determined from these data. Since this reaction has been noted as being of possible importance in primordial nucleosynthesis, its astrophysical S-factor was calculated from the data. In addition, the S-factor for the 7Li(3H, n)9Be reaction, also of importance in primordial nucleosynthesis, was estimated from the 7Li(3He, p)9Be data and its thermonuclear reaction rate was calculated. (orig.)

  11. Study of fusion in 6,7Li+197Au near barrier energies

    Excitation functions are measured for complete fusion and transfer reactions of 6Li and 7Li with 197Au at energies around the Coulomb barrier. Coupled channel calculations including the couplings to both target and projectile excited states have been performed and are found to explain the data at energies below the barrier. At above barrier energies the complete fusion cross sections are found to be suppressed compared to the coupled channel calculations for both the systems. A systematic comparison of fusion cross-section for halo nuclei 6,8He and weakly bound stable nuclei 6,7Li on 197Au target is also presented. Large neutron transfer cross-sections are observed for 6,7Li as compared to tightly bound projectiles 12C,16O. (authors)

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

    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.

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

    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.

  14. Search for a resonant enhancement of the 7Be + d reaction and primordial 7Li abundances

    Big Bang nucleosynthesis calculations, constrained by the Wilkinson Microwave Anisotropy Probe results, produce 7Li abundances almost a factor of four larger than those extrapolated from observations. Since primordial 7Li is believed to be mostly produced by the beta decay of 7Be, one proposed solution to this discrepancy is a resonant enhancement of the 7Be(d,p)2α reaction rate through the 5/2+ 16.7-MeV state in 9B. The 2H(7Be,d)7Be reaction was used to search for such a resonance; none was observed. An upper limit on the width of the proposed resonance was deduced.

  15. Determination of degradation constants of energetic 7*Li ion in liquid media using a thin boron film on silicon wafer

    A novel method to determine degradation constants has been developed for energetic 7*Li ions produced from the 10B (n, α) 7*Li reaction, moving in liquid media. The energetic 7*Li generated in a thin boron film on silicon wafer plunged into a liquid sample in which the wafer was immersed. The degradation constants were determined by analyzing the Doppler-broadened lineshapes of prompt γ-ray at 478 keV emitted from 7*Li. For comparison, degradation constants were also measured for solutions of boron compounds. Values obtained by the two methods gave fair agreement. (author)

  16. In vivo 31P NMR spectroscopic assessment of the endurance and recovery capacity of skeletal muscle: Comparison between the sedentaries and canoe athletes

    In vivo 3P NMR spectroscopic study of forearm wrist flexor muscles was performed in two groups of volunteers composed respectively of 6 sedentaries and 6 canoe athletes. A continuous isometric contraction of endurance exercise was adopted in order to assess the endurance capacity and recovery potential of skeletal muscles. Differences in high energy phosphorus metabolism between the sedentaries and athletes were evaluated with and emphasis on the intracellular pH and Pi/PCr ratio as indicators of high energy phosphorus metabolism, There were no differences of baseline pH and Pi/ PCr ratio between the two groups. The athletes sustained the exercise at a more acidic intracellular pH and at a higher Pi/ PCr radio of intracellular conditions for an all out than did the sedentaries. The recovery rate of pH showed no difference between the two groups. There was a tendency of faster recovery of Pi/ PCr in athletes showing half recovery time (T1/2) of 39.0 ± 3.0 seconds as compared to that of sedentaries (55.7 ± 7.5 seconds). The recovery rate of Pi/ PCr as a function of Pi/ PCr rate at a given period of time was significantly faster in athletes than in sedentaries (P<0.001). The correlation coefficient of the recovery rate of Pi/ PCr against the Pi/ PCr ratio was 0.985 and 0.914 respectively for the athletes and sedentaries. The pH and the Pi/ PCr ratio at an all-out state can be used as indicators of endurance capacity and the recovery rate of Pi/ PCr, as a recovery potential of skeletal muscles

  17. Constraints on Ωb from nucleosynthesis of 7Li in the standard big bang model

    We update standard big bang nucleosynthesis (SBBN) calculations on the basis of recent nuclear physics compilations (NACRE in particular), experimental and theoretical works. By a Monte Carlo technique, we calculate the uncertainties on the light element yields (4He, D, 3He and 7Li) related to nuclear reactions. The results are compared to observations that are thought to be representative of the corresponding primordial abundances. It is found that 7Li could lead to more stringent constraints on the baryonic density of the universe (Ωbh2) than deuterium, because of much higher observation statistics and an easier extrapolation to primordial values. The confrontation of SBBN results with 7Li observations is of special interest since other independent approaches have also recently provided Ωbh2 values: (i) the anisotropies of the cosmic microwave background by the BOOMERANG, CBI, DASI and MAXIMA experiments and (ii) the Lyman-α forest at high redshift. A comparison between these results obtained by different methods provides a test of their consistency and could provide a better determination of the baryonic density in the universe. However, the agreement between Ωbh2 values deduced from SBBN calculation and 7Li observation on the one hand and CMB observations on the other hand is only marginal

  18. THE NEW DETECTIONS OF 7Li/6Li ISOTOPIC RATIO IN THE INTERSTELLAR MEDIA

    We have determined the isotopic abundance ratio of 7Li/6Li in the interstellar media (ISMs) along lines of sight to HD169454 and HD250290 using the High-Dispersion Spectrograph on the Subaru Telescope. We also observed ζ Oph for comparison with previous data. The observed abundance ratios were 7Li/6Li = 8.1+3.6-1.8 and 6.3+3.0-1.7 for HD169454 and HD250290, respectively. These values are in reasonable agreement with those observed previously in the solar neighborhood ISMs within ±2σ error bars and are also consistent with our measurement of 7Li/6Li = 7.1+2.9-1.6 for a cloud along the line of sight to ζ Oph. This is good evidence for homogeneous mixing and instantaneous recycling of the gas component in the Galactic disk. We also discuss several source compositions of 7Li, Galactic cosmic-ray interactions, stellar nucleosynthesis, and big bang nucleosynthesis.

  19. Design of a 7Li rotating target for neutron production using a Van de Graaff accelerator

    We present a rotating target used for the production of monokinetic neutron fluxes. The neutrons are produced from the 7Li(p,n)7Be reaction for fast neutron elastic and inelastic scattering experiments. This target has been operated with a proton beam current of 8 to 10 μA during six consecutive weeks and has given entire satisfaction

  20. Push-through Direction Injectin NMR Automation

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

  1. 7Li nuclear magnetic resonance studies of dynamics in a ternary gel polymer electrolyte based on polymeric ionic liquids

    The influence of the polymeric ionic liquid (PIL) Poly(diallyldimethylammonium bis(trifluoromethylsulfonyl) imide) (PDADMATFSI) on the lithium dynamics was investigated in a ternary gel polymer electrolyte consisting of PDADMATFSI as stabilizing polymer, ionic liquid (1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl) imide, P14TFSI) and lithium salt (lithium bis(trifluoromethylsulfonyl) imide, LiTFSI). The diffusion coefficient of the lithium ions is investigated by pulsed-field-gradient NMR, the conductivity of the electrolyte is determined by impedance spectroscopy. The local lithium dynamics is characterized by 7Li spin lattice relaxation rates (R1). The relaxation rates are well described by Blombergen-Purcell-Pound (BPP) theory at all polymer concentrations (up to 45 mol%), implying that the Li dynamics is governed by one single motional mode. Interestingly, activation energies for this motion decrease from 20 kJ/mol to 15 kJ/mol with increasing polymer content and are independent on the salt content. We thus conclude that the polymer is interacting with the anion coordination shell, which is accompanied by a very beneficial effect on the local lithium dynamics, as the polymer PDADMATFSI reduces the Li-TFSI interactions. This result is promising for further investigations for potential use of PDADMATFSI-containing gels as electrolytes in energy storage devices

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

    Monakhova, Yulia B; Godelmann, Rolf; Hermann, Armin; Kuballa, Thomas; Cannet, Claire; Schäfer, Hartmut; Spraul, Manfred; Rutledge, Douglas N

    2014-06-23

    It is known that (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 (1)H NMR profiles are fused with stable isotope (SNIF-NMR, (18)O, (13)C) data. Variable selection based on clustering of latent variables was performed on (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 (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 (1)H NMR data alone in 82-89% respectively). Certain enhancement was obtained also for the year of vintage (from 88 to 97% for (1)H NMR to 99% for the fused data), whereas in case of grape varieties improved models were not obtained. The combination of (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. PMID:24909771

  3. In situ 7Li and 133Cs Nuclear Magnetic Resonance Investigations on the Role of Cs+ Additive in Lithium-Metal Deposition Process

    Hu, Jian Z.; Zhao, Zhenchao; Hu, Mary Y.; Feng, Ju; Deng, Xuchu; Chen, Xilin; Xu, Wu; Liu, Jun; Zhang, Jiguang

    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.

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

    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.

  5. Revisiting the 7Li(p,n)7Be reaction near threshold

    In this work we review all the available experimental neutron data for the 7Li(p,n) reaction near threshold which is necessary to obtain an accurate source model for Monte Carlo simulations in Boron Neutron Capture Therapy. Scattered published experimental results such as cross sections, differential neutron yields and total yields were collected and analyzed, exploring the sensitivity of the fitting parameters to the different possible variables and deriving a consistent working set of parameters to evaluate the neutron source near threshold. - Highlights: • We review neutron experimental data for the 7Li(p,n) reaction near threshold. • A new computational method was used to study all the available published data. • A consistent description of the neutron source was derived fitting the available data. • We found that the neutron yield at 0° studied by Kononov is the most sensitive curve. • A consistent set of parameters to parametrize the Breit–Wigner formula is presented

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

    Exclusive measurements of prompt γ-rays from the heavy-residues with various light charged particles in the 7Li + 198Pt system, at an energy near the Coulomb barrier (E/Vb∼1.6) are reported. Recent dynamic classical trajectory calculations, constrained by the measured fusion, α- 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 α clusters; whereas for 6He+p and 5He+d configurations, massive transfer is inferred to be the dominant mechanism. The present work clearly demonstrates the role played by the cluster structures of 7Li in understanding the reaction dynamics at energies around the Coulomb barrier.

  7. Excitation of continuum states in sup 7 Li and their decay by quantum tunneling

    Utsunomiya, H; Yamagata, T; Ohta, M; Aoki, Y; Hirota, K; Ieki, K; Iwata, Y; Katori, K; Hamada, S; Lui, Y W; Schmitt, R P; Typel, S; Baur, G

    1999-01-01

    Strong forward-backward asymmetries were found in the recent alpha-t coincidence measurement of Coulomb breakup of 42 MeV- sup 7 Li via continuum states. The competition between E1 and E2 multipolarities and higher order effects in Coulomb excitation were investigated by solving the time-dependent Schroedinger equation. It is shown that higher order effects are an essential ingredient to the observed large asymmetries. The relevant reaction mechanism is discussed.

  8. Exploring Light Neutron Rich Nuclei via the (7Li,7Be) Reaction

    A systematic study of the nuclei that can be described as an integer number of α particles plus three neutrons via the (7Li,7Be) reaction at about 8 MeV/u has shown the presence of Bound States Embedded in the Continuum in the energy spectra. These are experimental signatures of the dynamical correlations of an easily polarizable core with a single-particle state of the valence neutron.

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

    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. 7Li neutron-induced elastic scattering cross section measurement using a slowing-down spectrometer

    Heusch M.; Ghetta V.; Chabod S.; Brissot R.; Billebaud A.; Méplan O.; Kessedjian G.; Liatard E.

    2010-01-01

    A new integral measurement of the 7Li neutron induced elastic scattering cross section was determined in a wide neutron energy range. The measurement was performed on the LPSC-PEREN experimental facility using a heterogeneous graphite-LiF slowing-down time spectrometer coupled with an intense pulsed neutron generator (GENEPI-2). This method allows the measurement of the integral elastic scattering cross section in a slowing-down neutron spectrum. A Bayesian approach coupled to Monte Carlo cal...

  11. An update on the big bang nucleosynthesis prediction for 7Li: the problem worsens

    The lithium problem arises from the significant discrepancy between the primordial 7Li abundance as predicted by big bang nucleosynthesis (BBN) theory and the Wilkinson Microwave Anisotropy Probe (WMAP) baryon density, and the pre-Galactic lithium abundance inferred from observations of metal-poor (Population II) stars. This problem has loomed for the past decade, with a persistent discrepancy of a factor of 2–3 in 7Li/H. Recent developments have sharpened all aspects of the Li problem. Namely: (1) BBN theory predictions have sharpened due to new nuclear data; in particular, the uncertainty on the reaction rate for3He(α,γ)7Be has reduced to 7.4%, nearly a factor of 2 tighter than previous determinations. (2) The WMAP five-year data set now yields a cosmic baryon density with an uncertainty reduced to 2.7%. (3) Observations of metal-poor stars have tested for systematic effects. With these, we now find that the BBN+WMAP predicts7Li/H = (5.24−0.67+0.71) × 10−10. The central value represents an increase by 23%, most of which is due to the upward shift in the3He(α,γ)7Be rate. More significant is the reduction in the7Li/H uncertainty by almost a factor of 2, tracking the reduction in the3He(α,γ)7Be error bar. These changes exacerbate the Li problem; the discrepancy is now a factor 2.4 or 4.2σ (from globular cluster stars) to 4.3 or 5.3σ (from halo field stars). Possible resolutions to the lithium problem are briefly reviewed, and key experimental and astronomical measurements highlighted

  12. 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

    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.

  13. The 3H(α,γ)7Li reaction at low energies

    The 3H(α,γ) reaction, and its mirror 3He(α,γ) are responsible for 7Li production in the big bang. Discrepancies between experimental data sets, as well as differences between the experimental and theoretical energy dependences, cause the 3H(α,γ)7Li cross section to be uncertain by as much as a factor of two at the relevant astrophysical energies (Ec.m. ∼ 100 keV). The authors report new measurements for 50 c.m. 3H targets and an 85% high-purity germanium detector. Angular distributions were measured at nine energies between 115 and 1200 kev. The astrophysical S-factor is observed to increase moderately with decreasing energy to S(0) ∼ 0.10 keV-b. The branching ratio for captures to the first excited state and ground state of 7Li is found to be ∼0.44, independent of energy. The results are compared to previous experiments and theoretical calculations

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

    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...

  15. Electron affinity of (7)Li calculated with the inclusion of nuclear motion and relativistic corrections.

    Stanke, Monika; Kedziera, Dariusz; Bubin, Sergiy; Adamowicz, Ludwik

    2007-10-01

    Explicitly correlated Gaussian functions have been used to perform very accurate variational calculations for the ground states of (7)Li and (7)Li(-). The nuclear motion has been explicitly included in the calculations (i.e., they have been done without assuming the Born-Oppenheimer (BO) approximation). An approach based on the analytical energy gradient calculated with respect to the Gaussian exponential parameters was employed. This led to a noticeable improvement of the previously determined variational upper bound to the nonrelativistic energy of Li(-). The Li energy obtained in the calculations matches those of the most accurate results obtained with Hylleraas functions. The finite-mass (non-BO) wave functions were used to calculate the alpha(2) relativistic corrections (alpha=1c). With those corrections and the alpha(3) and alpha(4) corrections taken from Pachucki and Komasa [J. Chem. Phys. 125, 204304 (2006)], the electron affinity (EA) of (7)Li was determined. It agrees very well with the most recent experimental EA. PMID:17919011

  16. Systematic model-dependent behaviour of fusion involving weakly bound projectiles 6,7Li

    Many measurements on complete fusion (CF) cross section at above barrier energies involving weakly bound stable projectiles (e.g., 6Li, 7Li and 9Be) show suppression by various degrees compared to theoretical estimates as well as experimental CF cross sections of reactions involving strongly bound projectiles. However, there is no concrete picture at sub-barrier energies. The conclusions based on coupled-channels (CC) calculations using different codes (e.g., FRESCO or CCFULL) may differ as the theoretical models used to calculate fusion are not same. In a recent paper on complete fusion in 7Li+152Sm system, the fusion cross sections calculated by CCFULL and FRESCO have been shown to be different despite using same bare potential. It was observed that with the inclusion of only inelastic couplings, the results of FRESCO were much closer to the experimental data in the above barrier region, while the CCFULL results overpredict the data over the entire range. To explore the above observation in different systems involving 6,7Li as projectile, in the present work, a systematic and detailed study has been carried out by means of CC calculations using both FRESCO and CCFULL. The aim is to analyze the differences between the two models of calculations

  17. Probing the fusion of 7Li with 64Ni at near-barrier energies

    Shaikh, Md. Moin; Roy, Subinit; Rajbanshi, S.; Mukherjee, A.; Pradhan, M. K.; Basu, P.; Nanal, V.; Pal, S.; Shrivastava, A.; Saha, S.; Pillay, R. G.

    2016-04-01

    Background: The stable isotopes of Li, 6Li6 and 7Li, have two-body cluster structures of α +d and α +t with α -separation energies or breakup thresholds at 1.47 and 2.47 MeV, respectively. The weak binding of these projectiles introduces several new reaction channels not usually observed in the case of strongly bound projectiles. The impact of these breakup or breakup-like reaction channels on fusion, the dominant reaction process at near-barrier energies, with different target masses is of current interest. Purpose: Our purpose is to explore the fusion, at above and below the Coulmb barrier, of 7Li with 64Ni target in order to understand the effect of breakup or breakup-like processes with medium-mass target in comparison with 6Li, which has a lower breakup threshold. Measurement: The total fusion (TF) excitation of the weakly bound projectile 7Li with the medium-mass target 64Ni has been measured at the near-barrier energies (0.8 to 2 VB). The measurement was performed using the online characteristic γ -ray detection method. The complete fusion (CF) excitation function for the system was obtained using the x n -evaporation channels with the help of statistical model predictions. Results: At the above barrier energies CF cross sections exhibit an average suppression of about 6.5% compared to the one-dimensional barrier penetration model (1DBPM) predictions, while the model describes the measured TF cross section well. But below the barrier, both TF and CF show enhancements compared to 1DBPM predictions. Unlike 6Li, enhancement of CF for 7Li could not be explained by inelastic coupling alone. Conclusion: Whereas the σTF cross sections are almost the same for both the systems in the above barrier region, the suppression of σCF at above the barrier is less for the 7Li+64Ni system than for the 6+64Ni system. Also direct cluster transfer has been identified as the probable source for producing large enhancement in TF cross sections.

  18. NMR study of starch based polymer gel electrolytes: Humidity effects

    In this work, nuclear magnetic resonance spectroscopy (NMR) was used to study the effect of water absorption in polymer gel electrolytes formed by amylopectin rich starch, plasticized with glycerol and containing lithium perchlorate. The position of the 7Li spin-lattice relaxation rate maximum is shifted progressively towards lower temperatures with increasing hydration, reflecting an increase of the lithium mobility. The mechanism responsible for the spin-lattice relaxation of the 7Li nuclei in the gel electrolytes are the fluctuations of the quadrupolar interaction due to the lithium motions. The 7Li relaxation results of the gel electrolyte hydrated with 2.2 water per complex unit suggest that the lithium ions are almost decoupled from the polymer chain and coordinate, hence preferring the water molecules

  19. Use of {sup 7}Li(p,n) reaction as a neutron source in a PGNAA setup

    Naqvi, A.A. [Department of Physics, King Fahd University of Petroleum and Minerals, Box No. 1815, Dhahran 31261 (Saudi Arabia)]. E-mail: aanaqvi@kfupm.edu.sa; Nagadi, M.M. [Department of Physics, King Fahd University of Petroleum and Minerals, Box No. 1815, Dhahran 31261 (Saudi Arabia)

    2005-03-01

    The performance of a {sup 7}Li(p,n) reaction-based Prompt Gamma Ray Neutron Activation Analysis (PGNAA) setup has been determined for analysis of Portland cement samples using Monte Carlo study. The calculations were carried out for a {sup 7}Li(p,n) reaction-based PGNAA setup with an external moderator similar to the one used in a previous 2.8 MeV neutrons-based PGNAA setup. The optimum values of geometry parameters of the {sup 7}Li(p,n) reaction-based setup are different from those of the 2.8 MeV neutrons-based setup resulting in better performance of the {sup 7}Li(p,n) reaction-based setup. The prompt {gamma}-ray yield from the {sup 7}Li(p,n) reaction-based setup is 60-70% higher than that from the 2.8 MeV neutrons-based setup. Although the performances of the {sup 7}Li(p,n) reaction-based setup is comparable with that of a previously studied {sup 3}H(p,n) reaction-based setup, yet performance of the {sup 7}Li(p,n) reaction-based setup is superior to that of the {sup 3}H(p,n) reaction-based setup because it has less radiation hazard due to utilization of non-radioactive neutron producing target. This study has provided a theoretical base for experimental test of a {sup 7}Li(p,n) reaction-based PGNAA setup.

  20. Sequence variations of in vitro pUC18 plasmid DNA induced by high energy 7Li ion beams implantation

    High energy heavy ion beams is a new mutagen for crop mutation breeding, but limited data are available on the molecular level induced by this mutagen. The in vitro pUC18 plasmid DNA was implanted by 7Li ion beams by doses of 0, 20, 40, 60, 80 and 100Gy, respectively, with the energy of 42.3Mev. The results showed that the damage effects induced by 7Li ion beams implantation was different from low LET rays, even low doses of 7Li ion beam could induce high damage on hydrogen bonds. Percentage of damages on hydrogen bonds of in vitro DNA induced by 7Li ion beams implantation increased with dosage increase up to 40Gy, then reduced with dosage increase, and higher than those of gamma rays in the same dosage. The relationship of dosage and damage percentage was different from that of gamma rays which was positive-linear correlation. Mutation frequency of 7Li ion beam implantation was 1.6 to 4.3 times to that of spontaneous mutation. The relationship of mutation frequency and dosage was similar with that of damage effects on hydrogen bonds, and showed a peak at 40Gy. The above results were identical with biological effects of wheat implanted by 7Li ion beams. Ten mutants were used for sequence analysis, which indicated that the types of base changes included base transversion, transition and deletion. Among all base changes detected, the frequency of bases transition (60%) was higher than that of bases transversion (30%) and bases deletion (10%). It seemed that thymine was more sensitive to the implantation than any other bases and base changes were mainly T→C and C→T. Bases between T and C were seemed to be easily induced by 7Li ion beams. The high percentage of DNA sequence variations could explain primarily the biological effects caused by 7Li ion beams in the M1 generation of crops. (author)

  1. Implanted $^{7}$Be Targets For The Study of Neutron Interactions With $^{7}$Be : (The "Primordial $^{7}$Li Problem")

    The disagreement of the predicted abundance of primordial $^{7}$Li with the observed abundance is a longstanding problem in Big Bang Nucleosynthesis (BBN) theory (“Primordial $^{7}$Li problem”). While BBN theory correctly predicts the relative abundances of $^{2}$H/$^{1}$H, $^{3}$He/$^{1}$H and $^{4}$He/$^{1}$H (that vary over four orders of magnitudes), but it over-predicts the relative abundance of primordial $^{7}$Li/$^{1}$H by a factor of approximately 3-4 larger than observed (approximately 4-5$\\sigma$ discrepancy). Primordial $^{7}$Li is destroyed during the first 15 minutes primarily via the $^{7}$Li(p,$\\alpha$) reaction. Hence most of the primordial $^7$Li is predicted as the result of the (later when atoms are formed) electron capture $\\beta$-decay of the primordial $^{7}$Be that is produced primarily in the $^{3}$He($\\alpha$,$\\gamma$) )$^{7}$Be reaction. We propose to investigate the direct destruction of $^{7}$Be during (the first 15 minutes of) BBN via the $^{7}$Be(n,$\\alpha$) reaction to ch...

  2. Isoxazole derivatives of alpha-pinene isomers: Synthesis, crystal structure, spectroscopic characterization (FT-IR/NMR/GC-MS) and DFT studies

    Eryılmaz, Serpil; Gül, Melek; İnkaya, Ersin; Taş, Murat

    2016-03-01

    In this paper, the alpha-pinene isoxazole derivatives (3a-b-c, 4a-b) were synthesized via 1,3-dipolar cycloaddition and characterized with FT-IR, 1H NMR, 13C NMR and GC-MS. Isoxazole (C21H23NO) compound (4a) 6,6,7a,-trimethyl-3-(naphthalen-2-yl)-3a,4,5,6,7,7a-hexahydro-5,7-methanobenzo[d] was characterized by X-ray single crystal diffraction technique. The compound crystallizes in the monoclinic space group P 212121, with Z = 4. The molecular geometry of the compound was optimized by applying Density Functional Theory (DFT/B3LYP) method with 6-31G(d,p) and 6-311 + G(d,p) basis sets in the ground state and geometric parameters were compared with the X-ray analysis results of the structure. Results of the experimental FT-IR and NMR spectral analysis were examined in order to determine the compliance with vibrational frequencies, 1H NMR and 13C NMR chemical shifts values by using the Gauge-Independent Atomic Orbital (GIAO) method calculated over the optimized structure. Besides molecular electrostatic potential (MEP), frontier molecular orbitals (FMOs), some global reactivity descriptors, thermodynamic properties, non-linear optical (NLO) behaviour and Mulliken charge analysis of the (4a) compound were computed with the same method in gas phase, theoretically.

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

    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.

  4. Phenomenological and microscopic optical potentials for 88 MeV 7Li scattering

    The elastic scattering cross sections for 88 MeV 7Li ions have been measured for targets of 2426Mg and 4048Ca. Analyses using both phenomenological and microscopic optical potentials provide information on the energy dependence of optical parameters, and the extent to which the potentials are determined for these light ions. The use of a double-folding microscopic model demonstrates the need for normalisation of the real potential by a factor of 0.5 in contrast to measurements at lower energies. The contribution of exchange effects, density dependence and break-up are discussed. (author)

  5. Mechanochemical and solution synthesis, X-ray structure and IR and 31P solid state NMR spectroscopic studies of copper(I) thiocyanate adducts with bulky monodentate tertiary phosphine ligands.

    Bowmaker, Graham A; Hanna, John V; Hart, Robert D; Healy, Peter C; King, Scott P; Marchetti, Fabio; Pettinari, Claudio; Skelton, Brian W; Tabacaru, Aurel; White, Allan H

    2012-07-01

    A number of adducts of copper(I) thiocyanate with bulky tertiary phosphine ligands, and some nitrogen-base solvates, were synthesized and structurally and spectroscopically characterised. CuSCN:PCy3 (1:2), as crystallized from pyridine, is shown by a single crystal X-ray study to be a one-dimensional polymer ...(Cy3P)2CuSCN(Cy3P)2CuSCN... (1) with the four-coordinate copper atoms linked end-on by S-SCN-N bridging thiocyanate groups. A second form (2), obtained from acetonitrile, was also identified and shown by IR and 31P CPMAS NMR spectroscopy to be mononuclear, with the magnitude of the dν(Cu) parameter measured from the 31P CPMAS and the ν(CN) value from the IR clearly establishing this compound as three-coordinate [(Cy3P)2CuNCS]. Two further CuSCN/PCy3 compounds CuSCN:PCy3 (1:1) (3), and CuSCN:PCy3:py (1:1:1) (4) were also characterized spectroscopically, with the dν(Cu) parameters indicating three- and four-coordinate copper sites, respectively. Attempts to obtain a 1:2 adduct with tri-t-butylphosphine have yielded, from pyridine, the 1:1 adduct as a dimer [(Bu(t)3P)((SCN)(NCS))Cu(PBu(t)3)] (5), while similar attempts with tri-o-tolylphosphine (from acetonitrile and pyridine (= L)) resulted in solvated 1:1:1 CuSCN:P(o-tol)3:L forms as dimeric [{(o-tol)3P}LCu((SCN)(NCS))CuL{P(o-tol)3}] (6 and 8). The solvent-free 1:1 CuSCN:P(o-tol)3 adduct (7), obtained by desolvation of 6, was characterized spectroscopically and dν(Cu) measurements from the 31P CPMAS NMR data are consistent with the decrease in coordination number of the copper atom from four (for 6) (P,N(MeCN)Cu,S,N) to three (for 7) (PCuS,N) upon loss of the acetonitrile of solvation. These results are compared with those previously reported for mononuclear and binuclear PPh3 adducts which demonstrate a clear tendency for the copper centre to remain four-coordinate. The IR spectroscopic measurements on these compounds show that bands in the far-IR spectra provide a much more definitive criterion for

  6. Extremely slow cation exchange processes in Li4SiO4 probed directly by two-time 7Li stimulated-echo nuclear magnetic resonance spectroscopy

    Lithium self-diffusion in the low-temperature modification of polycrystalline lithium ortho-silicate Li4SiO4 is investigated by 7Li two-time stimulated echo NMR spectroscopy. Extremely slow Li exchange processes were directly monitored between 300 and 433 K by recording spin-alignment echoes as a function of mixing time varying over six decades from 10-5 to 10 s. In the investigated temperature range the hopping correlation functions show biexponential behaviour. Whereas the first decay step reflects directly Li jumps between electrically different sites, the second one is simply induced by the decay of alignment order due to quadrupolar relaxation. The echo decay rates τ-1 (101 s-1≤τ-1≤104 s-1), which can be identified with Li jump rates, show Arrhenius behaviour with an activation energy of 0.53(1) eV. The directly measured jump rates are in good agreement with those obtained recently by one- and two-dimensional 6Li exchange MAS NMR reported in the literature

  7. Synthesis, structural, and spectroscopic (FT-IR, NMR, and UV) Characterization of 1-(Cyclohexylmethyl)-2-(pyridin-2-yl)-1 H-benzo[ d]imidazole by experimental techniques and quantum chemical calculations

    Özdemir, Namık; Dayan, Osman; Demirmen, Selin

    2016-05-01

    The title compound ( II), 1-(cyclohexylmethyl)-2-(pyridin-2-yl)-1 H-benzo[ d]imidazole (C19H21N3), was synthesized via N-alkylation of 2-(pyridin-2-yl)-1 H-benzo[ d]imidazole ( I). Both compounds I and II were characterized by IR, NMR and UV-vis spectroscopy. Solid-state structure of compound II was determined by single-crystal X-ray diffraction technique. Furthermore, quantum chemical calculations employing density functional theory (DFT/B3LYP) method with the 6-311++ G( d, p) basis set were performed for the theoretical characterization of the molecular and spectroscopic features of the compounds. Using the TD-DFT method, electronic absorption spectra of the compounds have been predicted at same level. When the obtained results were compared with the experimental findings, it is seen that theoretical results support the experimental data and a good agreement exists between them.

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

    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…

  9. Total kinetic energy distribution of fission fragments in 6,7Li + 238U reactions

    The shape and width of fission-fragment (FF) mass and kinetic energy distribution provides a lot of information on the fission reaction mechanism and the structure of the compound nucleus (CN), the fragments as well as the interacting nuclei. The shape of the mass distribution of the fission fragments for the actinides induced by the proton or neutron is known to change with the incident energy. At low energies, it shows a double humped distribution which changes slowly to a single humped distribution as energy increases. However, for a reaction involving a weakly bound projectile (i.e., 6Li + 232Th), a sharp change in the shape of the mass distribution with energy was observed. The sharp increase in the peak to valley ratio (P:V) in the fission-fragment mass distribution in 6Li + 232Th reaction by Itkis et al. and in 6,7Li + 238U reactions by Santra et al. was concluded to be due to the reduced energy transfer to the composite system caused by incomplete fusion (ICF) of alpha or deuteron/triton followed by fissions. Total Kinetic Energy (TKE) distribution of fission fragments is another important observable on which the effect of projectile breakup is not explored yet. In this contribution, the study of breakup/transfer effect on average TKE distribution for 6,7Li + 238U reactions is presented

  10. Monte Carlo modelling of a TLD device containing 7LiF:Mg,Cu,P detectors

    The Monte Carlo code MCNP-4C2 is used to design a new personal thermoluminescence dosemeter that assesses both Hp(10) and Hp(0.07) in mixed photon/electron fields. The new dosemeter utilizes two 7LiF:Mg,Cu,P elements contained within a Harshaw TLD-700H card, itself inside a polypropylene holder with walls 2 mm thick. Several potential designs of holder are considered; the best incorporates a polytetrafluoroethylene cylinder of diameter 18 mm and thickness 4.3 mm that acts as a filter to provide the correct electron cut-off and an acceptably flat Hp(10) relative response to photons, with an open hole in front of the Hp(0.07) element. Response characteristics for both detectors in this final design are presented for irradiation from a variety of angles of interest, with source energies between 16 and 6174 keV used. Comparison is made between modelled and measured data at normal incidence; the relative responses generally agree well. A new estimate for the relative light conversion efficiency relevant to the 7LiF:Mg,Cu,P is also derived and presented

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

    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

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

    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.

  13. One pot synthesis, molecular structure and spectroscopic studies (X-ray, IR, NMR, UV-Vis) of novel 2-(4,6-dimethoxy-1,3,5-triazin-2-yl) amino acid ester derivatives

    El-Faham, Ayman; Soliman, Saied M.; Osman, Sameh M.; Ghabbour, Hazem A.; Siddiqui, Mohammed R. H.; Fun, Hoong-Kun; Albericio, Fernando

    2016-04-01

    Novel series of 2-(4,6-dimethoxy,1,3,5-triazin-2-yl) amino acid ester derivatives were synthesized using simple one pot method in methanol. The products were obtained in high yields and purities as observed from their spectral data, elemental analyses, GC-MS and X-ray crystallographic analysis. The B3LYP/6-311G(d,p) calculated molecular structures are well correlated with the geometrical parameters obtained from the X-ray analyses. The spectroscopic properties such as IR vibrational modes, NMR chemical shifts and UV-Vis electronic transitions were discussed both experimentally and theoretically. The IR vibrational frequencies showed good correlations with the experimental data (R2 = 0.9961-0.9995). The electronic spectra were assigned based on the TD-DFT results. Intense electronic transition band is calculated at 198.1 nm (f = 0.1389), 204.2 nm (f = 0.2053), 205.0 (f = 0.1704) and 205.7 (0.2971) for compounds 6a-i, respectively. The molecular orbital energy levels contributed in the longest wavelength transition band were explained. For all compounds, the experimental wavelengths showed red shifts compared to the calculations due to the solvent effect. The NMR chemical shifts were calculated using GIAO method. The NBO analyses were performed to predict the stabilization energies due to the electron delocalization processes occur in the studied systems.

  14. One pot synthesis, molecular structure and spectroscopic studies (X-ray, IR, NMR, UV-Vis) of novel 2-(4,6-dimethoxy-1,3,5-triazin-2-yl) amino acid ester derivatives.

    El-Faham, Ayman; Soliman, Saied M; Osman, Sameh M; Ghabbour, Hazem A; Siddiqui, Mohammed R H; Fun, Hoong-Kun; Albericio, Fernando

    2016-04-15

    Novel series of 2-(4,6-dimethoxy,1,3,5-triazin-2-yl) amino acid ester derivatives were synthesized using simple one pot method in methanol. The products were obtained in high yields and purities as observed from their spectral data, elemental analyses, GC-MS and X-ray crystallographic analysis. The B3LYP/6-311G(d,p) calculated molecular structures are well correlated with the geometrical parameters obtained from the X-ray analyses. The spectroscopic properties such as IR vibrational modes, NMR chemical shifts and UV-Vis electronic transitions were discussed both experimentally and theoretically. The IR vibrational frequencies showed good correlations with the experimental data (R(2)=0.9961-0.9995). The electronic spectra were assigned based on the TD-DFT results. Intense electronic transition band is calculated at 198.1 nm (f=0.1389), 204.2 nm (f=0.2053), 205.0 (f=0.1704) and 205.7 (0.2971) for compounds 6a-i, respectively. The molecular orbital energy levels contributed in the longest wavelength transition band were explained. For all compounds, the experimental wavelengths showed red shifts compared to the calculations due to the solvent effect. The NMR chemical shifts were calculated using GIAO method. The NBO analyses were performed to predict the stabilization energies due to the electron delocalization processes occur in the studied systems. PMID:26845586

  15. A novel strategy for site-directed chemical reactions in single stranded DNA--absorption and NMR spectroscopic studies of model compounds.

    Asseline, U; Rozelle, T; Lancelot, G; Thuong, N T

    1992-01-01

    A new and simple model enabling a chemical species to be brought to a preselected site in single strand DNA is reported. Two oligonucleotides containing a propanediol linkage were hybridized to their complementary sequences with an extra-base opposite the propanediol derivative. Absorption studies results shown that the addition of a bisacridine derivative strongly increased the stabilities of both duplexes when added in a 1:1 ratio. NMR studies on one of these duplexes brought evidence of th...

  16. NMR Spectroscopic Analysis on the Chiral Recognition of Noradrenaline by β-Cyclodextrin ( β-CD) and Carboxymethyl- β-cyclodextrin (CM- β-CD)

    β-CD and CM-β-CD as chiral NMR shift agents were used to resolve the enantiomers of noradrenaline (NA). The stoichiometry of each complex formed between the CDs and the enantiomers of NA was found to be 1 : 1 through the continuous variation plots. The binding constants (K) of the complexes were determined from 1H NMR titration curves. This result indicated that both β-CD and CM-β-CD formed the complexes with the S (+)-NA more preferentially than its R(.)-enantiomer. The K values for the complexes with β-CD (KS(+) = 537 M-1 and KR(-) = 516 M-1) was larger than those with CM-β-CD (KS(+) = 435 M-1 and KR(-) = 313 M-1), however, enantioselectivity (α) of S(+)- and R(-)-NA to CM-β-CD (α = 1.38) was larger than that to β-CD (α = 1.04), indicating that CM-β-CD was the better chiral NMR solvating agents for the recognition of the enantiomers of NA. Two dimensional rotating frame nuclear Overhauser enhancement spectroscopy (ROESY) experiments were also performed to explain the binding properties in terms of spatial fitting of the NA molecule into the macrocyclic cavities

  17. Study of the reactions 9Be (d, a0) 7Li, 9Be (d, a1) 7Li*, 9Be (dt)8Be and 9Be (dp0) 10Be from 300 to 1000 keV

    We present the excitation curves, the angular distributions and the total cross-sections for the reactions: 9Be (d α0)7Li, 9Be (d α1)7Li, 9Be (d, t)8Be, 9Be (dp0)10Be, in the energy range from 300 keV to 1 MeV. Our results are in good agreement with the few studies already carried out. In order that the results be presented in absolute values, we have normalized them with those of BIGGERSTAFF. (author)

  18. Study of the {sup 7}Li (p,{alpha}){sup 4}He Reaction at Astrophysical Energies Through the Trojan Horse Method

    Pellegriti, M.G.; Aliotta, M.; Cherubini, S.; Lattuada, M.; Miljanic, D.; Pizzone, R.G.; Romano, S.; Soic, N.; Spitaleri, C.; Zadro, M.; Zappala, R.A.

    2000-12-31

    The Trojan Horse Method has been applied to obtain information about {sup 7}Li(p,{alpha}),{sup 4}He reaction at astrophysical energies. The {sup 7}Li(d,{alpha} n){sup 4}He reaction has been used and the two body reaction cross section for the {sup 7}Li(p,{alpha}){sup 4}He has been extracted together with its astrophysical factor S(E).

  19. Experiment and theory for the reaction 7Li(γ,t)4He for E/sub γ/<50 MeV

    Differential and total cross sections for the 7Li(γ,t)4He reaction were measured. Both real and virtual photons were used in the experiment and gave self-consistent results. The data show a broad resonance indicating the presence of positive parity states near 8 MeV excitation in 7Li. A calculation using an α-3H cluster model of 7Li was also performed. Poor agreement is found between the calculation and experimental results

  20. Covariance analysis of n + 7Li data for ENDF/B-VI

    A new covariance analysis of n/plus/7Li experimental data has been completed for Version VI of ENDFB. The analysis basically updates our 1981 work for ENDFB-V.2 to include new data that has become available since that time and to incorporate cross correlations between different experiments. The bulk of the new measured data consists of some 10 new (or newly revised) tritium-production measurements involving about 70 new data points. The new analysis results in only small changes in the previous evaluation of the tritium-production cross section but significantly reduces the magnitudes of uncertainties due to the more extensive and accurate data base that was used

  1. New method to evaluate the 7Li(p, n)7Be reaction near threshold

    In this work a complete description of the 7Li(p, n)7Be 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

  2. Charge and mass distribution in 7Li induced fission of 232Th

    Formation cross sections of about forty fission products have been determined using recoil catcher technique followed by off line gamma-ray spectrometry in 7Li induced fission of 232Th at Elab=41.9, 36.6 and 31.4 MeV. The measured data have been used to deduce charge and mass distributions. Mass distribution is found to be asymmetric at all the three energies. Cross sections of evaporation residues formed in both transfer reactions (232,233,234Pa) as well as in complete fusion (234Np), have also been measured. The measured evaporation residue cross sections and the decay probabilities of target like nuclei (233,234,235Pa) formed in the various transfer reactions, as calculated by PACE2, have been used to estimate the transfer induced fission cross sections. The data indicated that the magnitude of transfer induced fission is very small

  3. Beam shaping assembly optimization for 7Li(p,n)7Be accelerator based BNCT

    Within the framework of accelerator-based BNCT, a project to develop a folded Tandem-ElectroStatic-Quadrupole accelerator is under way at the Atomic Energy Commission of Argentina. The proposed accelerator is conceived to deliver a proton beam of 30 mA at about 2.5 MeV. In this work we explore a Beam Shaping Assembly (BSA) design based on the 7Li(p,n)7Be neutron production reaction to obtain neutron beams to treat deep seated tumors. - Highlights: • A Beam Shaping Assembly for accelerator based BNCT has been designed. • A conical port for easy patient positioning and the cooling system are included. • Several configurations can deliver tumor doses greater than 55 RBEGy. • Good tumor doses can be obtained in less than 60 min of irradiation time

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

    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. (authors)

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

    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.

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

    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. PMID:26393239

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

    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. PMID:27506162

  8. 19F NMR spectroscopic and relaxation studies of SbF5 and AsF5 intercalated in graphite, graphite fibers, and polyacetylene

    19F NMR spectra are presented for graphite powder reacted with SbF5, NOSbF6, NO2SbF6, graphite fibers reacted with AsF5, and polyacetylene reacted with NOSbF6 and with AsF5. For polyacetylene the linewidths imply rapid rotation and slow diffusion. For the other specimens linewidths imply that both rotation and diffusion are rapid. For SbF5 in graphite an activation enthalpy of 5+-1 kcal/mol is deduced from the observed T1 behavior. (orig.)

  9. The reaction 7Li(e,3H)4He,e' between 6 and 15 MeV

    Tritons resulting from the electrodisintegration of 7Li have been measured at 90 deg for an incident electron energy of 23.8 MeV over an energy range which ensured that only tritons emitted in the two-body channel were detected. The electrodisintegration cross sections were converted to equivalent photodisintegration data and compared to earlier results. Large discrepancies are observed. It is found that the (γ,3H) channel contributes appreciably to the electric dipole sum rule for 7Li. (author)

  10. Rate of 3H(7Li,n0)9Be and big-bang nucleosynthesis

    The differential cross sections for the 3H(7Li,n0)9Be reaction measured at 5 angles in the energy range E(c.m.)=0.2-0.9 MeV using a pulsed 7Li beam and time-of-flight technique. Absolute values of the cross section were obtained by comparison with the well-known cross section of 3H(d,n)4He at Ed=1.0 MeV. The resulting reaction rates are obtained at temperatures relevant to big-bang nucleosynthesis, and consequences for primordial 9Be abundances are discussed. (orig.)

  11. Asymptotic and near-target direct breakup of 6Li and 7Li

    Kalkal, Sunil; Simpson, E. C.; Luong, D. H.; Cook, K. J.; Dasgupta, M.; Hinde, D. J.; Carter, I. P.; Jeung, D. Y.; Mohanto, G.; Palshetkar, C. S.; Prasad, E.; Rafferty, D. C.; Simenel, C.; Vo-Phuoc, K.; Williams, E.; Gasques, L. R.; Gomes, P. R. S.; Linares, R.

    2016-04-01

    Background: Li,76 and 9Be are weakly bound against breakup into their cluster constituents. Breakup location is important for determining the role of breakup in above-barrier complete fusion suppression. Recent works have pointed out that experimental observables can be used to separate near-target and asymptotic breakup. Purpose: Our purpose is to distinguish near-target and asymptotic direct breakup of Li,76 in reactions with nuclei in different mass regions. Method: Charged particle coincidence measurements are carried out with pulsed Li,76 beams on 58Ni and 64Zn targets at sub-barrier energies and compared with previous measurements using 208Pb and 209Bi targets. A detector array providing a large angular coverage is used, along with time-of-flight information to give definitive particle identification of the direct breakup fragments. Results: In interactions of 6Li with 58Ni and 64Zn, direct breakup occurs only asymptotically far away from the target. However, in interactions with 208Pb and 209Bi, near-target breakup occurs in addition to asymptotic breakup. Direct breakup of 7Li into α -t is not observed in interactions with 58Ni and 64Zn. However, near-target dominated direct breakup was observed in measurements with 208Pb and 209Bi. A modified version of the Monte Carlo classical trajectory model code platypus, which explicitly takes into account lifetimes associated with unbound states, is used to simulate sub-barrier breakup reactions. Conclusions: Near-target breakup in interactions with Li,76 is an important mechanism only for the heavy targets 208Pb and 209Bi. There is insignificant near-target direct breakup of 6Li and no direct breakup of 7Li in reactions with 58Ni and 64Zn. Therefore, direct breakup is unlikely to suppress the above-barrier fusion cross section in reactions of Li,76 with 58Ni and 64Zn nuclei.

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

    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 (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.

  13. NMR Studies of Lithium Iodide Based Solid Electrolytes

    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...

  14. Solid-state 51V NMR and infrared spectroscopic study of vanadium oxide supported on TiO2ZrO2

    Vanadium oxide catalyst supported on TiO2-ZrO2 has been prepared by adding Ti(OH)4-Zr(OH)4 powder to an aqueous solution of ammonium metavanadate followed by drying and calcining at high temperatures. The characterization of the prepared catalysts was performed using solid-state 51V NMR and FTIR. In the case of calcination temperature at 773 K, vanadium oxide was in a highly dispersed state for the samples containing low loading V2O5 below 25 wt %, but for samples containing high loading V2O5 equal to or above 25 wt %, vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of TiO2-ZrO2. The ZrV2O7 compound was formed through the reaction of V2O5 and ZrO2 at 773-973 K, whereas the V3Ti6O17 compound was formed through the reaction of V2O5 and TiO2 at 973-1073 K. The V3Ti6O17 compound decomposed to V2O5 and TiO2 at TiO2 at 1173 K, which were confirmed by FTR and 51V NMR

  15. Solid-state 51V NMR and infrared spectroscopic study of vanadium oxide supported on ZrO2-WO3

    Vanadium oxide catalyst supported on ZrO2-WO3 was prepared by adding the Zr(OH)4 powder into a mixed aqueous solution of ammonium metavanadate and ammonium metatungstate followed by drying and calcining at high temperatures. The characterization of prepared catalysts was performed using solid-state 51V NMR and FTIR. In the case of calcination temperature at 773 K, for the samples containing low loading V2O5 below 18 wt % vanadium oxide was in a highly dispersed state, while for samples containing high loading V2O5 equal to or above 18 wt % vanadium oxide was well crystallized due to the V2O5 loading exceeding the formation of monolayer on the surface of ZrO2-WO3. The ZrV2O7 compound was formed through the reaction of V2O5 and ZrO2 at 873 K and the compound decomposed into V2O5 and ZrO2 at 1073 K, which were confirmed by FTIR and 51V NMR

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

    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.

  17. Elemental and structural analysis of silicon forms in herbal drugs using silicon-29 MAS NMR and WD-XRF spectroscopic methods.

    Pajchel, L; Nykiel, P; Kolodziejski, W

    2011-12-01

    The objective of this work was to study concentration of silicon and its structural forms present in herbal drugs. Equisetum arvense and Urtica dioica L. from teapot bags, dietary supplements (tablets and capsules) containing those herbs, dry extract obtained from a teapot bag of E. arvense, and samples of the latter herb harvested in wild habitat over four months were studied using wavelength dispersive X-ray spectroscopy (WD-XRF) and high-resolution solid-state (29)Si NMR. The highest concentration of Si, ca. 27mg/g, was found in the herbal material from the teapot bags containing E. arvense. The Si content in natural E. arvense (whole plants) increased from May to August by ca. 7mg/g, reaching value 26mg/g. Three different silicon forms were detected in the studied herbal samples: Si(OSi)4 (Q(4)), Si(OH)(OSi)3 (Q(3)) and Si(OH)2(OSi)2 (Q(2)). Those sites were populated in E. arvense in the following order: Q(4)≫Q(3)>Q(2). A dramatic, ca. 50-fold decrease of the Si concentration during the infusion process was observed. The infusion process and the subsequent drying procedure augmented population of the Q(4) sites at the cost of the Q(2) sites. The WD-XRF and (29)Si NMR methods occurred useful and complementary in the study of herbal materials. PMID:21813258

  18. Post mortem energy metabolism and meat quality of porcine M. longissimus dorsi as influenced by stunning method - A (31)P NMR spectroscopic study.

    Bertram, Hanne Christine; Stødkilde-Jørgensen, Hans; Karlsson, Anders Hans; Andersen, Henrik Jørgen

    2002-09-01

    Post mortem changes in phosphorus metabolites and pH were studied in M. longissimus dorsi from pigs (n=10) stunned either by CO(2) (n=3), electrical (n=2), captive bolt pistol (n=2) or by anesthesia (ketamine) (n=3). (31)P-NMR spectroscopy revealed significant effects of stunning method on changes of the various phosphorus metabolites in the muscle post mortem, with the effect being most pronounced on the degradation of phosphocreatine (PCr). Moreover, the four stunning methods gave rise to large differences in the progress of pH as determined by (31)P-NMR spectroscopy. Using anesthesia as the reference showed that the captive bolt pistol caused the highest rates of post mortem degradation of phosphorus metabolites, electrical stunning intermediate, and CO(2)-stunning causing the lowest post mortem degradation rates, even though CO(2)-stunning also was associated with higher post mortem degradation rates compared with anesthesia. Finally, it was demonstrated that the water-holding capacity (WHC) of the meat was affected by the applied stunning method, as CO(2)-stunning, electrical stunning and captive bolt pistol resulted in mean drip losses of 6.4, 8.3 and 8.6%, respectively (P=0.02). The result displays the significance of induction and progress in post mortem changes on WHC in meat. PMID:22061199

  19. Organometallic derivatives of furan. LII. Synthesis of carbofunctional furylsilanes and their 1H, 13C, and 29Si NMR spectroscopic and quantum-chemical investigation

    Under the standard conditions for the synthesis of furan compounds it is possible to obtain the carbofunctional derivatives of silylated furfural with retention of the trimethylsilyl group in the ring. By NMR and CNDO/2 LCAO MO methods and also as a result of the investigation of the chemical characteristics of silylated furfural and its carbofunctional derivatives it was established that the introduction of a trimethylsilyl group at position 5 of the furan ring does not change the reactivity of the carbofunctional substituents at position 2. The electronic effects of the substituents are hardly transmitted through the furan ring at all. The effect of substituents in the carbofunctional furylsilanes on the electronic structure of the ring is additive

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

    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...... 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...

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

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

    2013-05-01

    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 1H and 13C NMR spectra were recorded and the chemical shifts of the molecule were calculated.

  2. Spectroscopic (FT-IR, FT-Raman, FT-NMR and UV-Vis) investigation on benzil dioxime using quantum computational methods

    Bakkiyaraj, D.; Periandy, S.; Xavier, S.

    2016-03-01

    The spectral analysis of benzil dioxime is carried out using the FTIR, FT Raman, FT NMR and UV-Vis spectra of the compound with the help of quantum computations by density functional theories. The FT-IR (4000 - 400 cm-1) and FT-Raman (4000-100 cm-1) spectra are recorded in solid phase, the 1H and 13C NMR spectra in DMSO phase and the UV spectrum (200-400 nm) in ethanol phase. The different conformers of the compound and their minimum energies are studied by potential energy surface scan, using semi-empirical method PM6. The computed wavenumbers from different methods are scaled so as to agree with the experimental values and the scaling factors are reported. All the fundamental modes have been assigned based on the potential energy distribution (PED) values and the structure the molecule is analyzed interms of parameters like bond length, bond angle and dihedral angles predicted byB3LYP and CAM-B3LYP methods with cc-pVDZ basis sets. The values of dipole moment (μ), polarizability (α) and hyperpolarizability (β) of the molecule are reported, using which the non -linear optical property of the molecule is discussed. The HOMO-LUMO mappings are reported which reveals the different charge transfer possibilities within the molecule. The isotropic chemical shifts predicted for 1H and 13C atoms using gauge invariant atomic orbital (GIAO) theory show good agreement with experimental shifts and the same is discussed in comparison with atomic charges, predicted by Mullikan and APT charge analysis. NBO analysis is carried out to picture the probable electronic transitions in the molecule.

  3. The value of B(E2;3/2- → 1/2-) for 7Li

    Previous experimental information from the Coulomb excitation of the 1/2- first excited state of 7Li is discussed and reanalysed, giving B(E2;3/2- → 1/2-) = 7.59 ± 0.10e2fm4. 28 refs., 3 tabs., 1 fig

  4. The α-continuum from the interaction of 70 MeV polarized 7Li with 54Fe

    The first- and second-rank analysing powers were measured for the α-particle continuum from the interaction of 70 MeV polarized 7Li with 54Fe. The data are consistent with a partial fusion reaction mechanism as the dominant process and can be described by a semiclassical model of analysing powers in transfer reactions. (author)

  5. On the hyperfine structures of the ground state(s) in the ${}^{6}$Li and ${}^{7}$Li atoms

    Frolov, Alexei M

    2016-01-01

    Hyperfine structure of the ground $2^{2}S-$states of the three-electron atoms and ions is investigated. By using our recent numerical values for the doublet electron density at the atomic nucleus we determine the hyperfine structure of the ground (doublet) $2^{2}S-$state(s) in the ${}^{6}$Li and ${}^{7}$Li atoms.

  6. About the reactions 3H(alpha,gamma)7Li and 3He(alpha,gamma)7Be

    In this article the current experimental and theoretical status of the radiative alpha capture reactions 3H(α,γ)7Li and 3He(α,γ)7Be and their relations to primordial nucleosynthesis and the solar neutrino problem are reviewed. (author)

  7. NMR and impedance studies of nanocrystalline and amorphous ion conductors: lithium niobate as a model system.

    Heitjans, Paul; Masoud, Muayad; Feldhoff, Armin; Wilkening, Martin

    2007-01-01

    Lithium niobate has been chosen as a model system for spectroscopic studies of the influence of different structural forms and preparation routes of an ionic conductor on its ion transport properties. The Li diffusivity in nanocrystalline LiNbO3, prepared either mechanically by high energy ball milling or chemically by a sol-gel route, was studied by means of impedance and solid state 7Li NMR spectroscopy. The Li diffusivity turned out to be strongly correlated with the different grain boundary microstructures of the two nanocrystalline samples and with the degree of disorder introduced during preparation, as seen especially by HRTEM and EXAFS. Although in both samples nanostructuring yields an enhancement of the Li diffusivity compared to that in coarse grained LiNbO3, the Li diffusivity in ball milled LiNbO3 is much higher than in chemically prepared nanocrystalline LiNbO3. The former LiNbO3 sample has a large volume fraction of highly disordered interfacial regions which seem to be responsible for fast Li diffusion and to have a structure very similar to that of the amorphous form. This is in contrast to the chemically prepared sample where these regions have a smaller volume fraction. PMID:17326563

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

    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

  9. Formation of ultracold (7)Li(85)Rb molecules in the lowest triplet electronic state by photoassociation and their detection by ionization spectroscopy.

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

    2015-03-21

    We report the formation of ultracold (7)Li(85)Rb molecules in the a(3)Σ(+) 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 (7)Li 2s (2)S1/2 + (85)Rb 5p (2)P1/2 asymptote. In addition, we use REMPI spectroscopy to probe the a(3)Σ(+) state and excited electronic 3(3)Π and 4(3)Σ(+) states and identify a(3)Σ(+) (v″ = 7-13), 3(3)Π (vΠ' = 0-10), and 4(3)Σ(+) (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. PMID:25796252

  10. 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

    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.)

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

    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.

  12. Stepwise substitution of Μ3-Te ligands in octahedral cluster core (Re6Te8)2+: NMR spectroscopic evidence of equilibrium between chemical forms

    High-temperature reactions of the (Re6Te8)Te7 rhenium telluride with elementary sulfur and selenium, leading to formation of substitution solid solutions of the (Re6Te8-xYx)Te7 type, where by Y=S, Se,; 0≤x≤8, are studied. Complex salts of the K4(Re6Te8-xYx)(CN)6 compositions, preserving the cluster nucleus of the source compounds, are synthesized through interaction of the (Re6Te8-xYx)Te7 solid phases with the KCN melt. The salts water solutions are studied through the NMR spectroscopy method on 77Se and 125Te nuclei. Complex spectra for various composition samples are obtained. The additive model applied adequately describes the NMP spectra for all studied samples. The conclusion is made on the basis of the data obtained that the (Re6Te8-xYx)Te7 phases with certain x-values contain practically the set of different chemical forms (with different values), whereby quantitative ratios between them are determined by corresponding equilibrium constants

  13. In Vitro Monitoring of Total Choline Levels in a Bioartificial Pancreas: 1H NMR Spectroscopic Studies of the Effects of Oxygen Level

    Long, Robert C.; Papas, Klearchos K.; Sambanis, Athanassios; Constantinidis, Ioannis

    2000-09-01

    This investigation implements specifically designed solvent-suppressed adiabatic pulses whose properties make possible the long-term monitoring of 1H NMR detectable metabolites from alginate/poly-l-lysine/alginate (APA)-encapsulated βTC3 cells. Our encapsulated preparations were maintained in a perfusion bioreactor for periods exceeding 30 days. During this prolonged cultivation period, the cells were exposed to repetitive hypoxic episodes of 4 and 24 h. The ratio of the total choline signal (3.20 ppm) to the reference signal (observed at 0.94 ppm assigned to isoleucine, leucine, and valine) decreased by 8-10% for the 4-h and by 20-32% for the 24-h episodes and returned to its prehypoxic level upon reoxygenation. The decrease in the mean value of total choline to reference signal ratio for three 4-h and two 24-h episodes in two different cultures was highly significant (P metabolism are suggested. In addition, the implications of these findings to the development of a noninvasive monitoring method for tissue-engineered constructs composed of encapsulated cells are discussed.

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

    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.

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

    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.

  16. 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

    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...

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

    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.

  18. Spectroscopic (FT-IR, FT-Raman, 1H- and 13C-NMR), theoretical and microbiological study of trans o-coumaric acid and alkali metal o-coumarates.

    Kowczyk-Sadowy, Małgorzata; Świsłocka, Renata; Lewandowska, Hanna; Piekut, Jolanta; Lewandowski, Włodzimierz

    2015-01-01

    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. PMID:25689641

  19. Search for solar axions emitted in the M1-transition of 7Li* with Borexino CTF

    Results of background measurements with a prototype of the Borexino detector were used to search for 478 keV solar axions emitted in the M1-transitions of 7Li*. The Compton conversion of axion to a photon A+e→e+γ, axioelectric effect A+e+Z→e+Z, decay of axion in two photons A→2γ and Primakoff conversion on nuclei A+Z→γ+Z are considered. The upper limit on constants of interaction of axion with electrons, photons and nucleons -gAegAN≤(1.0-2.4) x 10-10 at mA≤450 keV and gAγgAN≤5 x 10-9 GeV-1 at mA≤10 keV are obtained (90%c.l.). For heavy axions with mass at 100AAe-8 and gAγ-9-10-8 are obtained in assumption that gAN depends on mA as for KSVZ axion model. These limits are stronger than obtained in previous laboratory-based experiments using nuclear reactor and artificial radioactive sources. (orig.)

  20. Thick target neutron yields for the 7Li(p,n)7Be reaction near threshold

    Transportable accelerator sources of epithermal neutrons are crucial for the development of hospital-based boron neutron capture therapy (BNCT) as a treatment modality for brain cancers. One method for producing such epithermal neutrons is near-threshold (p,n) reactions as studied by our group, as well as several other investigators. As part of this effort, we have developed accurate methods for computing the angular distributions and energy spectra of neutrons from thick targets using the 7Li(p,n)7Be reaction near threshold. Neutron yields are calculated for lithium metal as well as several lithium compounds of low molecular weight. The calculational method is discussed, with emphasis on the improvements over previously published methods. Neutron energy spectra, angular distributions, and total yields for proton beam energies up to 120 keV above threshold are presented. A method is also demonstrated for calculating neutron yields for targets that are not sufficiently thick to slow protons past the reaction threshold

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

    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.

  2. Coherent photoproduction of π0- and η-mesons off 7Li

    Coherent photoproduction of π0-mesons from threshold (Eth ∼ 136 MeV) throughout the Δ-resonance region and of η-mesons close to the production threshold (Eth ∼ 570 MeV) for η has been measured for 7Li 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 π 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 η production had been only identified for the lightest nuclear systems (2H and 3He). For 3He 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 η production agree with a plane-wave approximation. Contrary to 3He, 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.)

  3. NMR and conductivity study of PEO-based composite polymer electrolytes

    The influence of the space charge created by the presence of TiO2 nanoparticles on the lithium and polymer chain mobility have been investigated in solid composite polymer electrolytes (CPE), poly(ethylene oxide) (PEO) LiClO4, by using complex impedance spectroscopy and nuclear magnetic resonance (NMR). Special care was taken with the synthesis and the characterization of the TiO2 particles and with the composite preparation. The conductivity and NMR measurements were undertaken in composite samples nanoparticles having constant total surface area. Proton (1H) and lithium (7Li) lineshapes and spin-lattice relaxation times were measured as a function of temperature. Activation energies extracted from the 7Li relaxation data are in the range 0.20-0.22 eV. The NMR decoupling experiment suggests that the Li-Li interactions are stronger in the composites when compared with those of the ceramic free electrolytes

  4. The 10B(n,α0)7Li and 10B(n,αlγ)7Li alpha-particle angular distributions, branching ratios and cross-sections measurements for En < 3 MeV

    Hambsch, F. J.; Ruskov, I.; Vidali, M.

    2010-01-01

    The 10B(n,α0)7Li and 10B(n,αiγ)7Li angular distributions have been measured at the GELINA time-of-flight spectrometer in the incident neutron energy range from 0.1 keV to 1 MeV by means of a twin Frisch-grid ionization chamber. With this type of detector it is possible to measure the angular distribution of the charged reaction fragments in a close to 2×2π solid angle with ~100% efficiency and a clear separation of both reaction channels: emission to the 7Li ground state (α0) or to its first excited state (α1). A strong angular anisotropy was observed at ~ 520 keV. In order to extend the energy range up to 2.5-3 MeV and to measure, also, the reaction cross sections, a double twin Frisch-grid ionization chamber was constructed. It is loaded with two very thin 94% 10B-enriched samples, mounted back-to-back with 235U samples on the common cathodes. New data acquisition, visualization and analysis software is used in a new set of long-term measurements, which are still going on.

  5. The 10B(n,α0)7Li and 10B(n,αlγ)7Li alpha-particle angular distributions, branching ratios and cross-sections measurements for En < 3 MeV

    The 10B(n,α0)7Li and 10B(n,αiγ)7Li angular distributions have been measured at the GELINA time-of-flight spectrometer in the incident neutron energy range from 0.1 keV to 1 MeV by means of a twin Frisch-grid ionization chamber. With this type of detector it is possible to measure the angular distribution of the charged reaction fragments in a close to 2x2π solid angle with ∼100% efficiency and a clear separation of both reaction channels: emission to the 7Li ground state (α0) or to its first excited state (α1). A strong angular anisotropy was observed at ∼ 520 keV. In order to extend the energy range up to 2.5-3 MeV and to measure, also, the reaction cross sections, a double twin Frisch-grid ionization chamber was constructed. It is loaded with two very thin 94% 10B-enriched samples, mounted back-to-back with 235U samples on the common cathodes. New data acquisition, visualization and analysis software is used in a new set of long-term measurements, which are still going on.

  6. Signal Processing for Spectroscopic Applications

    Gudmundson, Erik

    2010-01-01

    Spectroscopic techniques allow for studies of materials and organisms on the atomic and molecular level. Examples of such techniques are nuclear magnetic resonance (NMR) spectroscopy—one of the principal techniques to obtain physical, chemical, electronic and structural information about molecules—and magnetic resonance imaging (MRI)—an important medical imaging technique for, e.g., visualization of the internal structure of the human body. The less well-known spectroscopic technique of nucle...

  7. Spin and parity determinations of excited 15N based on polarized and unpolarized 12C(7Li, α)15N reaction data at E lab = 34 MeV

    From an experiment conducted at the Florida State University Accelerator Laboratory with a 34 MeV polarized 7Li beam bombarding a 12C target, we have obtained angular distributions and analyzing powers for states of 15N up to 20 MeV in excitation energy. This study not only offers the possibility to assign spin and parity to several states in 15N, but also serves to obtain nuclear potential parameters used in Distorted Wave Born (DWBA) and Coupled Channel Born (CCBA) Approximations to generate theoretical angular distributions and vector analyzing powers that give the best description of the experimental data. Under the assumption that the reaction mechanism is a three nucleon transfer, the determination of shell model nucleonic configurations and spectroscopic factors is possible for the 15N states studied

  8. Fission products yield in the neutron-induced fission of 232Th using neutrons source from 7Li( p, n)7Be reaction at incident proton energy of 20 MeV

    This paper presents the measurement of fission product yields from the neutron induced fission of 232Th. These measurements were carried out using the neutron source from 7Li (p,n) reaction at TIFR-BARC Pelletron facility. The yields were obtained using activation and off-line gamma ray spectroscopic technique. The fission yields values are reported for twelve fission products. Activated targets were counted in highly shielded HPGe detectors over a period of several weeks to identify decaying fission products. The results obtained from the present work were compared with the similar data of mono-energetic neutrons of comparable energy from literature and are found to be in good agreement

  9. Simultaneous description of CF, ICF and TF data of 6,7Li + 209Bi reaction using new ICF mode

    The systematic behavior of the fusion suppression factors and ICF probability as a function of target mass is not well understood, despite the CF experimental data being available for a number of projectile-target systems. In our recent paper, a new method was proposed to calculate the ICF probability which is based on absorption cross sections obtained from the CDCC calculations. In continuation of this work, we have also carried out similar calculations for 6,7Li + 209Bi where the experimental data of CF and ICF is available. In the recent paper by Marta et al., the semi-classical model calculations were attempted to understand CF and ICF data for 6,7Li + 209Bi, which was not explaining the data quite well. Here, we have demonstrated the use of quantum mechanical treatment for simultaneous explanation of CF, ICF and TF over a large energy range

  10. Determination of 2> from fission fragment anisotropy for reactions involving weakly bound 6,7Li projectiles

    Fission fragment (FF) angular distributions for 6,7Li+235,238U reactions and FF mass distributions for 6,7Li+238U reactions have been measured at energies around the Coulomb barrier and reported in earlier symposia. The aim is to investigate the effect of projectile breakup on various observables in fission reactions. Due to low breakup threshold there is a probability of breakup of the projectiles which in turn may affect the compound nucleus (CN) formation cross section. In the present study it is proposed to determine the 2 > from the measured fission fragment anisotropy and compare them with the ones obtained from coupled channels calculations to investigate the effect of projectile breakup

  11. RBEs of thermal neutron beam and the 10B(n,α)7Li reaction on skin in the hamster

    The skin relative biologic effectiveness (RBE) of a thermal neutron beam and the 10B(n,α)7Li reaction were determined by using Syrian (Golden) hamsters and compared with the RBE of a 9-MeV electron beam. The boron used in our experiment was 10B-paraboronophenylalanine (10B-BPA). The Kyoto University Research Reactor was used as the source of thermal neutrons. In the skin dose-response curve, thermal neutron beams produced an almost linear relationship between the maximum skin reaction and the absorbed dose. The RBE obtained in this experimental system was about 2.0. The RBEs of the 14N(n,p)14C and the 10B(n,α)7Li reaction were estimated as 3.1 and about 1.6, respectively, with the assumption that each component of radiation was additive

  12. Multinuclear NMR Imaging of Fluid Phases in Berea Sandstone

    Sarkar, S. N.; Dechter, J. J.; Komoroski, R. A.

    Multinuclear NMR of 7Li, 19F, and 1H has been investigated as a method for discriminating multiple fluid phases in porous rock. Good 7Li NMR images from LiCl brine in saturated Berea sandstone were obtained within a few hours at 1 × 1 × 5 mm 3 resolution using a low-TE, 3D volume imaging sequence. At 4.7 T, the 7Li T1 was 750 ms, and T2 was 10 ms. High-quality 19F and 1H images of a model fluorinated injectant (trifluorotoluene) in Berea were obtained at 0.4 × 0.4 × 3 mm 3 resolution in a few hours. Fluorine-19 imaging was found to be easier than 1H imaging due to the narrower 19F resonance and comparable T1 and T2 in Berea sandstone. Lithium-7 and 19F imaging offer alternatives for discriminating aqueous and organic phases unambiguously in flooded oil cores, especially where 1H signals for the two phases are unresolved.

  13. AB-BNCT beam shaping assembly based on 7Li(p,n)7Be reaction optimization

    A numerical optimization of a Beam Shaping Assembly (BSA) for Accelerator Based-Boron Neutron Capture Therapy (AB-BNCT) has been performed. The reaction 7Li(p,n)7Be 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.

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

    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.

  15. Cation and anion dynamics in the fast-ion conducting rotor phase of 7Li2SO4

    Complete text of publication follows. At 848 K, lithium sulfate undergoes a first-order phase transition. The high-temperature cubic a phase is a good cation conductor. At the same time, the oxo-anions are rotationally disordered. There has been a long debate about whether and how the rapid anion reorientation might enhance the canon transport through the crystal. We have performed quasielastic neutron scattering experiments on 7Li2SO4 in order to examine both anion and cation dynamics in this material. At Q -1, the quasielastic linewidth varies as DQ2 where D represents the Li tracer diffusion coefficient. At higher Q, we find a wave-like structure with linewidth maxima at 1.4 A-1 and 2.5 A-1 and a minimum at 1.9 A-1. This behavior is typical of coherent diffusion (7Li scatters both coherently and incoherently). We also see, at higher Q, a (coherent) quasielastic contribution from the oxygen nuclei due to the anion reorientation. Oxygen scattering is also found in the sodium cation conducting rotor phase of Na3PO4 where it is the predominant quasielastic component. Since the quasielastic scattering of 7Li2SO4 contains both cation and anion contributions, we perform classical molecular dynamics studies based on pair potentials from the literature. Results of these simulations are compared to the experimental dynamic structure factors. (author)

  16. Improved information on electron screening in 7Li(p,α)α using the Trojan-horse method

    The available astrophysical S(E) factor data for the reaction 7Li(p,α)α at 10b(E) factor curve for bare nuclides drops below the data, which in turn represent the case of electron-shielded nuclides, i.e. the electron-shielded Ss(E) factor. The comparison between Sb(E) and Ss(E) leads to an electron-screening potential energy Ue=350 eV, which is much higher than the adiabatic limit of 175 eV and not understood at present. The deduced value of Sb(0) is considerably smaller than the previously adopted value of 59 keV b, significantly increasing the calculated abundance of 7Li in big-bang nucleosynthesis. The Trojan-horse method was applied to the reaction 7Li(p,α)α to determine the energy dependence of the Sb(E) factor for 10b(E) curve and suggest that the THM may become a powerful way to obtain improved information on low-energy cross-sections and associated electron-screening effects in a model-independent way. (orig.)

  17. Local structure of LiB3O5 single crystal from 7Li nuclear magnetic resonance

    The local structure of LiB3O5 single crystal was investigated with 7Li (I=3/2) nuclear magnetic resonance measurements. We observed four different spectra, which could be divided into two groups corresponding to two kinds of lithium atoms, LiA and LiB, lying at crystallographically equivalent sites and magnetically inequivalent sites. From these results, the quadrupole coupling constants and the asymmetry parameters were determined at room temperature and are e2qQ/h=143±1 kHz and η=0.6±0.1 for 7Li. The directions of the principal axes of the electric field gradient tensors were also determined. The spectra for the two groups have the same principal values of the electric field gradient tensor, but different orientations, and originate from magnetically inequivalent sites. Also, the 7Li spin-lattice relaxation rate was measured, and the measured relaxation rate was found to be proportional to the temperature. The temperature-dependent single phonon process is considered to be more effective than the Raman process for nuclear quadrupole relaxation. In addition, we discuss the correlation between the asymmetry parameter and the largest nonlinear optical coefficient

  18. 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

    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

  19. Non-thermal processes in standard big bang nucleosynthesis: II. Two-body disintegration of D, 7Li, 7Be nuclei by fast neutrons

    Continuing the analysis of non-thermal effects in standard big bang nucleosynthesis (JCAP05(2008)010), we examine the role of suprathermal nuclear reactions induced in the early universe plasma by energetic nucleons of various origins. The processes of present interest are break-ups of D, 7Li, 7Be nuclei induced by 14-MeV neutrons generated in the plasma via the T(d, n)4He reaction. It is shown that this reaction forms the ensemble of fast neutrons whose fraction in the plasma neutron component is at the level of 0.01 %. In spite of the small percentage, such neutrons can effectively destroy the loosely bound D, 7Li, 7Be nuclei. It is found that at temperatures T9 7Li dominate over other reactions occurring in the n+D and n+7Li systems. However, the non-thermal neutronic effects prove to be insufficiently strong to modify the standard picture of nucleosynthesis. The D, 3He, 4He abundances are obtained to remain unchanged, and only a little effect is marked for primordial 7Li. The 0.01 % fraction of plasma neutrons (fast DT neutrons) reduces the 7Li abundance by 0.02 %

  20. Spectral flux of the p-7Li(C Q-M neutron source measured by proton recoil telescope

    Simakov S.P.

    2010-10-01

    Full Text Available The cyclotron-based fast neutron source at NPI produces mono-energetic neutron fields up to 35 MeV neutron energy using the p + 7Li(carbon backing reactions. To be applied for activation cross-section measurements, not only the intensity of neutron peak, but also the contribution of low-energy continuum in the spectra must be well determined. Simulations of the spectral flux from present source at a position of irradiated samples were performed using CYRIC TOF-data validated in the present work against LA150h by calculations with the transport Monte Carlo code MCNPX. Simulated spectra were tested by absolute measurements using a proton-recoil telescope technique. The recoil-proton spectrometer consisted of a shielded scattering chamber with polyethylene and carbon radiators and the ΔE1-ΔE2-E telescope of silicon-surface detectors located to the neutron beam axis at 45° in the laboratory system. Si-detectors were handled by usual data acquisition system. Dead-time – and pulse-overlap losses of events were determined from the count rate of pulse generator registered during duty cycle of accelerator operation. The proton beam charge and data were taken in the list mode for later replay and analysis. The calculations for 7Li(p,n and 12C(p,n reactions reasonably reproduce CYRIC TOF neutron source spectra. The influence of neutron source set-up (proton beam dimensions, 7Li-foil, carbon stopper, cooling medium, target support/chamber and the geometry-arrangement of irradiated sample on the spectral flux is discussed in details.

  1. Improved information on electron screening in {sup 7}Li(p,{alpha}){alpha} using the Trojan-horse method

    Aliotta, M.; Rolfs, C.; Strieder, F. [Inst. fuer Physik mit Ionenstrahlen, Ruhr-Universitaet Bochum (Germany); Spitaleri, C.; Lattuada, M.; Musumarra, A.; Pizzone, R.G. [Dipt. di Metodologie Fisiche e Chimiche per l' Ingegneria, Univ. di Catania (Italy); Tumino, A. [Catania Univ. (Italy). Ist. di Astronomia

    2000-12-01

    The available astrophysical S(E) factor data for the reaction {sup 7}Li(p,{alpha}){alpha} at 10=}100 keV, while at lower energies this calculated S{sub b}(E) factor curve for bare nuclides drops below the data, which in turn represent the case of electron-shielded nuclides, i.e. the electron-shielded S{sub s}(E) factor. The comparison between S{sub b}(E) and S{sub s}(E) leads to an electron-screening potential energy U{sub e}=350 eV, which is much higher than the adiabatic limit of 175 eV and not understood at present. The deduced value of S{sub b}(0) is considerably smaller than the previously adopted value of 59 keV b, significantly increasing the calculated abundance of {sup 7}Li in big-bang nucleosynthesis. The Trojan-horse method was applied to the reaction {sup 7}Li(p,{alpha}){alpha} to determine the energy dependence of the S{sub b}(E) factor for 10

  2. Angular measurement of the energy distribution of neutrons from the thick target 7Li(p,n)7Be source

    The energy spectrum of neutrons emitted from a thick lithium target bombarded by protons has been measured as a function of neutron angle of emission. The measurements were done at proton energies up to 2.8 MeV and at 30 deg. intervals in the range 0 to 120 deg. using proportional detectors with gas fillings of hydrogen and methane. A review is given of papers published on the 7Li(p,n)7 Be reactions at 0 deg.; where applicable, comparisons are made with the present results

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

    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.

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

    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.

  5. R-matrix Analysis for the 8Be System and Features in the p+7Li Reaction Over Resonance Region

    Kunieda Satoshi

    2016-01-01

    Full Text Available A comprehensive R-matrix analysis is currently underway for the 8Be compound system toward a consistent evaluation of the p+7Li reaction cross-sections over the resonance energy region. In this analysis, the energy eigenvalues are fixed to the level energies given in ENSDF, and we searched for values of the boundary condition parameters as well as the reduced-width amplitudes. It is found that some additional levels are necessary to fit the resonant shape of experimental cross-sections. Besides, the channel radii obtained may be consistent with well-known physical pictures of the atomic nucleus.

  6. R-matrix Analysis for the 8Be System and Features in the p+7Li Reaction Over Resonance Region

    Kunieda, Satoshi

    2016-06-01

    A comprehensive R-matrix analysis is currently underway for the 8Be compound system toward a consistent evaluation of the p+7Li reaction cross-sections over the resonance energy region. In this analysis, the energy eigenvalues are fixed to the level energies given in ENSDF, and we searched for values of the boundary condition parameters as well as the reduced-width amplitudes. It is found that some additional levels are necessary to fit the resonant shape of experimental cross-sections. Besides, the channel radii obtained may be consistent with well-known physical pictures of the atomic nucleus.

  7. 7Li(p-arrow-right,π+)8Li and 7Li(p-arrow-right,π-)8B reactions at T/sub p/ = 200 MeV

    Angular distributions of the cross sections and analyzing powers for the 7Li(p,π/sup +- /) reactions leading to the ground and first two excited states of the isobaric analog final nuclei 8Li and 8B have been measured at T/sub p/ = 200.4 MeV and 199.2 MeV, respectively. The (p,π+) cross sections are an order of magnitude larger than those of the (p,π-) reaction and exhibit a much stronger angular dependence. The (p,π+) analyzing power patterns are essentially state independent and similar to that of the elementary pp→dπ+ reaction near threshold. The analyzing power angular distribution for the 7Li(p,π-) 8B(2.32 MeV, 3+) transition exhibits a ''signature'' characteristic of (p,π-) transitions to stretched high-spin two-particle one-hole final states, which is distinctly different from the pattern observed for transitions to low-spin final states. The differences between the two reactions are interpreted in terms of the dynamics of the elementary pp→dπ+ and pn→ppπ- processes

  8. NMR spectroscopic investigations on flavin catalyzed photooxidations

    Feldmeier, Christian

    2015-01-01

    Nature makes broad use of sunlight as an energy source for chemical conversions. In recent years the use of light as a driving force for chemical conversions has gained much attention in synthetic chemistry and the area of photocatalysis has seen rapid advances. These rapid developments in synthetic applications have heightened the need for comprehensive mechanistic pictures of the underlying mechanisms to enable a rational design of photocatalytic systems. Transient absorption spectroscopy h...

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

    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.

  10. Study of the reactions 6Li(pα)3He, 6Li(dα)4He, 6Li(dp0)7Li and 6Li(dp1)7Li* from 300 keV to 1000 keV

    Experimental results are presented for the four reactions 6Li (pα)3He, 6Li (dα)4He, 6Li (dp0)7Li and 6Li (dp1)7Li* between 300 keV and 1000 keV. The angular distributions, the excitation curves and the total cross-section curves are presented in absolute values. (authors)

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

    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-7Li 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, 238U and 232Th fission counters, 7LiF and natLiF TLDs and solid state nuclear track detector, are numerically provided in this report in the energy region between 10-4 eV and the energy of peak neutrons generated by the 7Li(p,n) reaction. (author)

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

    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).

  13. Compact NMR

    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.

  14. Compact NMR

    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.

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

    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.

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

    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

  17. The photonuclear reaction 7Li(γ, t)α and the model of light cluster interaction

    The characteristic of photonuclear reaction 7Li(γ, t)α have been computed in different αt-cluster models. Two pure attractive αt-potentials and two their spectrum- and phase-equivalent supersymmetric partners with repulsive core were used. Both an ordinary two-cluster model and the orthogonality conditions model by Saito have been applied. The process amplitude has been calculated in coordinate representation based on multipole expansion of wave functions and transition operator. Both for states of the continuous spectrum and for bound state, the wave functions of relative motion in the αt-system are computed directly from the Schroedinger equation. The sensitivity of the reaction characteristics to the choice of model and potential is revealed. The Saito model and potentials with no repulsive core provide somewhat better description of experimental data

  18. Analysis of diffractive features in elastic scattering of {sup 7}Li by different target nuclei at different energies

    Badran, R. I.; Masri, Dana Al [Physics Department, Faculty of Sciences, The Hashemite University, Zarqa (Jordan)

    2013-12-16

    The diffractive features of angular distribution have been investigated by analyzing the experimental data for a set of elastic scattering processes of {sup 7}Li by different target nuclei at different laboratory energies. Both Frahn-Venter and McIntyre models are used to analyze experimental data of angular distribution for elastic scattering processes. The theoretical models can reasonably reproduce the general pattern of the data. Some geometrical parameters for colliding nuclei have been obtained from the elastic scattering processes. It is found that interpretation of the diffractive features of the data is model-independent. The values of extracted parameters, from adopted models, are found comparable to each other and to those of others. The total reaction cross section is correlated to the incident laboratory energy for each scattering and values of total reaction cross section are found comparable with those of others.

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

    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.

  20. Elastic and inelastic angular distributions of the 7Li+120Sn system for energies near the Coulomb barrier

    Zagatto, V. A. B.; Oliveira, J. R. B.; Gasques, L. R.; Alcántara-Núñez, J. A.; Duarte, J. G.; Aguiar, V. P.; Medina, N. H.; Seale, W. A.; Pires, K. C. C.; Freitas, A.; Lubian, J.; Shorto, J. M. B.; Genezini, F. A.; Rossi, E. S., Jr.

    2016-06-01

    The reaction of 7Li+120Sn has been measured at bombarding energies of 21, 24 and 27 MeV. The {2}+\\to {0}+ γ -ray transition in 120Sn was observed and the angular distribution for the 2+ excited state was obtained. Coupled channels and coupled-reaction channels calculations, including the dynamical polarization potential due to the projectile break-up, obtained from continuum discretized coupled channel calculations, were performed. The comparison between the existing experimental elastic angular distribution with the coupled-reaction channels calculations indicates that the 1n stripping transfer is the most intense channel to be coupled and the 2n stripping reaction occurs sequentially rather than directly, however, further data must be analyzed to confirm this indication. The experimental elastic and inelastic scattering data were well described by the calculations, but some discrepancies in these channels may indicate the need for corrections to the nuclear potential and/or the necessity to incorporate further channels.

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

    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.

  2. Separation of no-carrier-added 62Zn from 7Li irradiated cobalt target using calcium alginate beads

    A 59Co target was irradiated with 47 MeV 7Li, which produced NCA 62Zn in the target matrix. NCA 62Zn was separated from the target matrix by adsorption on calcium alginate beads kept in HNO3 solutions of different pH values (1-6). The optimum separation condition was achieved at pH 5, where ∼83% NCA 62Zn was adsorbed on the alginate beads along with some contamination from the bulk Co. The complete separation of 62Zn from the bulk was achieved on desorbing Co from the beads with 0.1 M NaNO2. The remaining 62Zn was separated on re-adsorption under the same condition. (author)

  3. R-matrix analysis of reactions in the 9B compound system applied to the 7Li problem in BBN

    Paris, M.; Hale, G.; Hayes-Sterbenz, A.; Jungman, G.

    2016-01-01

    Recent activity in solving the ‘lithium problem’ in big bang nucleosynthesis has focused on the role that putative resonances may play in resonance-enhanced destruction of 7Li. Particular attention has been paid to the reactions involving the 9B compound nuclear system, d+7Be → 9B. These reactions are analyzed via the multichannel, two-body unitary R-matrix method using the code EDA developed by Hale and collaborators. We employ much of the known elastic and reaction data, in a four-channel treatment. The data include elastic 3He +6Li differential cross sections from 0.7 to 2.0 MeV, integrated reaction cross sections for energies from 0.7 to 5.0 MeV for 6Li(3He,p)8Be* and from 0.4 to 5.0 MeV for the 6Li(3He,d)7Be reaction. Capture data have been added to an earlier analysis with integrated cross section measurements from 0.7 to 0.825 MeV for 6Li(3He,γ)9B. The resulting resonance parameters are compared with tabulated values, and previously unidentified resonances are noted. Our results show that there are no near d+7Be threshold resonances with widths that are 10’s of keV and reduce the likelihood that a resonance-enhanced mass-7 destruction mechanism, as suggested in recently published work, can explain the 7Li problem.

  4. 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

    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.

  5. 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.

    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. PMID:27054702

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

    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. The 3He(alpha, gamma)7Be reaction rate, solar 7Be and 8B neutrino fluxes, and the production of 7Li during the Big Bang

    The 3He(α,γ)7Be reaction plays an important role both in determining the predicted fluxes of 7Be and 8B neutrinos from our Sun, and in the calculation of primordial 7Li production. In light of the highly precise determination of the baryon-to-photon ratio from the cosmic microwave background data, it is necessary to re-determine primordial 7Li production. Recent experimental nuclear astrophysics work has led to an improved determination of the 3He(α,γ)7Be cross section, with several experiments clustered at E = 0.5 MeV center-of-mass energy and above [2, and references therein]. On the other hand, precisely calibrated 7Be and 8B neutrino fluxes from the Sun are now available. Assuming the accepted solar central temperature to be correct, the neutrino flux data can be used to determine the 3He(α,γ)7Be cross section at the solar Gamow peak, E = 0.03 MeV. The energy range relevant for Big Bang 7Li production lies just between 0.03 and 0.5 MeV. The poster aims to use the two above described levels in order to improve the precision of the predicted primordial abundance of 7Li. It updates a previous work that appeared before the new cross section, solar neutrino and microwave background data were available. (author)

  8. Electrical conductivity, differential scanning calorimetry, X-ray diffraction, and 7Li nuclear magnetic resonance studies of n-CxH(2x+1)OSO3Li (x = 12, 14, 16, 18, and 20)

    Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C xH(2x+1)OSO3Li (x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C xH(2x+1)OSO3Na and n-C xH(2x+1)OSO3K (x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (ΔS). For n-C 18H37OSO3Li and n-C 20H41OSO3Li salts, each melting point produced a small ΔSmp value compared with the total entropy change in the solid phases (ΔStr1+ΔStr2). Additionally, Li + ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. 7Li NMR spectra of n-C 18H37OSO3Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li + ions are localized at asymmetric sites in the crystals

  9. Ab initio calculation on the analytic potential energy functions for the state a3∑u+ and the state b3∏u of spin-aligned trimer 7Li2

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

    2005-01-01

    The energies, equilibrium geometries and harmonic frequencies of the triplet excited states (a3∑u+ and b3∏u) of spin-aligned trimer 7Li2 are firstly calculated by using a symmetry adapted cluster-configuration interaction method.The potential curves for the two excited states have least squares fitted by the Murrell-Sorbie function. The spectroscopic data (Be, αe, ωe, and ωeχe) and the force constants (f2, f3 and f4) are calculated. It is found that the spin-aligned triplet excited state b3∏u is more stable than the ground state X1∑g+, and that the Murrell-Sorbie function form is suitable not only for the ground state but also for the spin-aligned triplet excited states. Comparison between the theoretical determinations of dissociation energies, equilibrium interatomic distances and harmonic frequencies with the agreement between theories and experiments.

  10. 1H, 13C and 31P-NMR spectroscopic study of glucose metabolism of muscle larva Trichinella spiralis (U.S.A. strain), and the effects of the end-products on the host (mouse)

    1H- and 13C-nuclear magnetic resonance (NMR) spectroscopy was used to identify and quantitate metabolites excreted by muscle larva Trichinella spiralis maintained aerobically in the presence of D- (13C6) glucose and (1, 1'-13C2) succinate. End-products of glucose metabolism studied by 1H-NMR were lactate, acetate, succinate, proionate, n-valerate and alanine, at the molar ratio of 1:2:1:0.6:0.5:0.6. 13C-NMR measurement proved that all the products originated from the glucose in the medium via the phosphoenolpyruvate carboxykinase-succinate pathway and the tricarboxylic acid cycle. In vivo 31P-NMR spectra were also taken by the surface coil method from the leg muscle of mice which had been infected with T. spiralis. Intracelluar pH and relative amount of ATP in the leg muscle of the infected mice were found to decrease significantly as compared with that of control mice. (author)

  11. Effect of 10B(n, α)7Li irradiation on the structure of a sodium borosilicate glass

    The effects of the nuclear reaction 10B(n, α)7Li on the properties and structure of a sodium borosilicate glass were analysed by density, hardness and fracture toughness measurements, Raman and Nuclear Magnetic Resonance spectroscopy and Transmission Electronic Microscopy (TEM) characterization. The TEM observations showed a homogeneous irradiated glass structure up to the nanometer scale. Modifications of the local order around the main cations were noticed, mainly a slight decrease of the mean boron coordination number and an increase of non-bridging oxygen concentrations. At the glass medium range order, the appearance of the D2 Raman band and a modification of the Si–O–Si angle distribution were also observed after irradiation. A comparison with other irradiation conditions with Swift Heavy Ions (Kr with 74 MeV) and Gold irradiation (with energies ranging from 1 to 7 MeV) is presented. Raman spectroscopy showed a similar final structure for irradiation conditions under which the glass evolutions are controlled by electronic energy loss in the ion tracks formation regime or nuclear energy loss. Despite important differences in energy deposition regimes, the similarities observed between the final glass structures suggest that structural evolutions are controlled by the glass relaxation mechanisms during the high quenching rate step that follows the energy deposition step

  12. Evaluation of d + 6,7Li data for deuteron incident energies up to 50 MeV

    A new evaluation of the nuclear data for a particle transport calculations was performed for d + 6,7Li interactions in the energy region from 4 to 50 MeV incident energy. Use was made of the available new optical model potential for d + Li interactions. For the description of a neutron emission a new optical model potential for n + 9Be was elaborated for the neutron energies from 0.1 to 22 MeV. Global optical model potentials were used for the neutrons above 22 MeV and for protons, tritons, He-3 and alphas - in the whole energy range. The following nuclear processes were accounted for: particle evaporation and preequilibrium emission, stripping of the proton from the deuteron and direct interactions of deuterons with lithium nuclei. GNASH and ECIS96 codes were applied for the first two process descriptions, the Serber model was utilised for stripping processes and the DWUCK4 code was used for direct reaction processes modelling. Total neutron emission spectra were calculated as a sum of the spectra in all these processes. A complete transport file was finally prepared in ENDF-6 format covering the deuteron incident energies up to 50 MeV. The newly evaluated data are in good agreement with experimental data for neutron emission spectra. The evaluated data files were successfully tested with a modified version of the MCNP computer code

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

    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.

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

    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.

  15. Production and separation of no-carrier-added 73As and 75Se from 7Li irradiated germanium oxide target

    This work reports for the first time 7Li-induced accelerator based production of 71,72,73,74As, 75,76,77Br and 73,75Se radionuclides in their no-carrier-added (nca) state. After the decay of all short-lived radionuclides 75Se and 73As were only existing radionuclides in germanium oxide target, which were subsequently separated by liquid-liquid extraction (LLX) using trioctylamine (TOA) dissolved in cyclohexane as liquid ion exchanger. The presence of stable germanium in various fractions was examined by Inductively Coupled Plasma Optical Spectrometry (ICP-OES). At 0.1 M TOA and 10 M HCl concentration, 75Se and stable Ge were extracted into the organic phase leaving 73As in the aqueous phase. The bulk Ge was stripped back to the aqueous phase by 1 M NaOH, keeping 75Se in the organic phase. Therefore complete separation between 73As, 75Se and bulk Ge was achieved. (orig.)

  16. Spectator invariance test in the study of the 6,7Li fusion reactions via the Trojan Horse Method

    Fusion reactions play a crucial role for several astrophysical scenarios. At the low energies typical of such environments direct measurements of reaction cross sections are very difficult, and even sometimes impossible. In such cases the use of indirect methods can give a substantial help. The Trojan Horse Method (THM) is based on the quasi-free break-up of a nucleus, which can be described in terms of a cluster structure. In such applications the independence of THM results with different break-up schemes, was tested using the quasi free 3He(6Li,αα)H and 3He(7Li,αα)2H reactions. Results were then compared with the direct behaviours obtained from available data as well as with the cross sections extracted from previous indirect investigations of the same binary reactions using a different nuclide as a Trojan Horse nucleus. We conclude that the PWIA (Plane Wave Impulse Approximation) is valid in both cases and that the use of a different spectator particle does not influence the THM result

  17. A computer study of the experimental feasibility of observing the nuclear excitation of 7Li by reactor antineutrinos

    Avignone, F. T.; Donnelly, T. W.

    1981-01-01

    A computer study of the feasibility of observing the 0.478 MeV γ-ray following the antineutrino excitation of 7Li has been carried out in a simple geometry involving two large Ge detectors placed on the axis inside a 20 kg target of natural lithium. The background γ-ray flux was assumed to be that observed by Fiorini and his co-workers in their search for neutrinoless double beta decay of 76Ge. The target was assumed to be inside a rectangular live shield of NaI(Tl) which has a wall thickness of 10.16 cm. The results for the Weinberg-Salam model clearly show that the direct observation of this reaction is feasible even if the background is almost two orders of magnitude more intense than the background observed by Fiorini et al. This conclusion was found to be valid even if most of the background originates inside the cryostat itself. If the background is no more than three times as intense as that observed by Fiorini et al., the excitation can at least be observed with a larger target and with no NaI(Tl) annulus.

  18. Investigation of the antiprotonic X-ray spectrum of the lithium isotopes 6Li and 7Li

    Antiprotons of the low-energy separated anti p-beam K23 at CERN in Geneva have been stopped in thin (0.6 g/cm2) targets of the Lithium isotopes 6Li and 7Li. The characteristic X-rays of the formed antiprotonic atoms were measured with four identical high-resolution Si (Li) detectors. Three lines of the N- series, four lines of the M-series and the 3d-2p transition of the Balmer series were observed. The measured relative intensities of the M- and N-series transitions are well described by the simple cascade model of Eisenberg and Kessler. The 3d-2p transition is considerably influenced by the strong interaction between antiproton and nucleus and thus drastically reduced in intensity. The analysis of this transition yields the shift and width of the 2p level, whereas the width of the 3d level is deduced from intensity considerations. (orig./HSI)

  19. Exploring the N{alpha}+3n light nuclei via the ({sup 7}Li,{sup 7}Be) reaction

    Nociforo, C.; Cappuzzello, F.; Orrigo, S.E.A.; Winfield, J.S. [INFN-Laboratori Nazionali del Sud, Catania (Italy); Cunsolo, A.; Cavallaro, M. [INFN-Laboratori Nazionali del Sud, Catania (Italy); Universita di Catania, Dipartimento di Fisica e Astronomia, Catania (Italy); Foti, A. [Universita di Catania, Dipartimento di Fisica e Astronomia, Catania (Italy); INFN-Sezione di Catania, Catania (Italy); Fortier, S.; Beaumel, D. [Institut de Physique Nucleaire, Orsay Cedex (France); Lenske, H. [Universitaet Giessen, Institut fuer Theoretische Physik, Giessen (Germany)

    2006-03-15

    Experimental signatures of the dynamical correlations of a core with a single-particle neutron have been found in light neutron-rich nuclei investigated via the ({sup 7}Li,{sup 7}Be) charge-exchange reactions at around 8 MeV/u. Of particular astrophysical relevance are low-lying narrow resonances ({gamma}{proportional_to}200 keV FWHM) BSEC (Bound States Embedded in the Continuum). Because of their long lifetime BSEC states are likely to effect the capture rates in any scenario for nucleosynthesis in neutron-rich environment. They have been observed in the continuum of {sup 11}Be and {sup 15}C nuclei. A microscopic nuclear structure model based on QRPA theory, which takes into account Dynamical Core Polarisation (DCP) correlations, gives a suitable description of these resonances as well as single-particle states of the studied systems. In this context, high-energy narrow structures populated in nuclei having an integer number of {alpha}-particles plus three neutrons are good BSEC candidates and can be systematically investigated. (orig.)

  20. Thermally stimulated exoelectron emission observed in mixed Li2B4O7-LiCl ceramics

    Previous investigations of thermally stimulated exoelectron emission (TSEE) in Li2B4O7 ceramics showed that microcrystallized samples gave rise to well-isolated and fairly strong TSEE peaks when they were cooled to about -1100C or to lower temperatures before the heating to measure the TSEE, without previous irradiation which is often required to induce TSEE. It was considered that the origin of such TSEE without irradiation might be related to the piezoelectric nature of the Li2B4O7 crystal. In the present investigation the TSEE induced by quenching to liquid nitrogen temperature for sintered samples of Li2B4O7-LiCl mixtures in different ratios was measured. The samples lose their piezoelectricity with the increased contents of LiCl. The results showed a decrease in TSEE with increased LiCl content, supporting the hypothesis. The decrease was not proportional to the LiCl content, however. Additional peaks appearing in samples irradiated with X-rays offer the possibility of an application to radiation dosimetry. (U.K.)

  1. New high S/N observations of the (6Li) /(7) Li blend in HD 84937 and two other metal-poor stars

    Cayrel, R.; Spite, M.; Spite, F.; Vangioni-Flam, E.; Cassé, M.; Audouze, J.

    1999-03-01

    High signal to noise ratio spectra have been obtained with the GECKO spectrograph at CFHT, at a spectral resolution of 100 000, for three metal-poor stars in order to obtain more accurate abundances of the very fragile element (6) Li. For two newly observed stars, BD +42 2667 and BD +36 2165 it appears that the first may have a detectable amount of (6) Li, whereas no (6) Li is found in the second one. The S/N ratio of only a few hundreds obtained for these two faint stars preclude however a firm conclusion. For the third star, the well known object HD84937, a very high S/N of 650 per pixel (over 1000 per resolved spectral element) was obtained, yielding greatly improved accuracy over previous determinations. A value of (6) Li / (7) Li = 0.052 +/- 0.019 (one sigma) is obtained. We also conclude that the no- (6) Li assumption is ruled out at the 95 per cent level, even in the most permissive case, when a variation of all the other free parameters (wavelength zero-point, continuum location, macroturbulent broadening, abundance of (7) Li) is allowed. The possibility that the (6) Li feature is an artifact due to a once suspected binarity of HD 84937 is discussed, with the conclusion that this assumption is ruled out by the extant data on the radial velocity of the object. The (6) Li abundance is compared with recent models of formation of the light elements Li, Be and B. This comparison shows that (6) Li is either undepleted, or only moderately depleted in HD 84937, from its initial value. Under the assumption that the atmospheric depletion of (6) Li and (7) Li in stars is by slow mixing with hot layers (underneath the convective zone), in which these elements can burn, we conclude that the depletion of (7) Li by this mechanism in HD 84937 is less than 0.1 dex. This new upper limit to the efficiency of the depletion of (7) Li by slow mixing burning, in a star located on the Spite plateau, leads to a more secure estimation of the primordial abundance of (7) Li. However

  2. NMR spectroscopy

    The book reviews the applications of NMR-spectroscopy in medicine and biology. The first chapter of about 40 pages summarizes the history of development and explains the chemical and physical fundamentals of this new and non-invasive method in an easily comprehensible manner. The other chapters summarize diagnostic results obtained with this method in organs and tissues, so that the reader will find a systematic overview of the available findings obtained in the various organ systems. It must be noted, however, that ongoing research work and new insight quite naturally will necessitate corrections to be done, as is the case here with some biochemical interpretations which would need adjustment to latest research results. NMR-spectroscopy is able to measure very fine energy differences on the molecular level, and thus offers insight into metabolic processes, with the advantage that there is no need of applying ionizing radiation in order to qualitatively or quantitatively analyse the metabolic processes in the various organ systems. (orig./DG) With 40 figs., 4 tabs

  3. HPLC/1H NMR spectroscopic studies of the reactive alpha-1-O-acyl isomer formed during acyl migration of S-naproxen beta-1-O-acyl glucuronide.

    Corcoran, O; Mortensen, R W; Hansen, S H; Troke, J; Nicholson, J K

    2001-10-01

    A widely held view in drug metabolism and pharmacokinetic studies is that the initial 1-isomer to 2-isomer step in the intramolecular acyl migration of drug ester glucuronides is irreversible, and that alpha-1-O-acyl isomers do not occur under physiological conditions. We investigated this hypothesis using high-performance liquid chromatography directly coupled to proton nuclear magnetic resonance spectroscopy (HPLC/1H NMR) and mass spectrometry (LC/MS) to probe the migration reactions of S-naproxen beta-1-O-acyl glucuronide, in phosphate buffer at pH 7.4, 37 degrees C. We report the first direct observation of the alpha-1-O-acyl isomer of a drug ester glucuronide (S-naproxen) formed in a biosystem via the facile acyl migration of the corresponding pure beta-1-O-acyl glucuronide. The unequivocal identification of the reactive product was achieved using stopped-flow one-dimensional HPLC/1H NMR and two-dimensional 1H-1H total correlation spectroscopy (1H-1H TOCSY). Parallel LC/ion-trap mass spectrometry yielded the confirmatory glucuronide masses. Moreover, "dynamic" stopped-flow HPLC/1H NMR experiments revealed transacylation of the isolated alpha-1-O-acyl isomer to a mixture of alpha/beta-2-O-acyl isomers; the reverse reaction from the isolated alpha/beta-2-O-acyl isomers to the alpha-1-O-acyl isomer was also clearly demonstrated. This application of "dynamic" stopped-flow HPLC/1H NMR allows key kinetic data to be obtained on a reactive metabolite that would otherwise be difficult to follow by conventional HPLC and NMR methods where sample preparation and off-line separations are necessary. These data challenge the widely held view that the alpha-1-O-acyl isomers of drug ester glucuronides do not occur under physiological conditions. Furthermore, the similar formation of alpha-1-O-acyl isomers from zomepirac and diflunisal beta-1-O-acyl glucuronides has recently been confirmed (Corcoran et al., unpublished results). Such reactions are also likely to be widespread

  4. Cross-section measurement for the 10B(n, alpha)7Li reaction at 4.0 and 5.0 MeV.

    Zhang, Guohui; Guo, Li'an; Cao, Rongtai; Zhang, Jiaguo; Chen, Jinxiang

    2008-10-01

    Cross-sections of the (10)B(n, alpha)(7)Li reaction were measured at En=4.0 and 5.0 MeV. A gridded ionization chamber (GIC) was used as charged particle detector. Neutrons were produced through the D(d, n)(3)He reaction with a deuterium gas target. Experiments were performed at the 4.5 MV Van de Graaff accelerator of Peking University. Cross-section data of the (238)U(n, f) reaction were employed as standard. The measured cross-sections of the (10)B(n, alpha)(7)Li reaction at 4.0 and 5.0 MeV are 211+/-17 and 169+/-14 mb, respectively, and they are compared with existing results of measurements and evaluations. PMID:18387305

  5. Neutron characterization study for D–T, p-{sup 7}Li neutron sources with new BCA based direct collision coupling method

    Wang, Guan-bo, E-mail: wgb04dep@hotmail.com [Insititute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Yang, Xin [Insititute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China); Department of Engineering Physics, Tsinghua University, Beijing 100084 (China); Qian, Da-zhi; Li, Run-dong; Tang, Bin [Insititute of Nuclear Physics and Chemistry, China Academy of Engineering Physics, Mianyang 621900 (China)

    2014-09-01

    The T(D,n){sup 4}He and {sup 7}Li(p,n){sup 7}Be neutron sources have been used for decades in nuclear physics research, stellar nucleosynthesis research and neutron therapy research. In this work, the neutron characterization including neutron yield, spectra, and angular distribution for D–T and p-{sup 7}Li sources have been studied with our new binary collision approximation (BCA) based direct collision coupling method. Distinguished from the traditional path integration method for getting the neutron weight, the new model establishes a relationship between the scattering cross section and the impact parameter, which allows the secondary neutron generation carrying out jointly with ions BCA tracking. The experimental measurements of neutron characterizations have been employed for these two reactions, and the new algorithm is validated.

  6. Simulation of the neutron spectrum from the 7Li(p,n) reaction with a liquid-lithium target at Soreq Applied Research Accelerator Facility

    The 7Li(p,n)7Be reaction has been used for the last 25 years to produce quasi-Maxwellian neutrons in order to measure Maxwellian-Averaged Cross-Sections in the relevant temperatures for stellar nucleosynthesis. A liquid-lithium target at the Soreq Applied Research Accelerator Facility is expected to allow us to perform such measurements at higher neutron intensities. Here we describe a Monte Carlo tool, SimLiT, developed to evaluate neutron spectra, intensities and angular distributions resulting from this reaction. We also demonstrate the feasibility to couple SimLiT with an advanced transport code, resulting in a powerful tool for planning and analysis of experiments using the 7Li(p,n) reaction as a neutron source.

  7. Production cross section of At radionuclides from $^{7}$Li+$^{\\textrm{nat}}$Pb and $^{9}$Be+$^{\\textrm{nat}}$Tl reactions

    Maiti, Moumita

    2011-01-01

    Earlier we reported theoretical studies on the probable production of astatine radionuclides from $^{6,7}$Li and $^{9}$Be-induced reactions on natural lead and thalliun targets, respectively. For the first time, in this report, production of astatine radionuclides has been investigated experimentally with two heavy ion induced reactions: $^{9}$Be+$^{\\textrm{nat}}$Tl and $^{7}$Li+$^{\\textrm{nat}}$Pb. Formation cross sections of the evaporation residues, $^{207,208,209,210}$At, produced in (HI, xn) channel, have been measured by the stacked-foil technique followed by the off-line $\\gamma$-spectrometry at the low incident energies ($<$50 MeV). Measured excitation functions have been explained in terms of compound nuclear reaction mechanism using Weisskopf-Ewing and Hauser-Feshbach model. Absolute cross section values are lower than the respective theoretical predictions.

  8. 3He (α , γ)7Be and 3H (α , γ)7Li astrophysical S factors from the no-core shell model with continuum

    Dohet-Eraly, Jérémy; Navrátil, Petr; Quaglioni, Sofia; Horiuchi, Wataru; Hupin, Guillaume; Raimondi, Francesco

    2016-06-01

    The 3He(α , γ)7Be and 3H(α , γ)7Li astrophysical S factors are calculated within the no-core shell model with continuum using a renormalized chiral nucleon-nucleon interaction. The 3He(α , γ)7Be astrophysical S factors agree reasonably well with the experimental data while the 3H(α , γ)7Li ones are overestimated. The seven-nucleon bound and resonance states and the α + 3He/3H elastic scattering are also studied and compared with experiment. The low-lying resonance properties are rather well reproduced by our approach. At low energies, the s-wave phase shift, which is non-resonant, is overestimated.

  9. Trojan horse particle invariance studied with the 6Li(d,α)4He and 7Li(p,α)4He reactions

    The Trojan horse nucleus invariance for the binary reaction cross section extracted from the Trojan horse reaction was tested using the quasifree 3He(6Li,αα)H and 3He(7Li,αα)2H reactions. The cross sections for the 6Li(d,α)4He and 7Li(p,α)4He binary processes were extracted in the framework of the plane wave approximation. They are compared with direct behaviors as well as with cross sections extracted from previous indirect investigations of the same binary reactions using deuteron as the Trojan horse nucleus instead of 3He. The very good agreement confirms the applicability of the plane wave approximation which suggests the independence of the binary indirect cross section on the chosen Trojan horse nucleus, at least for the investigated cases.

  10. Investigation of 7Li+d cluster channel at the photodisintegration of 9Be nucleus presented by 2αn-model

    In present work the process 9Be(γ, d)7Li has been investigated within the energy range of Eγ from the threshold up to 40 MeV. In the framework of cluster approach method of analysis of differential cross sections resonance structure has been developed. Wave functions of 7Lid cluster channel were obtained analytically by projecting of 2αn wave functions of 9Be nucleus. (author)

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

    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.

  12. Green methods for the radiochemical separations of no-carrier-added 61Cu, 62Zn from 7Li irradiated cobalt target

    A natCo target was irradiated with 47 MeV 7Li beam to produce no-carrier-added 61Cu, 62Zn in the target matrix. Two new green radiochemical methods were developed for separation of 61Cu and 62Zn from the target matrix, (i) liquid-liquid extraction (LLX) technique using room temperature ionic liquid (RTIL) 1-butyl-3-methylimidazolium hexafluorophosphate ([C4mim][PF6]) and ammonium pyrrolidinedithiocarbamate (APDC) (ii) adsorption on calcium alginate beads. (author)

  13. Study of the 7Be(p,γ)8B and 7Li(n,γ)8Li capture reactions using the shell model embedded in the continuum

    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: 8B and 8Li, as well as to the description of low energy cross sections (the astrophysical S factors) in the capture reactions: 7Be(p,γ)8B and 7Li(n,γ)8Li. (author)

  14. NMR in solid ionic and nanoionics

    Full text: Nuclear Magnetic Resonance (NMR) is a spectroscopic technique which employs magnetic nuclei to study, among others, the dynamics of condensed matter at the atomic level. Thus, NMR has been and still is a successful instrument in the research field of solid electrolytes also known as solid ionics. This paper presents the typical NMR experiments performed in solid ionics together with some examples from nanoionics. The experiments to be discussed comprise: (i) measurements of the diffusion coefficient employing the pulsed-field gradient and the static fringe-field method; (ii) the experimentally related NMR imaging; (iii) double resonance experiments like spin-echo double resonance (SEDOR) and two-dimensional Fourier transform NMR (2D-FT NMR); (iv) various types of nuclear relaxation, in particular spin-lattice relaxation. The NMR techniques yield information on topics like the following: type and number of mobile atoms and defects, diffusion pathways (e.g. dimensionality restrictions), atomic jump frequencies, activation energy and activation volume of these movements, diffusion coefficient with activation energy and prefactor, correlation effects in atomic movements, space correlation factor, cooperative phenomena, symmetry of atomic sites, behavior at phase transitions. These applications will be illustrated by giving examples from crystals, glasses, and polymers. (author)

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

    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...

  16. 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

    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

  17. 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

    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.

  18. Test of special relativity theory by means of laser spectroscopy on relativistic 7Li+ ions in the ESR

    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 7Li+ 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 1s2s3S1→1s2p3P2 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 earlier measurements performed at a

  19. Spectroscopic analysis (FT-IR, FT-Raman and NMR) and molecular docking study of ethyl 2-(4-oxo-3-phenethyl-3,4-dihydroquinazolin-2-ylthio)-acetate

    El-Azab, Adel S.; Jalaja, K.; Abdel-Aziz, Alaa A.-M.; Al-Obaid, Abdulrahman M.; Sheena Mary, Y.; Yohannan Panicker, C.; Van Alsenoy, C.

    2016-09-01

    The vibrational wavenumbers, molecular structure, MEP, NLO, NBO and HOMO, LUMO analysis of Ethyl 2-(4-oxo-3-phenethyl-3,4-dihydroquinazolin-2-ylthio)-acetate (EPDA) were reported. The change in electron density in the antibonding orbitals and stabilization energies have been calculated by NBO analysis to give clear evidence of stabilization in the hyperconjugation of hydrogen bonded interaction. The difference in HOMO and LUMO energy support the charge transfer interaction within the molecule. NMR studies and Fukui functions are also reported. From molecular electrostatic potential plot it is evident that the negative charge covers the carbonyl groups, phenyl rings and the positive region is over the CH2 groups with the acetate group. Molecular docking studies shows that the title compound forms a stable complex with pyrrole inhibitor and gives a binding affinity value of -8.3 kcal/mol and the results suggest that the compound might exhibit inhibitory activity against pyrrole inhibitor.

  20. (29)Si, (47)Ti, (49)Ti and (195)Pt solid state MAS NMR spectroscopic investigations of ternary silicides TPtSi, germanides TPtGe (T = Ti, Zr, Hf) and stannide TiPtSn.

    Benndorf, Christopher; Eckert, Hellmut; Pöttgen, Rainer

    2016-05-10

    Eight ternary tetrelides TPtX (T = Ti, Zr, Hf; X = Si, Ge, Sn) were synthesized from the elements by arc-melting and subsequent annealing. TiPtSi, ZrPtSi, ZrPtGe, HfPtSi and HfPtGe crystallize with the orthorhombic TiNiSi type structure, in the space group Pnma. The structures of HfPtSi (a = 654.44(9), b = 387.97(6), c = 750.0(1) pm, wR2 = 0.0592, 411 F(2) values, 20 variables) and HfPtGe (a = 660.36(7), b = 395.18(4), c = 763.05(8) pm, wR2 = 0.0495, 430 F(2) values, 20 variables) were refined from single crystal X-ray diffractometer data. TiPtSn adopts the cubic MgAgAs type. TiPtGe is dimorphic with a TiNiSi type high-temperature modification which transforms to cubic LT-TiPtGe (MgAgAs type). All phases were investigated by high resolution (29)Si, (47)Ti, (49)Ti and (195)Pt solid state MAS NMR spectroscopy. In the cubic compounds, the (47/49)Ti NMR signals are easily detected owing to the absence of quadrupolar broadening effects. The (195)Pt resonances of the orthorhombic compounds are characterized by strongly negative isotropic Knight shifts and large Knight shift anisotropies, whereas positive isotropic Knight shifts and no anisotropies are observed for the cubic compounds. These results indicate that the phase transition in TiPtGe is associated with dramatic changes in the electronic properties. Within each group of isotypic compounds the isotropic (29)Si, (47/49)Ti and (195)Pt Knight shifts show systematic dependences on the transition metal or tetrel atomic number, suggesting that the numerical values are influenced by the electronegativities of the metallic (or metalloid) neighbours. PMID:27097719

  1. 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

    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.

  2. 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

    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.

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

    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.

  4. Probing Organometallic Reactions With 19F NMR

    Hawrelak, Eric James

    2002-01-01

    This dissertation explores fundamental aspects of the reaction of group 4 metallocenes with methylaluminoxane (MAO) that lead to active Ziegler-Natta olefin polymerization catalysts. A novel experimental approach is described, in which a unique spectroscopic probe (a fluorinated substituent) is attached to the metallocene ancillary ligands and the metallocene/MAO mixtures are analyzed using 19F NMR spectroscopy. Group 4 metallocene dimethides bearing pentafluorophenyl (C6F5) substituents ...

  5. Spectroscopic data

    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...

  6. NMR study of thermal decomposition of lithium tetrahydroaluminate

    Pyrolysis of lithium aluminotetrahydrides and deuterides, LiAlH4 and LiAlD4, was studied by 1H, 7Li, 27Al NMR in 20-700 deg C range. 20-30 time constriction of resonance lines of studied nuclei at 170 deg C testifies to melting of the compounds. It is shown that at LiAlD4 melting point the first stage of pyrolysis is described by two parallel reactions: LiAlD4 -> LiD + Al + D2, LiAlD4 + LiD -> Li3AlD6, which proceed with different rates. It was revealed that reactions of lithium hydride (deuteride) with metallic aluminium at temperatures above 400 deg C resulted to formation of intermetallic compounds of LiAl and LiAl3 composition. LiAl is characterized by higher thermal stability, than LiAl3. 20 refs., 6 figs., 2 tabs

  7. Spectroscopic databases - A tool for structure elucidation

    Spectroscopic databases have developed to useful tools in the process of structure elucidation. Besides the conventional library searches, new intelligent programs have been added, that are able to predict structural features from measured spectra or to simulate for a given structure. The example of the C13NMR/IR database developed at BASF and available on STN is used to illustrate the present capabilities of online database. New developments in the field of spectrum simulation and methods for the prediction of complete structures from spectroscopic information are reviewed. (author). 10 refs, 5 figs

  8. Coupled channels description of single and mutual excitation in the scattering of 7Li from 12C and 24, 26Mg

    Cook, J.; Clarice, N. M.; Coopersmith, J.; Griffiths, R. J.

    1982-09-01

    Coupled channels calculations have been made for the scattering of 7Li from 12C at 63 and 79 MeV and from 24,26Mg at 88 MeV. The calculations describe, simultaneously, the elastic scattering, excitation of 7Li to the 478 keV {1}/{2}- state, excitation of the target to its first 2 + state, and the mutual excitation of both projectile and target to their {1}/{2}- and 2 + states respectively. The potentials have been calculated by a double folding model using the M3Y effective interaction for the real part, and a gaussian effective interaction for the imaginary part. Realistic densities have been used for the ground states of 7Li, 12C and 24, 26Mg and also the transition densities to the excited states using a microscopic plus macroscopic prescription. For the mutual excitation, both one-step processes with l = 0, 2 and 4 and two-step processes were included. The calculations show that the two-step processes are the dominant contribution to the mutual excitation, but at forward angles, the oscillations in the data are only reproduced with the coherent addition of the one-step processes, which are dominated by the l = 4 contribution. Even when coupling to all single and mutual excitations are included the real potential still requires a normalization of about 0.6. The addition of the quadrupole re-orientation matrix element for the ground state does not significantly change this value. These calculations confirm that the coupling to the first excited inelastic levels of target and ejectile is not the source of the anomalous M3Y normalization, and that the dominant mode for mutual excitation is a two-step process. However, direct one-step mutual excitation is important for small angles (θ ≲ 20°).

  9. Coupled channels description of single and mutual excitation in the scatttering of /sup 7/Li from /sup 12/C and sup(24,26)Mg

    Cook, J.; Clarke, N.M.; Coopersmith, J.; Griffiths, R.J. (King' s Coll., London (UK). Wheatstone Physics Lab.)

    1982-09-27

    Coupled channels calculations have been made for the scattering of /sup 7/Li from /sup 12/C at 63 and 79 MeV and from sup(24,26)Mg at 88 MeV. The calculations describe, simultaneously, the elastic scattering, excitation of /sup 7/Li to the 478 keV 1/2/sup -/ state, excitation of the target to its first 2/sup +/ state, and the mutual excitation of both projectile and target to their 1/2/sup -/ and 2/sup +/ states respectively. The potentials have been used for the ground states of /sup 7/Li, /sup 12/C and sup(24,26)Mg and also the transition densities to the excited states using a microscopic plus macroscopic prescription. For the mutual excitation, both one-step processes with iota = 0, 2 and 4 and two-step processes were included. The calculations show that the two-step processes are the dominant contribution to the mutual excitation, but at forward angles, the oscillations in the data are only reproduced with the coherent addition of the one-step processes, which are dominated by the iota = 4 contribution. Even when coupling to all single and mutual excitations are included the real potential still requires a normalization of about 0.6. The addition of the quadrupole re-orientation matrix element for the ground state dows not significantly change this value. These calculations confirm that the coupling to the first excited inelastic levels of target and ejectile is not the source of the anomalous M3Y normalization, and that the dominant mode of mutual excitation is a two-step processes. However, direct one-step mutual excitation is important for small angles (THETA approx. <= 20/sup 0/).

  10. Coupled channels description of single and mutual excitation in the scatttering of 7Li from 12C and sup(24,26)Mg

    Coupled channels calculations have been made for the scattering of 7Li from 12C at 63 and 79 MeV and from sup(24,26)Mg at 88 MeV. The calculations describe, simultaneously, the elastic scattering, excitation of 7Li to the 478 keV 1/2- state, excitation of the target to its first 2+ state, and the mutual excitation of both projectile and target to their 1/2- and 2+ states respectively. The potentials have been used for the ground states of 7Li, 12C and sup(24,26)Mg and also the transition densities to the excited states using a microscopic plus macroscopic prescription. For the mutual excitation, both one-step processes with iota = 0, 2 and 4 and two-step processes were included. The calculations show that the two-step processes are the dominant contribution to the mutual excitation, but at forward angles, the oscillations in the data are only reproduced with the coherent addition of the one-step processes, which are dominated by the iota = 4 contribution. Even when coupling to all single and mutual excitations are included the real potential still requires a normalization of about 0.6. The addition of the quadrupole re-orientation matrix element for the ground state dows not significantly change this value. These calculations confirm that the coupling to the first excited inelastic levels of target and ejectile is not the source of the anomalous M3Y normalization, and that the dominant mode of mutual excitation is a two-step processes. However, direct one-step mutual excitation is important for small angles (THETA approx. 0). (orig.)

  11. Formation of 1:1 and 2:1 host-guest inclusion complexes of α-cyclodextrin with cycloalkanols: A 1H and 13C NMR spectroscopic study

    Akita, Tomoki; Yoshikiyo, Keisuke; Yamamoto, Tatsuyuki

    2014-09-01

    Binding constants (Ka's) for the formation of inclusion complexes of α-cyclodextrin (α-CD) with cycloalkanols (c-CnOH; n = 4-8) were determined by means of 1H and 13C NMR titration, under two different conditions: (i) only 1:1 host-guest inclusion complexes are formed when the guest is in excess; (ii) the formation of 2:1 inclusion complexes occurs only after that of 1:1 inclusion complexes, when the host is in excess. The results of this work showed that α-CD can include c-C4OH or c-C5OH only when the molar ratio is 1:1; larger ring-sized cycloalkanols such as c-C6OH, c-C7OH or c-C8OH can be included only when the molar ratio is 2:1. These findings, together with those obtained for the four derivatives of α-CD, per-6-O-methyl-α-CD, per-2-O-methyl-α-CD, per-3-O-methyl-α-CD, and per-2,6-di-O-methyl-α-CD, suggested that α-CD forms 2:1 inclusion complexes with c-C6OH, c-C7OH or c-C8OH in a tail-to-tail manner, in which the secondary hydroxy sides of the two CD molecules face each other. Two-dimensional ROESY measurements confirmed our results.

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

    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.

  13. Thermochromism in nickel(II) complexes: thermal, IR spectroscopic, solid-state 1H NMR and single crystal X-ray analysis of diaqua-bis(2,2-dimethyl-1,3-propanediamine) nickel(II) nitrate

    Koner, Subratanath; Ghosh, Ashutosh; Pariya, Chandi; Das, Debasis; Kikuchi, Hikomitsu; Okamoto, Ken-Ichi; Ikeda, Ryuichi

    1995-02-01

    The newly synthesized complex [Ni(dmtn) 2(H 2O) 2](NO 3) 2 (dmtn = 2,2-dimethyl-1,3-propanediamine) undergoes a reversible thermochromic phase transition in the range of 180-202°C ( ΔH = 10.4kJ mol -1) on heating after dehydration (dehydration temperature range 43-102°C). The complex has been characterized by X-ray crystallography at room temperature. The crystals are monoclinic, space group {C2}/{m}, a = 20.385(2), b = 6.9004(4), c = 6.9552(3) Å, β = 102.60(5)°, V = 954.8(1) Å3, Z = 2 and R = 0.046. The geometry of the nickel atom in the complex is tetragonally distorted octahedral with two H 2O molecules coordinated at the trans position. The diamine chelate rings are in the trans chair-chair conformations. The broad-line 1H NMR of partially deuterated [Ni(dmtn- d4) 2(NO 3) 2] (deuterated amine protons) indicates the onset of dynamic disorder of the diamine chelate rings at the phase transition temperature. The high temperature IR spectral measurement shows the complex retains its trans configuration after dehydration and phase transition with NO -3 ions coordinated as a monodentate ligand.

  14. 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.

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

    2014-10-24

    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. PMID:25459717

  15. 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

    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.

  16. 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

    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.

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

    Olsen, Kjeld J; Hansen, Johnny

    1984-01-01

    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...

  18. HOTSPUR progress report: neutron source spectrum characterization, and 6Li(n,xα) and 7Li(n,xα) cross section determination

    As a prerequisite to high accuracy measurements involving the bulk configuration of 6LiD we must have a good grasp of the details of the RTNS-I neutron source energy spectrum. Experiments to this end involving neutron yield vs deuteron energy, ratios of foil activation of selected elements, and pulse height distributions of a Si surface barrier detector are described. With this knowledge, the 4He-production cross sections for 6Li and 7Li are found experimentally to be 0.512b and 0.336b, respectively, at anti E/sub N/ = 15.0 MeV in free-field geometry. 14 references

  19. Quantum effects in the case of (6)Li+ and (7)Li+ ions evolving in a neutral (6)Li gas at a wide range of temperatures.

    Bouchelaghem, F; Bouledroua, M

    2014-02-01

    This work deals with the quantum-mechanical calculation of the temperature-dependent mobility of ionic lithium atoms diffusing in their parent gas. The computation of the quantal phase shifts in connection with the gerade and ungerade potential-energy curves, through which Li(+) approaches Li(2s), leads to the computation of the charge-transfer and diffusion cross sections. The behavior of the coefficients of diffusion and mobility with temperature is also examined. Throughout this work, the isotopic effects in the (6)Li(+)-(6)Li and (7)Li(+)-(6)Li collisions are emphasized. PMID:24326775

  20. Branching ratio of 8Be* high excited states in the 10B(dα)2α and 10B(dα)p7Li reaction

    Three-particle channels of 10B(dα)2α and 10B(dα)p7Li reactions with the excitation of short-living 19.86, 4+ and 20.1 MeV, 2+ state of 8Be* nucleus are investigated under 13.6 MeV incident deuteron energy in kinematically complete experiment. Angular correlation functions for these states and branching ratio by α-particle and proton channels are obtained. Spatial anisotropy of 8Be* nucleus parameter change as of two-cluster non-isolated subsystem is revealed

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

    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)

  2. NMR studies of metabolism

    In this paper, the authors present applications of NMR to the study of different aspects of metabolism. The authors begin with a brief outline of localization methods that are commonly used to obtain in vivo NMR spectra. The authors then describe in more detail metabolic information recently obtained by NMR of perfused organs, intact animals, and humans. Previous reviews have already covered the applications of NMR to the study of metabolism in microorganisms, isolated or cultivated cells, and tumors. NMR spectroscopy of the brain, and human in vivo NMR spectroscopy have also been reviewed

  3. Structural characterisation of amorphous materials by solid state NMR

    Mollison, N B

    2002-01-01

    Solid state nuclear magnetic resonance (NMR) is a structural elucidation technique that is ideal as a probe in the investigation of atomic structure of highly complex amorphous materials. In this study, NMR is employed in the structural characterisation of a series of sodium-lithium disilicate glasses. These so-called 'mixed-alkali' glasses are of great scientific interest, since they exhibit non-linear ionic transport related properties; the theory of which is not understood, but is thought to be related to the cation distribution in the disilicate network. This project attempts to utilise solid state NMR to its fullest potential, by combining several techniques, including the novel MQMAS experiment and a series of double resonance measurements. The double resonance techniques TRAPDOR and SEDOR have been attempted to measure sup 2 sup 9 Si-left brace sup 2 sup 3 Na right brace and sup 6 sup , sup 7 Li-left brace sup 7 sup , sup 6 Li right brace interactions respectively. Since these experiments rely on the d...

  4. Stereochemistry Determination by Powder X-ray Diffraction Analysis and NMR Spectroscopy Residual Dipolar Couplings

    Garcia, M.; Pagola, S; Navarro-Vasquez, A; Phillips, D; Gayathri, C; Krakauer, H; Stephens, P; Nicotra, V; Gil, R

    2009-01-01

    A matter of technique: For a new steroidal lactol, jaborosalactol 24 (1), isolated from Jaborosa parviflora, NMR spectroscopy residual dipolar couplings and powder X-ray diffraction analysis independently gave the same stereochemistry at C23-C26. Conventional NMR spectroscopic techniques, such as NOE and {sup 3}J coupling-constant analysis failed to unambiguously determine this stereochemistry.

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

    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...

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

    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. Study of the reduction in detection limits of track detectors used for 10B(n,α)7Li reaction rate measure through annealing and chemical etching experiments

    The Boron Neutron Capture Therapy (BNCT) is an experimental radiotherapy for cancer treatment. It is based on 10B(n, α)7Li 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 the10B(n, α)7Li 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)

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

    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.

  9. Microdosimetry spectra and RBE of {sup 1}H, {sup 4}He, {sup 7}Li and {sup 12}C nuclei in water studied with Geant4

    Burigo, Lucas, E-mail: burigo@fias.uni-frankfurt.de [Frankfurt Institute for Advanced Studies, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany); Institut für Theoretische Physik, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany); Pshenichnov, Igor, E-mail: pshenich@fias.uni-frankfurt.de [Frankfurt Institute for Advanced Studies, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany); Institute for Nuclear Research, Russian Academy of Sciences, 117312 Moscow (Russian Federation); Mishustin, Igor [Frankfurt Institute for Advanced Studies, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany); Kurchatov Institute, Russian Research Center, 123182 Moscow (Russian Federation); Bleicher, Marcus [Frankfurt Institute for Advanced Studies, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany); Institut für Theoretische Physik, Johann Wolfgang Goethe University, 60438 Frankfurt am Main (Germany)

    2014-02-01

    A Geant4-based Monte Carlo model for Heavy-Ion Therapy (MCHIT) is used to study radiation fields of {sup 1}H, {sup 4}He, {sup 7}Li and {sup 12}C beams with similar ranges (∼160–180 mm) in water. Microdosimetry spectra are simulated for wall-less and walled Tissue Equivalent Proportional Counters (TEPCs) placed outside or inside a phantom, as in experiments performed, respectively, at NIRS, Japan and GSI, Germany. The impact of fragmentation reactions on microdosimetry spectra is investigated for {sup 4}He, {sup 7}Li and {sup 12}C, and contributions from nuclear fragments of different charge are evaluated for various TEPC positions in the phantom. The microdosimetry spectra measured on the beam axis are well described by MCHIT, in particular, in the vicinity of the Bragg peak. However, the simulated spectra for the walled TEPC far from the beam axis are underestimated. Relative Biological Effectiveness (RBE) of the considered beams is estimated using a modified microdosimetric-kinetic model. Calculations show a similar rise of the RBE up to 2.2–2.9 close to the Bragg peak for helium, lithium and carbon beams compared to the modest values of 1–1.2 at the plateau region. Our results suggest that helium and lithium beams are also promising options for cancer therapy.

  10. Relation between (e,e') sum rules in 6,7Li and 4He nuclei.Experiment and cluster model

    Efros, V D; Buki, A Yu

    2016-01-01

    The sums over (e,e') spectra of 6Li and 7Li 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 alpha-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^{-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^{-1} the longitudinal correlation functions of 6Li and 7Li nuclei are found to be close to that of the alpha-particle. The experimental longitudinal sums in the range between 0.450 and 1.625 fm^{-1} are employed to perform comparison with those calculated in the framework of cluster models. Out of the mentioned experimental sums, those in the range between 0.750 and 1.000 fm^{-1} in the 6Li case ...

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

    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...

  12. NMR analysis of biodiesel

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

  13. 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

    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

  14. Search for the p1/2- resonance in 7He with the 7Li(d,2He) reaction and measurement of the deuteron electrodisintegration under 180 deg at the S-DALINAC

    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 7He 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 p1/2- spin-orbit partner of the 7He ground state with a dominant p3/2- single-particle character. In order to clarify this question a study of the 7Li(d,2He)7He 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 ΔE ∼ 150 keV (FWHM) in the measured spectra, better than the line width of the ground state of 7He. The unbound 2He system was identified by detecting coincidences between two protons with small relative energy. The data were taken over the angular range Θcm=0 -11.3 . A possible resonance at an excitation energy Ex=(1.45-0.5+0.7) MeV with a width Γ=(2.0-1.1+1.0) MeV is suggested by a decomposition of the spectrum using known resonances, the breakup behaviour of 7He and quasifree charge-exchange contributions, taking into account the cluster structure of 7Li. Gamow-Teller strengths for transitions to the lowest states in 7He are in remarkable agreement with results from ab initio Quantum Monte Carlo calculations. The neutron spectroscopic factor Sn=0.64±0.09 of the 7He ground state (7He=6He x n) is extracted by an R-matrix analysis. In the second part of the thesis the deuteron breakup has been studied in the 2H(e,e') reaction at Θ=180 . The present measurements were performed in March and April 2006 at the superconducting Darmstadt electron linear accelerator S-DALINAC at an incident electron energy E0=27.8 MeV and 74 MeV. At low momentum transfer (q=0.28 fm-1 and 0.73 fm-1, respectively

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

    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.

  16. Structure elucidation and conformational analysis of the sesquiterpene tremulenedial by inverse detection NMR and NOE experiments

    Phellinus tremulae produced a series of new sesquiterpenes possessing a previously unreported carbon skeleton, which was called tremulane. The spectroscopic analysis was performed in the dibenzyl derivative and was mainly based on inverse detection NMR and NOE experiments, although other NMR experiments were crucial for the structure elucidation. 1 H and 13 C NMR spectra and chemical shift data were shown. The stereochemistry was also studied

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

    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)

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

    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.

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

    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. (author)

  20. Structural investigations of humic acid from leonardite by spectroscopic methods and thermal analysis

    Ricca, G.; Federico, L.; Asteri, C.; Gallo, R. (Milan University, Milan (Italy). Dept. of Organic and Industrial Chemistry)

    1993-04-01

    Humic acid from leonardite, an immature coal, has been examined by spectroscopic methods (UV-VIS, IR-FT, H-1, P-31, C-13-NMR), mass spectrometry (FAB-MS) and thermal analysis. These techniques provided complementary information. A quantitative C-13-NMR technique was applied to this humic acid: the aromaticity calculated from the NMR data is high, about 76%, in agreement with mass spectrometric and thermal analysis data.

  1. A novel laser-collider used to produce monoenergetic 13.3 MeV 7Li (d, n) neutrons

    Zhao, J. R.; Zhang, X. P.; Yuan, D. W.; Li, Y. T.; Li, D. Z.; Rhee, Y. J.; Zhang, Z.; Li, F.; Zhu, B. J.; Li, Yan F.; Han, B.; Liu, C.; Ma, Y.; Li, Yi F.; Tao, M. Z.; Li, M. H.; Guo, X.; Huang, X. G.; Fu, S. Z.; Zhu, J. Q.; Zhao, G.; Chen, L. M.; Fu, C. B.; Zhang, J.

    2016-06-01

    Neutron energy is directly correlated with the energy of the incident ions in experiments involving laser-driven nuclear reactions. Using high-energy incident ions reduces the energy concentration of the generated neutrons. A novel “laser-collider” method was used at the Shenguang II laser facility to produce monoenergetic neutrons via 7Li (d, n) nuclear reactions. The specially designed K-shaped target significantly increased the numbers of incident d and Li ions at the keV level. Ultimately, 13.3 MeV neutrons were obtained. Considering the time resolution of the neutron detector, we demonstrated that the produced neutrons were monoenergetic. Interferometry and a Multi hydro-dynamics simulation confirmed the monoenergetic nature of these neutrons.

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

    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.

  3. A novel laser-collider used to produce monoenergetic 13.3 MeV (7)Li (d, n) neutrons.

    Zhao, J R; Zhang, X P; Yuan, D W; Li, Y T; Li, D Z; Rhee, Y J; Zhang, Z; Li, F; Zhu, B J; Li, Yan F; Han, B; Liu, C; Ma, Y; Li, Yi F; Tao, M Z; Li, M H; Guo, X; Huang, X G; Fu, S Z; Zhu, J Q; Zhao, G; Chen, L M; Fu, C B; Zhang, J

    2016-01-01

    Neutron energy is directly correlated with the energy of the incident ions in experiments involving laser-driven nuclear reactions. Using high-energy incident ions reduces the energy concentration of the generated neutrons. A novel "laser-collider" method was used at the Shenguang II laser facility to produce monoenergetic neutrons via (7)Li (d, n) nuclear reactions. The specially designed K-shaped target significantly increased the numbers of incident d and Li ions at the keV level. Ultimately, 13.3 MeV neutrons were obtained. Considering the time resolution of the neutron detector, we demonstrated that the produced neutrons were monoenergetic. Interferometry and a Multi hydro-dynamics simulation confirmed the monoenergetic nature of these neutrons. PMID:27250660

  4. Radiative transition probabilities for the B 1PI - X 1SIGMA+ and B 1PI - A 1SIGMA+ of 7LiH

    The recently reported (J. Chem. Phys. 66, 5412 (1977)) hybrid potential curves for the X 1Σ+ and A 1Σ+ states of LiH and the herein reported hybrid potential curve for the B 1Pi state of LiH are combined with the ab initio transition moments of Docken and Hinze (J. Chem. Phys. 57, 4936 (1972)) to calculate radiative transition probabilities between all B 1Pi (v' less than or equal to 2) and all X 1Σ+ (v'' less than or equal to 23) and A 1Σ+ (v'' less than or equal to 26) vibrational levels of 7LiH. The strongest single emission band found is the B 1Pi (v' = 2) → X 1Σ+ (v'' = 23) band between the highest ''long-range'' levels in each potential. For all B 1Pi levels, the emission is dominated by B → X rather than B → A emission

  5. A novel laser-collider used to produce monoenergetic 13.3 MeV 7Li (d, n) neutrons

    Zhao, J. R.; Zhang, X. P.; Yuan, D. W.; Li, Y. T.; Li, D. Z.; Rhee, Y. J.; Zhang, Z.; Li, F.; Zhu, B. J.; Li, Yan F.; Han, B.; Liu, C.; Ma, Y.; Li, Yi F.; Tao, M. Z.; Li, M. H.; Guo, X.; Huang, X. G.; Fu, S. Z.; Zhu, J. Q.; Zhao, G.; Chen, L. M.; Fu, C. B.; Zhang, J.

    2016-01-01

    Neutron energy is directly correlated with the energy of the incident ions in experiments involving laser-driven nuclear reactions. Using high-energy incident ions reduces the energy concentration of the generated neutrons. A novel “laser-collider” method was used at the Shenguang II laser facility to produce monoenergetic neutrons via 7Li (d, n) nuclear reactions. The specially designed K-shaped target significantly increased the numbers of incident d and Li ions at the keV level. Ultimately, 13.3 MeV neutrons were obtained. Considering the time resolution of the neutron detector, we demonstrated that the produced neutrons were monoenergetic. Interferometry and a Multi hydro-dynamics simulation confirmed the monoenergetic nature of these neutrons. PMID:27250660

  6. Lithium isotope separation by 6Li/7Li countercurrent exchange between lithium-amalgam and aqueous LiOH in a spray column

    Lithium isotope separation by 6Li/7Li exchange between lithium-amalgam and aqueous LiOH has been investigated by using a column consisting of a vertical Pyrex glass tube in which aqueous LiOH flows up and a fine spray of lithium-amalgam falls down. As the number of theoretical plates, a value of 48 was obtained on a single column while the amalgam stability was η = 0.74, where η is the ratio between Li concentration in amalgam at the column bottom and that at the column top. That is, a large separation may be obtained in a single column in spite of amalgam decomposition which takes place as a side reaction. (author)

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

    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.

  8. Spectator invariance test in the study of the Trojan Horse Method 6,7Li fusion reactions via the Trojan Horse Method

    Li C.

    2011-10-01

    Full Text Available Fusion reactions play a crucial role for several astrophysical scenarios. At the low energies typical of such environments direct measurements of reaction cross sections are very difficult, and even sometimes impossible. In such cases the use of indirect methods can give a substantial help. The Trojan Horse Method (THM is based on the quasi-free break-up of a nucleus, which can be described in terms of a cluster structure. In such applications the independence of THM results with different break-up schemes, was tested using the quasi free3 He(6Li,ααH and 3He(7Li,αα2H reactions. Results were then compared with the direct behaviours obtained from available data as well as with the cross sections extracted from previous indirect investigations of the same binary reactions using a different nuclide as a Trojan Horse nucleus.

  9. Search for solar axion emission from $^7$Li and D(p,$\\gamma)^3$He nuclear decays with the CAST $\\gamma$-ray calorimeter

    Andriamonje, S; Autiero, D; Barth, K; Belov, A; Beltran, B; Brauninger, H; Carmona, J M; Cebrian, S; Collar, J I; Dafni, T; Davenport, M; Di Lella, L; Eleftheriadis, C; Englhauser, J; Fanourakis, G; Ferrer-Ribas, E; Fischer, H; Franz, J; Friedrich, P; Geralis, T; Giomataris, I; Gninenko, S; Gomez, H; Hasinoff, M; Heinsius, F H; Hoffmann, D.H H; Irastorza, I G; Jacoby, J; Jakovcic, K; Kang, D; Konigsmann, K; Kotthaus, R; Krcmar, M; Kousouris, K; Kuster, M; Lakic, B; Lasseur, C; Liolios, A; Ljubicic, A; Lutz, G; Luzon, G; Miller, D W; Morales, J; Ortiz, A; Papaevangelou, T; Placci, A; Raffelt, G; Riege, H; Rodriguez, A; Ruz, J; Savvidis, I; Semertzidis, Y; Serpico, P; Stewart, L; Vieira, J D; Villar, J; Vogel, J; Walckiers, L; Zioutas, K

    2010-01-01

    We present the results of a search for a high-energy axion emission signal from 7Li (0.478 MeV) and D(p,gamma)3He (5.5 MeV) nuclear transitions using a low-background gamma-ray calorimeter during Phase I of the CAST experiment. These so-called "hadronic axions" could provide a solution to the long-standing strong-CP problem and can be emitted from the solar core from nuclear M1 transitions. This is the first such search for high-energy pseudoscalar bosons with couplings to nucleons conducted using a helioscope approach. No excess signal above background was found.

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

    Ibraheem, Awad A.; Aygun, M.

    2016-06-01

    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.

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

    Highlights: • Full material characterization as far as hydrogen transport properties are concern. • Quantification of permeator leaks and material degasification. • Analysis of H2 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

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

    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.

  13. NMR at 900 MHz

    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.

  14. NMR studies of nucleic acid dynamics

    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.

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

    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.

  16. 31P NMR Study on Some Phosphorus-Containing Compounds

    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.

  17. Lectures on pulsed NMR

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

  18. Lectures on pulsed NMR

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

  19. Diffraction dissociation of {sup 7}Li and {sup 7}Be relativistic nuclei on proton targets through the {sup 3}H({sup 3}He)+{sup 4}He channels

    Fetisov, V. N., E-mail: ffetisov@mail.ru [Russian Academy of Sciences, Lebedev Physical Institute (Russian Federation)

    2015-07-15

    For the fragmentation of {sup 7}Li and {sup 7}Be relativistic nuclei (with momenta of, respectively, P = 3 GeV/c and P = 1.6 GeV/c per nucleon) on proton targets through the {sup 3}H({sup 3}He) + {sup 4}He channels, the differential cross sections with respect to the momentum transfer Q to the fragments were calculated on the basis of the cluster version of Akhiezer–Glauber–Sitenko diffraction theory by employing the twobody cluster model for the {sup 7}Li ({sup 3}H + {sup 4}He) and {sup 7}Be ({sup 3}He + {sup 4}He) nuclei. These calculations, performed in the impulse approximation in the interaction of intranuclear clusters with the target nucleus, explained a strong suppression of the cross sections for reactions on protons at Q lower than 100 MeV/c and higher than 350 MeV/c and the observed irregularities in the behavior off the cross section for {sup 7}Li fragmentation on complex track-emulsion nuclei. Cross-section values close to their experimental counterparts were obtained upon setting the coefficient of two-body clustering in the {sup 7}Li and {sup 7}Be nuclei to k ≃ 0.7.

  20. TL response of pairs of 6LiF:Mg,Cu,Si/7LiF:Mg,Cu,Si and TLD-600/TLD-700 to 0.1–12 MeV neutrons

    Neutron dosimetery continues to remain an important and a challenging aspect of radiation protection due to the higher biological effectiveness of neutrons than that of gamma rays and the intricacy in the responses of the detectors. The need for personal dosimetry in mixed fields of neutrons and gamma rays has considerably increased due to the rising number of nuclear facilities, nuclear power plants, medical therapy equipment, accelerators and so on. The most widely used technique for personal dosimetry has been the albedo technique employing pairs of neutron sensitive 6LiF:Mg,Ti (TLD-600) and neutron insensitive 7LiF:Mg,Ti (TLD-700) thermoluminescent dosimeters (TLDs). Off late, LiF:Mg,Cu,Si has emerged as one of the most promising TLD material, having the advantages of high sensitivity, near tissue equivalence to gamma rays, negligible fading on pre and post-irradiation storage, thermal stability for readout and negligible residual signal after the readout. In this study, neutron energy response of indigenously developed 6LiF:Mg,Cu,Si and 7LiF:Mg,Cu,Si TLD pairs was evaluated to neutrons of energy from thermal to 11.6 MeV and was compared with the response of TLD-600 and TLD-700 pairs. The net TL per unit neutron dose for the 6LiF:Mg,Cu,Si/7LiF:Mg,Cu,Si TLD pair was found to be about 10 times of that of the TLD-600/TLD-700 pair. Unlike, TLD-600 and TLD-700, the glow curve structure of 6LiF:Mg,Cu,Si and 7LiF:Mg,Cu,Si remained almost the same for all the irradiations. Thus, 6LiF:Mg,Cu,Si and 7LiF:Mg,Cu,Si TLDs provided a better alternate to TLD-600 and TLD-700 for the dosimetry of mixed fields of neutrons and gamma rays. -- Highlights: ► High sensitivity 6Li and 7Li enriched LiF:Mg,Cu,Si TLDs have been developed at KAERI, Korea. ► Main TL glow peak remains unchanged for 6Li and 7Li enrichment and radiation type. ► Net TL/mSv is about 10 times of that of TLD-600/TLD-700 pairs

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

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

    2011-08-01

    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. PMID:21698335

  2. BOOK REVIEW: NMR Imaging of Materials

    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

  3. NMR spectroscopic studies of organocopper compounds and Zintl anions

    Neumeier, Maria

    2013-01-01

    The breath-taking development and the frequent use of organocuprates illustrate their synthetic importance for regio- and diastereoselective carbon-carbon bond formation reactions. Since their discovery by Gilman, organocuprates are the focus of proceeding studies. Empiric optimization of reaction conditions motivated the clarification of the reaction mechanism, forming the basis for further improvements. A lot of expertise was spent on the structure elucidation of organocuprates in the solid...

  4. Structure, dynamics and reactivity of carbohydrates : NMR spectroscopic studies

    Rönnols, Jerk

    2013-01-01

    The main focus of this thesis is on the ring conformations of carbohydrate molecules; how the conformational equilibria and the rates of the associated interconversions are affected by the molecular constitution and their surroundings. The conformational equilibria of a group of amine linked pseudodisaccharides, designed as potential glycosidase inhibitors, comprising α-D-altrosides are described in Chapter 3. The OS2 conformation was largely populated, and the ring conformation was found to ...

  5. NMR spectroscopic studies of 15N labelled geminally disubstituted cyclotriphosphazenes

    It is demonstrated by means of some selected 15N labelled geminally disubstituted cyclotriphosphazenes, 15N3P3X4Y2 (X = Cl; Y = F, NH2, or SEt), as an example, that the coupling constants 1Jsub(PN) may be of different signs. The absolute value of 1Jsub(PN) is significantly influenced only by those substituents, which are bonded to the phosphorus nucleus directly concerned in the coupling. Also the 15N chemical shifts are only changed by substituents on directly bonded phosphorus atoms. (author)

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

    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 studies in different contexts. The potential of ssNMR to determine molecular structure is illustrated by means of a homopolymeric protein hydrogel with sequence similarities to the scNsp1p nucleop...

  7. Near-threshold 7Li(p,n)7Be neutrons on the practical conditions using thick Li-target and Gaussian proton energies for BNCT

    The near threshold 7Li(p,n)7Be neutrons generated by incident proton energy having Gaussian distribution with mean energies from 1.85 to 1.95 MeV, were studied as a practical neutron source for BNCT wherein an RFQ accelerator and a thick Li-target are used. Gaussian energy distributions with the standard deviation of 0, 10, 20 and 40 keV for mean proton energies from 1.85 to 1.95 MeV were surveyed in 0.01 MeV increments. A thick liquid Li-target whose dimensions were established in our previous experiments (i.e., 1 mm-thick with 50 mm width and 50 mm length) was considered in this study. The suitable incident proton energy and physical dimensions of Pb layer which serves as a gamma absorber and a Polyethylene layer which is used as a BDE were surveyed by means of the concepts of TPD. Dose distribution were calculated by using MCNP5. A proton beam with mean energy of 1.92 MeV and a Gaussian energy distribution with a standard deviation of 20 keV at a current of 10 mA was selected from the viewpoint of irradiation time and practically achievable proton current. The suitable thicknesses of Pb gamma absorber was estimated to be about 3 cm. The estimated thickness of the polyethylene BDE was about 24 mm for an ideal proton current of 13 mA, and was 18 mm for a practical proton current of 10 mA. - Highlights: • Proton enrgy from 1.85 to 1.95 MeV were studied for near threshold 7Li(p,n)7Be neutrons. • Practical conditions were applied for RFQ type accelerator and a thick Li-target. • Gaussian distribution of proton energies were checked for the standard deviation of 0, 10, 20 and 40 keV. • The mean energy of 1.92 MeV protons with Gaussian distribution of 20 keV was feasible. • The suitable thicknesses of Lead layer as gamma absorber was about 3 cm. • The suitable thicknesses of polyethylene BDE was about 24 mm at the proton current of 13 mA

  8. Development of liquid-lithium film jet-flow for the target of 7Li(p,n)7Be reactions for BNCT

    A feasibility study on liquid lithium target in the form of a flowing film was performed to evaluate its potential use as a neutron generation target of 7Li(p,n)7Be reaction in BNCT. The target is a windowless-type flowing film on a concave wall. Its configuration was adapted for a proton beam which is 30 mm in diameter and with energy and current of up to 3 MeV and 20 mA, respectively. The flowing film of liquid lithium was 0.6 mm in thickness, 50 mm in width and 50 mm in length. The shapes of the nozzle and concave back wall, which create a stable flowing film jet, were decided based on water experiments. A lithium hydrodynamic experiment was performed to observe the stability of liquid lithium flow behavior. The flowing film of liquid lithium was found to be feasible at temperatures below the liquid lithium boiling saturation of 342 °C at the surface pressure of 1×10−3 Pa. Using a proto-type liquid lithium-circulating loop for BNCT, the stability of the film flow was confirmed for velocities up to 30 m/s at 220 °C and 250 °C in vacuum at a pressure lower than 10−3 Pa. It is expected that for practical use, a flowing liquid lithium target of a windowless type can solve the problem of radiation damage and target cooling. - Highlights: • A feasibility study of liquid lithium target was performed for the 7Li(p,n)7Be reaction for BNCT. • The flowing film on the concave wall is a windowless type target. • The flowing film of liquid lithium was feasible at temperatures below 342 °C at a pressure of 1×10−3 Pa. • The stability of the film flow was confirmed up to 30 m/s at 220 °C at a pressure of 10−3 Pa. • Flowing liquid lithium target of a windowless type can solve both radiation damage and cooling

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

    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. PMID:9716484

  10. Localized double-quantum-filtered 1H NMR spectroscopy

    Thomas, M. A.; Hetherington, H. P.; Meyerhoff, D. J.; Twieg, D. B.

    The image-guided in vivo spectroscopic (ISIS) pulse sequence has been combined with a double-quantum-filter scheme in order to obtain localized and water-suppressed 1H NMR spectra of J-coupled metabolites. The coherence-transfer efficiency associated with the DQ filter for AX and A 3X spin systems is described. Phantom results of carnosine, alanine, and ethanol in aqueous solution are presented. For comparison, the 1H NMR spectrum of alanine in aqueous solution with the binomial (1331, 2662) spin-echo sequence is also shown.

  11. In situ solid-state NMR spectroscopy of electrochemical cells: batteries, supercapacitors, and fuel cells.

    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

  12. Li dynamics in carbon-rich polymer-derived SiCN ceramics probed by NMR

    Baek, Seung-Ho; Reinold, Lukas; Graczyk-Zajac, Magdalena; Riedel, Ralf; Hammerath, Franziska; Buechner, Bernd; Grafe, Hajo

    2014-03-01

    We report 7Li, 29Si, and 13C NMR studies of two different carbon-rich SiCN ceramics SiCN-1 and SiCN-3 derived from the preceramic polymers polyphenylvinylsilylcarbodiimide and polyphenylvinylsilazane, respectively. From the spectral analysis of the three nuclei at room temperature, we find that only the 13C spectrum is strongly influenced by Li insertion/extraction, suggesting that carbon phases are the major electrochemically active sites for Li storage. Temperature and Larmor frequency (ωL) dependences of the 7Li linewidth and spin-lattice relaxation rates T1-1 are described by an activated law with the activation energy EA of 0.31 eV and the correlation time τ0 in the high temperature limit of 1.3 ps. The 3 / 2 power law dependence of T1-1 on ωL which deviates from the standard Bloembergen, Purcell, and Pound (BPP) model implies that the Li motion on the μs timescale is governed by continuum diffusion mechanism rather than jump diffusion. On the other hand, the rotating frame relaxation rate T1ρ-1 results suggest that the slow motion of Li on the ms timescale may be affected by complex diffusion and/or non-diffusion processes.

  13. Spectroscopy of particle-phonon coupled states in $^{133}$Sb by the cluster transfer reaction of $^{132}$Sn on $^{7}$Li: an advanced test of nuclear interactions

    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 133Sb 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 only...

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

    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...

  15. A novel BNCT irradiation system with an on-line monitor using 7Li(P,N)7Be near threshold neutrons

    A neutron irradiation system for boron neutron capture therapy using accelerators with an online dose monitoring system was studied for the possible practical implementation of hospital-based BNCT. For this purpose the neutrons produced by the near threshold 7Li(p,n)7Be reaction, i.e. an incident proton energy of around 1.90 MeV, have suitable properties. Such as the maximum energy below 100 keV and mostly forward-directed. A good candidate material to shield gamma rays from the Li-target was Lead and the suitable boron-dose enhancer was polyethylene. The optimum physical dimensions and configuration of the irradiation system was determined using the concept of treatbale protocol depth as figures of merit. For the online monitor system, the single photon emission computed tomography using prompt gamma-ray was studied to provide an ideal dose estimation system. A neutron producing target system with a liquid lithium jet flow of about 30 m/s at a thickness of 1 mm and a cross-sectional area of 50 mm × 50 mm is proposed.

  16. R-matrix analysis of the 12C(α,γ) reaction with inputs from 12C(7Li,t)16O∗ transfer reaction

    The 12C(α,γ) reaction at 300 keV determines the ratio of 16O to 12C abundance at the end of helium burning in stars. The direct measurement of the cross-section of this reaction is almost impossible with the presently available techniques. Extrapolation of the cross-section or the astrophysical S-factor from higher energy data is presently adopted. There are several direct measurements of the 12C(α,γ) reaction but the lowest energy upto which measurement has been done is only upto 1 MeV. R-matrix extrapolation of the E2 and E1 capture data is complicated by the lack of knowledge of the cluster structure of the 6.92 MeV (2+) and 7.12 MeV (1-) states of 16O. In this paper we report a study of the E2 capture data that is analysed with the ANC of the 6.92 MeV state determined from 12C(7Li,t) alpha transfer measurements

  17. Levels in 148Tb excited by the (6Li,2n), (7Li,3n) and (10B,4n) reactions

    High spin states in 148Tb have been excited by means of 144Sm(6Li,2n), 144Sm(7Li,3n), and 142Nd(10B,4n) reactions and studied by γ-ray and electron measurements. Gamma-ray singles, excitation functions, angular distributions, internal conversion coefficients, and γ-γ coincidence measurements have been made. A seven-fold gamma-gamma cascade feeding the 9+ isomeric state in 148Tb and originating in a level 4137keV above that state is strongly excited. The spin and parity assignments are made on the basis of angular distribution and internal conversion coefficients. On the basis of these measurements, the 1006keV transition is E3 in character; the half-life of the 1006keV(12-) level is established to be 25 +- 2ns. These experiments also confirm the existence of a number of high spin states in 148Gd seen by earlier workers. (author)

  18. Manufacturing of thin films of boron for the measurement of the {sup 10}B(n, {alpha}){sup 7} Li reaction used in BNCT

    Smilgys, Barbara; Oliveira, Sandro Guedes de; Hadler Neto, Julio Cesar; Vellame, Igor Alencar [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Inst. de Fisica Gleb Wataghin; Soares, Cleber Jose; Salim, Leonardo Alfredo [Universidade Estadual Paulista (UNESP), Rio Claro, SP (Brazil). Inst. de Geociencias e Ciencias Exatas; Coelho, Paulo Rogerio Pinto [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Engenharia Nuclear

    2011-07-01

    Full text: The Boron Neutron Capture Therapy (BNCT) is considered to be a possible treatment for different types of aggressive cancers located in areas of difficult access or which already have metastasis. The working principle of this therapy is the selective delivery of a greater amount of boron to the tumor cells than to the healthy ones, followed by the neutron irradiation that will induce the emission of {alpha} particles through the {sup 10}B(n, {alpha}){sup 7} Li reaction used in BNCT reaction. The high energy deposition of the product particles causes the death of the cells and this therapy becomes much effective if the healthy tissue is less exposed to this radiation. The objective of this work is to develop a method for measuring the rate of this reaction by using thin films of boron. We have manufactured thin films with different concentrations of boron deposited on mica and the thin films were exposed to different irradiation time intervals at the reactor IEA-R1 located at IPEN, Sao Paulo. Here we show our first results on the density and uniformity of the thin films, where the detection of the particles is made using plastic track detectors (CR-39) which have their structures damaged by the passage of ions. (author)

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

    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.

  20. Li(+) Local Structure in Li-Tetraglyme Solvate Ionic Liquid Revealed by Neutron Total Scattering Experiments with the (6/7)Li Isotopic Substitution Technique.

    Saito, Soshi; Watanabe, Hikari; Hayashi, Yutaka; Matsugami, Masaru; Tsuzuki, Seiji; Seki, Shiro; Canongia Lopes, José N; Atkin, Rob; Ueno, Kazuhide; Dokko, Kaoru; Watanabe, Masayoshi; Kameda, Yasuo; Umebayashi, Yasuhiro

    2016-07-21

    Equimolar mixtures of lithium bis(trifluoromethanesulfonyl)amide (LiTFSA) and tetraglyme (G4: CH3O-(CH2CH2O)4-CH3) yield the solvate (or chelate) ionic liquid [Li(G4)][TFSA], which is a homogeneous transparent solution at room temperature. Solvate ionic liquids (SILs) are currently attracting increasing research interest, especially as new electrolytes for Li-sulfur batteries. Here, we performed neutron total scattering experiments with (6/7)Li isotopic substitution to reveal the Li(+) solvation/local structure in [Li(G4)][TFSA] SILs. The experimental interference function and radial distribution function around Li(+) agree well with predictions from ab initio calculations and MD simulations. The model solvation/local structure was optimized with nonlinear least-squares analysis to yield structural parameters. The refined Li(+) solvation/local structure in the [Li(G4)][TFSA] SIL shows that lithium cations are not coordinated to all five oxygen atoms of the G4 molecule (deficient five-coordination) but only to four of them (actual four-coordination). The solvate cation is thus considerably distorted, which can be ascribed to the limited phase space of the ethylene oxide chain and competition for coordination sites from the TFSA anion. PMID:27388117

  1. Functional studies using NMR

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

  2. Renal transplant NMR

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

  3. Discrete analysis of stochastic NMR.II

    Wong, S. T. S.; Rods, M. S.; Newmark, R. D.; Budinger, T. F.

    Stochastic NMR is an efficient technique for high-field in vivo imaging and spectroscopic studies where the peak RF power required may be prohibitively high for conventional pulsed NMR techniques. A stochastic NMR experiment excites the spin system with a sequence of RF pulses where the flip angles or the phases of the pulses are samples of a discrete stochastic process. In a previous paper the stochastic experiment was analyzed and analytic expressions for the input-output cross-correlations, average signal power, and signal spectral density were obtained for a general stochastic RF excitation. In this paper specific cases of excitation with random phase, fixed flip angle, and excitation with two random components in quadrature are analyzed. The input-output cross-correlation for these two types of excitations is shown to be Lorentzian. Line broadening is the only spectral distortion as the RF excitation power is increased. The systematic noise power is inversely proportional to the number of data points N used in the spectral reconstruction. The use of a complete maximum length sequence (MLS) may improve the signal-to-systematic-noise ratio by 20 dB relative to random binary excitation, but peculiar features in the higher-order autocorrelations of MLS cause noise-like distortion in the reconstructed spectra when the excitation power is high. The amount of noise-like distortion depends on the choice of the MLS generator.

  4. NMR clinical imaging and spectroscopy: Its impact on nuclear medicine

    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

  5. Temperature {sup 1}H, {sup 13}C, {sup 15}N NMR and CP/MAS {sup 15}N NMR spectra of benzotriazole derivatives - prototropic tautomerism; Widma temperaturowe {sup 1}H, {sup 13}C, {sup 15}N NMR oraz CP/MAS {sup 15}N NMR pochodnych benzotriazolu - tautomeria prototropowa

    Wiench, J.W.; Stefaniak, L. [Inst. Chemii Organicznej, Polska Akademia Nauk, Warsaw (Poland)

    1994-12-31

    The prototropic tautomerism in benzotriazole derivatives solutions has been investigated in different temperatures by means of {sup 1}H, {sup 13}C and {sup 15}N NMR and {sup 15}N CP/MAS NMR spectra. The ratio of different tautomeric forms and kinetics of proton exchange have been measured for the systems studied on the base of observed spectroscopic factors. 5 refs, 2 figs, 3 tabs.

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

    Santos, Maiara S.; Edenir R. Pereira-Filho; Antonio G. Ferreira; Elisangela F. Boffo; Figueira, Glyn M.

    2012-01-01

    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, ¹H HR-MAS NMR and ¹H NMR in solution, combined with chemo...

  7. Computer systems for laboratory networks and high-performance NMR.

    Levy, G C; Begemann, J H

    1985-08-01

    Modern computer technology is significantly enhancing the associated tasks of spectroscopic data acquisition and data reduction and analysis. Distributed data processing techniques, particularly laboratory computer networking, are rapidly changing the scientist's ability to optimize results from complex experiments. Optimization of nuclear magnetic resonance spectroscopy (NMR) and magnetic resonance imaging (MRI) experimental results requires use of powerful, large-memory (virtual memory preferred) computers with integrated (and supported) high-speed links to magnetic resonance instrumentation. Laboratory architectures with larger computers, in order to extend data reduction capabilities, have facilitated the transition to NMR laboratory computer networking. Examples of a polymer microstructure analysis and in vivo 31P metabolic analysis are given. This paper also discusses laboratory data processing trends anticipated over the next 5-10 years. Full networking of NMR laboratories is just now becoming a reality. PMID:3840171

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

    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.

  9. Analysis of the {sup 11}B({sup 7}Li, {sup 7}Be){sup 11}Be reaction at 57 MeV in a microscopic approach

    Cappuzzello, F. E-mail: cappuzzello@lns.infn.it; Lenske, H.; Cunsolo, A.; Beaumel, D.; Fortier, S.; Foti, A.; Lazzaro, A.; Nociforo, C.; Orrigo, S.E.A.; Winfield, J.S

    2004-07-12

    The {sup 11}B({sup 7}Li, {sup 7}Be){sup 11}Be charge exchange reaction has been studied at an incident energy of 57 MeV. Spectra were measured at forward angles, {theta}{sub cm}{<=}35 degrees. The good energy resolution ({approx}50 keV) allowed the identification of transitions both to the {sup 7}Be (3/2{sup -}, gs) and {sup 7}Be(1/2{sup -}, 429 keV) exit channels and hence the direct measurement of the ratio of the respective cross sections and angular distributions. Besides the bound ground and first excited state of {sup 11}Be several low lying excitations just above the neutron threshold are observed. A structure seen at E{sup *}=9.4 MeV with FWHM {approx}7 MeV is compatible with the spin dipole resonance (SDR). The data are analysed in a many-body approach. For the projectile transitions shell model results are used. In order to account properly for the special features of the weakly bound {sup 11}Be system the target transitions are described microscopically by Hartree-Fock-Bogoliubov (HFB) and quasi-particle random phase approximation (QRPA) theory. The HFB ground state densities and the QRPA transition densities, respectively, are used in folding calculations for the optical potentials and transition form factors. Spectra and {beta}-decay transitions strengths are reasonably well described. The measured cross section are well reproduced by one-step direct charge exchange distorted wave born approximation (DWBA) calculations. A dominance of unnatural parity transitions is found. This is explained in terms of the spin transfer behaviour of the nucleon-nucleon isovector interaction at low bombarding energy.

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

    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.

  11. 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

    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.

  12. 234U/238U - δ7Li - δ11B isotope systematics on aquifer groundwaters from deep scientific boreholes from the Meuse-Haute Marne site. Preliminary results

    direction more or less parallel to the groundwater flow, i.e. on a NWSE axis. The lowest activity ratios (0.54) are measured in the North (MSE 101 borehole), whereas sampling points located in the South (EST 322 borehole) display higher activity ratios, one of them being even slightly higher than the equilibrium (1.18). These U activities may still result from water-rock interaction processes, but may also indicate different flow rates of groundwaters characterized by U activity ratios largely lower than the equilibrium value at the recharge areas. In this case, the flow rate would be much higher in the North (234U/238U < 0.6) than in the South. Such a hypothesis is compatible with the presence of karstification at the recharge areas (Doc. Agence de l'Eau Rhin-Meuse). δ7Li and δ11B, measured in Oxfordian groundwaters range from 11.6 to 18.6 0/00 (with one exception) and from 0.75 to 19.9 0/00, respectively. Dogger groundwaters display lithium isotopic compositions that are comparable though more homogeneous (between 14.7 and 18 0/00), whereas boron isotopic compositions are much 'heavier', from 17.5 to 28.4 0/00. Hence waters derived from the two aquifers may be clearly distinguished when reported on a δ7Li vs. d11B diagram. It is noticeable that, in this diagram, Oxfordian groundwaters from boreholes EST 342 (this water may have been contaminated during sampling by contact to argillites which have been partly drilled before sampling of Oxfordian groundwater) and EST 421, as well as Dogger waters from boreholes EST 342 and EST 432 display isotopic signatures that are very comparable (δ11B ∼ 19 0/00; δ7Li ∼ 15.5 0/00). It is remarkable that these data are from the boreholes that are located on the Joinville - Commercy line (see above). Additional samples that have been recovered in the framework of the BULiTh research project are at present being analyzed. It is expected that the next results will help to propose a more comprehensive scheme for

  13. Contribution to the study of the influence of the Pauli principle and of its modelization in nuclear reactions between heavy ions: application to the reaction 7Li

    A simple model based on the Hackenbroich approach of the R.G.M. theory which simulates the Pauli principle among clusters has been derived in the following way. The exact antisymmetrization between the nucleon belonging to a given cluster has been kept. The contribution of the exchange terms between two different clusters, which give rise to non-local potentials, has been simulated by the matrix elements of an effective local, l-dependent, energy-independent nucleon-nucleon potential. With these potentials (added to the regular n-n interaction) the low energy levels of 8Be and 7Li as well as the phase shifts l=0,2,4 for α-α scattering and l=0 to 4 for α-n and α-t scattering for energies below 10MeV (c.m.) have been calculated. Good agreement between exact antisymmetrized and modelized calculations is achieved. With this model elastic and inelastic scattering of α on 7Li have been calculated. The 7Li has been described in terms of α,t clusters. The coupling with the 8Be + t channel has been taken into account. A good agreement between experimental data and modelized theoretical calculations is achieved when the projectile energy is less than 5MeV (lab. system). It appears that the coupling with the 8Be + t channel is not negligible even below this channel threshold

  14. The 10B(n,α)7Li reaction in PWR coolants: calculations of the effect on coolant pH and on decreases in 10B isotopic fractions

    Boron is used as a chemical shim in PWRs for reactivity control and is added in the form of boric acid to the primary coolant. The 10B(n,α)7Li reaction leads to a continuous increase in 7Li in the primary coolant and to a continuous decrease in 10B the isotope of boron responsible for control of reactivity. The rate of increase in coolant pH due to 7Li production is calculated for the Sizewell 'B' PWR to enable judgements to be made on the frequency of sampling and removal of lithium required to maintain the pH of the primary coolant within the desired limits. Calculations are contrasted for the cases of natural boron and 100% 10B chemical shims, for both a normal cycle and an extended 18 month cycle. Calculations of 10B depletion over 30 years of operation as a function of the quantity of boron discharged to waste are also presented. 10B isotopic fractions are calculated for the reactor coolant (RC), boric acid tanks (BATs) and refuelling water storage tank (RWST) assuming rapid mixing of BAT and RC boron for tritium control and other reasons. Such predictions enable assessments of the reactor physics implications of 10B consumption to be made. (author)

  15. NMR Aerosolomics: Novel NMR Method for Organic Aerosol Analysis

    Horník, Štěpán; Schwarz, Jaroslav; Sýkora, Jan

    - : -, 2015, s. 162. ISBN N. [Small Molecule NMR Conference - SMASH 2015. Baveno (IT), 20.09.2015-23.09.2015] Institutional support: RVO:67985858 Keywords : aerosol * analysis * NMR Subject RIV: CC - Organic Chemistry

  16. NMR imaging technique

    This invention provides a method that can be adapted to existing NMR tomographic scanners of producing spectra of any given point in the image of the specimen slice, the intensity distribution of a selected resonance within an area of the image of the specimen slice, or an entire NMR spectrum of the given area. The method comprises acquiring n projections of the specimen slice, where n is greater than 1. Each of the projections is then shifted by Δ f for the point (the frequency offset of the signal arising from the point, from the true chemical shift)

  17. Spectroscopic investigation of the interaction between β-cyclodextrin and ascorbic acid

    Inclusion compound of vitamin C (ascorbic acid) with β-cyclodextrin (β-CD), prepared by different methods (kneading, co-precipitation and freeze-drying) has been caracterized by several spectroscopic techniques (FTIR, 1H NMR, UV-Vis), powder X-ray diffraction and DSC technique. Based on the chemical shifts observed in the 1H-NMR and on FTIR spectra the tentative conclusion is that vitamin C probably enters the cyclodextrin torus forming the inclusion complex.

  18. Occurrence, biological activities and 13C NMR data of amides from Piper (Piperaceae

    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.

  19. Study of a Conformational Equilibrium of Lisinopril by HPLC, NMR, and DFT

    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

  20. Occurrence, biological activities and {sup 13}C NMR data of amides from Piper (Piperaceae)

    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)

  1. NMR a substitute for CT

    The possibility that NMR (Nuclear Magnetic Resonance) can be a substitute for CT (Computerized Tomography), is described. NMR focus on the nuclei in the atoms of certain elements, for example hydrogen

  2. International symposium on NMR spectroscopy

    The publication consists of 32 papers and presentations from the field of NMR spectroscopy applications submitted to the International Symposium on NMR Spectroscopy held at Smolenice between 29 Sep and 3 Oct, 1980. (B.S.)

  3. Spectroscopic, Thermal and Biological Studies on Some Trivalent Ruthenium and Rhodium NS Chelating Thiosemicarbazone Complexes

    Vinod K Sharma; Shipra Srivastava; Ankita Srivastava

    2007-01-01

    The synthetic, spectroscopic, and biological studies of sixteen ring-substituted 4-phenylthiosemicarbazones and 4-nitrophenyl-thiosemicarbazones of anisaldehyde, 4-chlorobenzaldehyde, 4-fluorobenzaldehyde, and vanillin with ruthenium(III) and rhodium(III) chlorides are reported here. Their structures were determined on the basis of the elemental analyses, spectroscopic data (IR, electronic, 1H and 13C NMR) along with magnetic susceptibility measurements, molar conductivity and thermogravimetr...

  4. Preparation of RNA samples with narrow line widths for solid state NMR investigations

    Huang, Wei; Bardaro, Michael F.; Varani, Gabriele; Drobny, Gary P.

    2012-10-01

    Solid state NMR can provide detailed structural and dynamic information on biological systems that cannot be studied under solution conditions, and can investigate motions which occur with rates that cannot be fully studied by solution NMR. This approach has successfully been used to study proteins, but the application of multidimensional solid state NMR to RNA has been limited because reported line widths have been too broad to execute most multidimensional experiments successfully. A reliable method to generate spectra with narrow line widths is necessary to apply the full range of solid state NMR spectroscopic approaches to RNA. Using the HIV-1 transactivation response (TAR) RNA as a model, we present an approach based on precipitation with polyethylene glycol that improves the line width of 13C signals in TAR from >6 ppm to about 1 ppm, making solid state 2D NMR studies of selectively enriched RNAs feasible at ambient temperature.

  5. NMR crystallography of polylactide

    Czernek, Jiří

    Prague : Institute of Macromolecular Chemistry AS CR, v. v. i, 2013. s. 60. ISBN 978-80-85009-77-4. [European Symposium on Polymer Spectroscopy /19./ - ESOPS19. Prague Meeting on Macromolecules /77./. 07.07.2013-11.07.2013, Prague] Institutional support: RVO:61389013 Keywords : NMR crystallography * polylactide Subject RIV: CD - Macromolecular Chemistry

  6. In situ NMR observation of the lithium extraction/insertion from LiCoO2 cathode

    Abstract: Rechargeable lithium-ion batteries (LIBs) are currently accepted to be one of the most suitable energy storage resources in portable electronic devices because of their high gravimetric and volumetric energy density. To understand the behavior of Li+ ions on electrochemical lithium extraction/insertion process, we performed in situ7Li nuclear magnetic resonance (NMR) measurements for LiCoO2 cathode in a plastic cell battery, and the spectral evolutions of the 7Li NMR signal of LixCoO2 (0 ≤ x ≤ 1) were well investigated. Very narrow solid solution region of LixCoO2 (∼0.99 ≤ x 2 signal at ∼0 ppm, which is related to the localized nature of the electronic spin of paramagnetic Co4+ ion formed at the very early delithiation stage. With further decreasing the signal intensity of LiCoO2, a Knight-shifted signal corresponding to an electrically conductive LixCoO2 phase emerged at x = 0.97, which then monotonously decreased in intensity for x xCoO2. These observations acquired in situ fully confirm the earlier studies obtained in ex situ measurements, although the present study offers more quantitative information. Moreover, it was shown that the peak position of the NMR shift for LixCoO2 moved as a function of lithium content, which behavior is analogous to the change in its c lattice parameter. Also, the growth and consumption of dendritic/mossy metallic lithium on the counter electrode was clearly observed during the charge/discharge cycles

  7. Soils, Pores, and NMR

    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

  8. Nuclear reaction of 10 B (n, α) 7 Li and grain size effects on the production of free radicals in alanine

    In general, it is important to know the physical and chemical properties of any material that is exposed to ionizing radiation. In particular, in dosimetric work, the amount of the absorbed doses by these materials is of much interest, in such a way that several methods have been developed in the past. An important and quantitatively accessible radiation effect in organic substances is the production of free radicals that can be easily measured by 'ELECTRON PARAMAGNETIC RESONANCE SPECTROSCOPY (EPR)'. Numerous studies have been now been made on pure D L-Alanine irradiated with different radiation sources. Examination of the irradiated samples reveals the production of a stable free radical (CH3 - CH. -COOH). In particular, gamma and electron irradiated D L-Alanine has received wide attention in the high doses interval (10 - 105 Gy). In contrast, there are very few EPR studies on thermal neutron radiation induced free radicals in pure D L-alanine. This may be due to the weak EPR signals observed in the irradiated samples. The objective of this work is to study for the first time the increase of the radical yield produced in neutron irradiated borated alanine by the EPR technique. For this purpose alanine has been mixed with borax in different stoichiometric proportions and grain sizes. When the mixture is neutron irradiated, the boron of the borax may experience a neutron capture reaction, 10 B (n, α) 7 Li. With this nuclear reaction it is supposed that the α particles will may impinge on the alanine molecules, producing in this way extra free radicals. Samples were irradiated in the thermal column of a Triga Mark III nuclear reactor with a thermal neutron flux of 5 x 10 7 n/Cm2 -s. A signal enhancement of up to 1260 % is observed when samples of alanine-borax were intimately mixed in a stoichiometric ratio of 1:1. We also studied dosimetric characteristics of the mixed samples such as: a) Sensibility. b) Accuracy. c) Traceability. d) Stability. e)Fading. f

  9. Spectroscopic Dosimeter Project

    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...

  10. Electrical conductivity, differential scanning calorimetry, X-ray diffraction, and {sup 7}Li nuclear magnetic resonance studies of n-C{sub x}H{sub (2x+1)}OSO{sub 3}Li (x = 12, 14, 16, 18, and 20)

    Hirakawa, Satoru [Yokohama City University, Graduate School of Nanobioscience (Japan); Morimoto, Yoshiaki [Yokohama City University, International College of Arts and Sciences (Japan); Honda, Hisashi, E-mail: hhonda@yokohama-cu.ac.jp [Yokohama City University, Graduate School of Nanobioscience (Japan)

    2015-04-15

    Electrical conductivity (σ), differential scanning calorimetry (DSC), and X-ray diffraction (XRD) measurements of n-C {sub x}H{sub (2x+1)}OSO{sub 3}Li (x= 12, 14, 16, 18, and 20) crystals were performed as a function of temperature. In addition, σ, DSC, and XRD observations of n-C {sub x}H{sub (2x+1)}OSO{sub 3}Na and n-C {sub x}H{sub (2x+1)}OSO{sub 3}K (x= 12, 14, 16, 18, and 20) crystals were carried out for comparison. DSC results of the salts revealed several solid-solid phase transitions with large entropy changes (ΔS). For n-C {sub 18}H{sub 37}OSO{sub 3}Li and n-C {sub 20}H{sub 41}OSO{sub 3}Li salts, each melting point produced a small ΔS{sub mp} value compared with the total entropy change in the solid phases (ΔS{sub tr1}+ΔS{sub tr2}). Additionally, Li {sup +} ion diffusion was detected in the highest temperature solid phases. For K salts, larger σ values were detected for potassium alkylsulfates compared with those reported for alkyl carboxylate. {sup 7}Li NMR spectra of n-C {sub 18}H{sub 37}OSO{sub 3}Li crystals recorded in the low-temperature phase showed large asymmetry parameters, suggesting the Li {sup +} ions are localized at asymmetric sites in the crystals.

  11. Application of Solution NMR Spectroscopy to Study Protein Dynamics

    Christoph Göbl

    2012-03-01

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

  12. Structure Determination of Unknown Organic Liquids Using NMR and IR Spectroscopy: A General Chemistry Laboratory

    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…

  13. Study of the spectroscopic characteristics of methyl (ligand) cobaloximes and their antibacterial activity

    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.

  14. NMR Methods for the Study of Instrinsically Disordered Proteins Structure, Dynamics, and Interactions: General Overview and Practical Guidelines.

    Brutscher, Bernhard; Felli, Isabella C; Gil-Caballero, Sergio; Hošek, Tomáš; Kümmerle, Rainer; Piai, Alessandro; Pierattelli, Roberta; Sólyom, Zsófia

    2015-01-01

    Thanks to recent improvements in NMR instrumentation, pulse sequence design, and sample preparation, a panoply of new NMR tools has become available for atomic resolution characterization of intrinsically disordered proteins (IDPs) that are optimized for the particular chemical and spectroscopic properties of these molecules. A wide range of NMR observables can now be measured on increasingly complex IDPs that report on their structural and dynamic properties in isolation, as part of a larger complex, or even inside an entire living cell. Herein we present basic NMR concepts, as well as optimised tools available for the study of IDPs in solution. In particular, the following sections are discussed hereafter: a short introduction to NMR spectroscopy and instrumentation (Sect. 3.1), the effect of order and disorder on NMR observables (Sect. 3.2), particular challenges and bottlenecks for NMR studies of IDPs (Sect. 3.3), 2D HN and CON NMR experiments: the fingerprint of an IDP (Sect. 3.4), tools for overcoming major bottlenecks of IDP NMR studies (Sect. 3.5), 13C detected experiments (Sect. 3.6), from 2D to 3D: from simple snapshots to site-resolved characterization of IDPs (Sect. 3.7), sequential NMR assignment: 3D experiments (Sect. 3.8), high-dimensional NMR experiments (nD, with n>3) (Sect. 3.9) and conclusions and perspectives (Sect. 3.10). PMID:26387100

  15. The NMR study of Li ion motion in K3LiNb6O17 and K3LiTa6O17

    The temperature dependences of the NMR relaxation times of 7Li in K3LiNb6 O17(KLN-2) and K3LiTa6O17(KLT-2) are reported. The logarithms of the relaxation times give straight lines against the inverse temperature, and the activation energies are estimated to be 0.29 eV and 0.33 eV from the lingitudinal relaxation times for KLN-2 and KLT-2, respectively. The motion of Li ions observed by NMR is discussed in connection with the ionic comduction in these materials and it is shown that the relaxation process is due to short-range ionic motion. (author)

  16. Spectroscopic study of 44Ti by reactions 40Ca(α,γ)44Ti, 40Ca(7Li,p2nγ)44Ti and 42Ca(α,2nγ)44Ti

    The first reaction allowed to populate states of excitation energies between 9.2 and 9.8 MeV and to measure their γ-decays to low-lying states in 44Ti. Moreover this reaction helps in measuring the mean lifetime of 12 states by using the Doppler shift attenuation method. The second reaction was used to find the levels predicted by the shell model and among them the highest spin allowed Jsup(π)=12+. The third reaction helps in measuring the mean lifetime tau=3.0+-0.6 ns of the Jsup(π)=(12+) state at Esub(x)=8.040 MeV. In this measurement the delayed coincidence technique with a pulsed beam was used. A confrontation of the experimental and theoretical studies on the 44Ti nucleus is presented in this work

  17. NMR of unfolded proteins

    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.

  18. NMR, water and plants

    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 other body fluids in human and animals. The method is based on a pulse sequence of equidistant π pulses in combination with a linear magnetic field gradient. (Auth.)

  19. Spectroscopic Characterization of Metallofullerenes

    Bethune, D. S.; de Vries, M. S.; Macfarlane, R.; Wittman, G.; Grannan, S.; Birmingham, J.; Richards, P.; Stevenson, S.; Glass, T.; Burbank, P.; Sun, Z.; Dorn, H. C.

    1996-03-01

    Scandium and Erbium metallofullerenes have been isolated using HPLC techniques and characterized by NMR, optical and far IR spectroscopy. In particular, Sc NMR spectra of Sc_2@C_2n species for several n have been obtained, and far infrared spectra of both discandium and and dierbium metallofullerenes have been measured. These show structure in the 20-200 cm-2 where vibrations of the encapsulated metal atoms are expected. Fluorescence spectra from dierbium metallofullerenes in the 1.5 μm region have been obtained at He and room temperatures.

  20. Cluster model of A = 7 nuclei revisited, and the astrophysical S factors for 3He(α,γ)7Be and 3H(α,γ)7Li at zero energy

    A local potential cluster model treatment of the A = 7 nuclei is updated in the light of a recent re-analysis of old experimental data and some new experimental measurements. The model is then used to calculate directly (without any energy extrapolation) the astrophysical S factors for 3He(α, γ)7Be and 3H(α, γ)7Li at zero energy. We find S0 = 0.51 ± 0.03 keV b for the former reaction and S0 = 0.09 ± 0.03 keV b for the latter, in good agreement with direct cross section measurements. (author)

  1. On the production of Be7 in the NRX reactor by the B10 (p, α) Be7, Li7 (p, n) Be7 and Li6 (d, n) Be7 reactions

    Three different reactions have been observed to yield Be7 in the NRX reactor. They are: Li7 (p, n) Be7, B10 (p, α) Be7, Li6 (d, n) Be7. The (p, α) reaction was initiated by recoil protons from neutron irradiation of boric acid. The (p, n) and (d, n) reactions were induced either by the recoil protons and deuterons from neutron irradiation of LiOH and LiOD targets or by protons and deuterons produced by (n, p) and (n, d) reactions on lithium or other elements chemically combined with lithium. (author)

  2. Analysis of adulterated herbal medicines and dietary supplements marketed for weight loss by DOSY 1H NMR

    VAYSSE, Julie; BALAYSSAC, Stéphane; GILARD, Véronique; DESOUBZDANNE, Denis; MALET-MARTINO, Myriam; Martino, Robert

    2010-01-01

    Abstract Twenty herbal medicines or dietary supplements marketed as natural slimming products were analyzed by Diffusion Ordered SpectroscopY (DOSY) 1H NMR and DOSY-COSY 1H NMR. The method allows analysis of the whole sample with detection of both active and inactive ingredients in these complex matrices. Among the 20 formulations analyzed, 2 were strictly herbal and 4 had a composition corresponding to declared ingredients on the packaging or the leaflet. The others were all adult...

  3. Reproducibility of NMR Analysis of Urine Samples: Impact of Sample Preparation, Storage Conditions, and Animal Health Status

    Christina Schreier; Werner Kremer; Fritz Huber; Sindy Neumann; Philipp Pagel; Kai Lienemann; Sabine Pestel

    2013-01-01

    Introduction. Spectroscopic analysis of urine samples from laboratory animals can be used to predict the efficacy and side effects of drugs. This employs methods combining 1H NMR spectroscopy with quantification of biomarkers or with multivariate data analysis. The most critical steps in data evaluation are analytical reproducibility of NMR data (collection, storage, and processing) and the health status of the animals, which may influence urine pH and osmolarity. Methods. We treated rats wit...

  4. Metabolic profiling of Rhodiola rosea rhizomes by 1H NMR spectroscopy

    Ioset, Karine Ndjoko; Nyberg, Nils T; Van Diermen, Daphne;

    2011-01-01

    Introduction - Rhodiola rosea is a broadly used medicinal plant with largely unexplored natural variability in secondary metabolite levels.Objective - The aim of this work was to develop a non-target procedure for (1)H NMR spectroscopic fingerprinting of rhizome extracts for pattern recognition...... demonstrated the usefulness of the established procedure for multivariate non-target (1)H NMR metabolic profiling of Rhodiola rosea. Copyright © 2010 John Wiley & Sons, Ltd....

  5. NMR molecular photography

    Khitrin, Anatoly K.; Ermakov, Vladimir L.; Fung, B M

    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 si...

  6. Structural properties of carbon nanotubes derived from 13C NMR

    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.

  7. NMR study of magnetic excitation in LiVX2 (X = O, S)

    Magnetic excitation in the two-dimensional triangular lattice LiVO2 and its itinerant analogue LiVS2 are investigated by 51V- and 7Li-NMR experiments. The nuclear spin-lattice relaxation rate 1/T1 on 51V and 7Li nuclei shows thermally activated behavior with different size of spin gap, Δ/kB ∼ 3400 K for LiVO2 and ∼ 1900 K for LiVS2, below the transition temperature Tc from magnetic to non-magnetic ground state. In 51(1/T1(T))/51(1/T1(Tc)) vs. T/Tc plot, the normalized relaxation rate for both materials seems to fall on the same curve. This scaling behavior indicates that the ground states of LiVO2 and LiVS2 are the same, i.e., V3+ (3d2 S = 1) spins form spin singlet with the formation of triangular vanadium clusters, although the replacement of oxygen by sulfur may broaden the band width and largely suppresses Tc from ∼ 500 K in LiVO2 to ∼ 310 K in LiVS2. However, the magnetic properties in the high temperature phase are different between LiVO2 and LiVS2. The value of 7(1/T1T) in LiVS2 becomes smaller with decreasing temperature, which suggests the development of pseudogap above Tc, in qualitatively consistent with the results from the magnetic susceptibility and the small change in entropy at Tc. This is a contrast to the case in LiVO2 where 51(1/T1T) is proportional to 1/T and it is explained by a localized spin model well above Tc.

  8. Structure and Ionic Conductivity of Halocomplexes of Main Group Metallic Elements Studied by NMR and NQR

    Li3InBr6 undergoes phase transition to a lithium superionic conductor at Ttr = 314 K (σ = 5.0 x 10-4 S cm-1 at 330 K). The Rietveld analysis and the DSC measurement suggested that the positional disorder is introduced at the cationic sites above Ttr. The X-ray powder diffraction pattern at the superionic phase changes gradually with temperature and finally shows a simple powder pattern at 420 K which is quite similar to that of LiBr. This rock salt structure contains intrinsic vacancies because one In3+ and two vacancies substitute for three Li+. 7Li and 115In NMR support the rapid diffusion of the Li+ and the introduction of the In3+ into the rock salt structure. On the other hand, the ionic conductivity for Na3InCl6 was 10-5 S cm-1 even at 500 K. Conduction path for the sodium ions could be proposed by means of the Rietveld analysis and the NMR experiment using a single crystal.

  9. Three dimensional nuclear magnetic resonance spectroscopic imaging of sodium ions using stochastic excitation and oscillating gradients

    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.

  10. Three dimensional nuclear magnetic resonance spectroscopic imaging of sodium ions using stochastic excitation and oscillating gradients

    Nuclear magnetic resonance (NMR) spectroscopic imaging of 23Na holds promise as a non-invasive method of mapping Na+ distributions, and for differentiating pools of Na+ ions in biological tissues. However, due to NMR relaxation properties of 23Na in vivo, a large fraction of Na+ 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 T2. Contemporary NMR imaging techniques have dead times of up to several hundred microseconds between excitation and sampling, comparable to the shortest in vivo 23Na T2 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 1H and 23Na spectroscopic imaging experiments have been performed on a small animal system with dead times as low as 25μs, 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

  11. Shell model and spectroscopic factors

    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)

  12. Efficient cellular solid-state NMR of membrane proteins by targeted protein labeling

    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

  13. Applications of high resolution NMR to geochemistry: crystalline, glass, and molten silicates

    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 29Si NMR spectroscopy. The local structure of glass aluminosilicates as observed by NMR, is presented with analysis of the information content of 29Si spectra. A high-temperature (to 13000C) 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 (T1 and T2) measurements as a function of composition and temperature for 23Na and 29Si

  14. Efficient cellular solid-state NMR of membrane proteins by targeted protein labeling

    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.

  15. Automatic Tuning Matching Cycler (ATMC) in situ NMR spectroscopy as a novel approach for real-time investigations of Li- and Na-ion batteries

    Pecher, Oliver; Bayley, Paul M.; Liu, Hao; Liu, Zigeng; Trease, Nicole M.; Grey, Clare P.

    2016-04-01

    We have developed and explored the use of a new Automatic Tuning Matching Cycler (ATMC) in situ NMR probe system to track the formation of intermediate phases and investigate electrolyte decomposition during electrochemical cycling of Li- and Na-ion batteries (LIBs and NIBs). The new approach addresses many of the issues arising during in situ NMR, e.g., significantly different shifts of the multi-component samples, changing sample conditions (such as the magnetic susceptibility and conductivity) during cycling, signal broadening due to paramagnetism as well as interferences between the NMR and external cycler circuit that might impair the experiments. We provide practical insight into how to conduct ATMC in situ NMR experiments and discuss applications of the methodology to LiFePO4 (LFP) and Na3V2(PO4)2F3 cathodes as well as Na metal anodes. Automatic frequency sweep 7Li in situ NMR reveals significant changes of the strongly paramagnetic broadened LFP line shape in agreement with the structural changes due to delithiation. Additionally, 31P in situ NMR shows a full separation of the electrolyte and cathode NMR signals and is a key feature for a deeper understanding of the processes occurring during charge/discharge on the local atomic scale of NMR. 31P in situ NMR with "on-the-fly" re-calibrated, varying carrier frequencies on Na3V2(PO4)2F3 as a cathode in a NIB enabled the detection of different P signals within a huge frequency range of 4000 ppm. The experiments show a significant shift and changes in the number as well as intensities of 31P signals during desodiation/sodiation of the cathode. The in situ experiments reveal changes of local P environments that in part have not been seen in ex situ NMR investigations. Furthermore, we applied ATMC 23Na in situ NMR on symmetrical Na-Na cells during galvanostatic plating. An automatic adjustment of the NMR carrier frequency during the in situ experiment ensured on-resonance conditions for the Na metal and

  16. 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

    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)

  17. X-Nuclei NMR Self-Diffusion Studies in Mesoporous Silica Foam and Microporous MOF CuBTC

    Frank Stallmach

    2012-04-01

    Full Text Available A standard X-observe NMR probe was equipped with a z-gradient coil to enable high-sensitivity pulsed field gradient NMR diffusion studies of Li+ and Cs+ cations of aqueous salt solutions in a high-porosity mesocellular silica foam (MCF and of CO2 adsorbed in metal-organic frameworks (MOF. The coil design and the necessary probe modifications, which yield pulsed field gradients of up to ±16.2Tm−1, are introduced. The system was calibrated at 2H resonance frequency and successfully applied for diffusion studies at 7Li, 23Na, 13C and 133Cs frequencies. Significant reductions of the diffusivities of the cations in LiClac and CsClac solution introduced into MCFs are observed. By comparison of the diffusion behavior with the bulk solutions, a tortuosity of the silica foam of 4.5 ± 0.6 was derived. Single component self-diffusion of CO2 and CH4 (measured by 1H NMR as well as self-diffusion of the individual components in CO2/CH4 mixtures was studied in the MOF CuBTC. The experimental results confirm high mobilities of the adsorbed gases and trends for diffusion separation factors predicted by MD simulations.

  18. NMR spectrometers as "magnetic tongues"

    Malmendal, Anders; Amoresano, Claudia; Trotta, Roberta;

    2011-01-01

    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...

  19. NMR in pulsed magnetic field

    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.

  20. Structural Biology: Practical NMR Applications

    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.

  1. Fundamentals of Protein NMR Spectroscopy

    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...

  2. Constants of NMR spectra

    The NMR (nuclear magnetic resonance) spectroscopy is a method for studying matter. It has been developed in a lot of fields of physics, physical chemistry, chemistry and biology. It concerns both the solid state and the liquid state. The study in solution of synthesis organic molecules or of organic molecules of natural origin and of biological molecules is particularly stressed on but it is also possible to study inorganic molecules. The originality of this method is to give both data on each atoms of the studied structure, on the atoms sequence in this structure, on the conformation and on the related configurations. It allows to reveal the interactions between separate molecules too. It is also a precious tool for the analysis of molecular movements. The development of this method for the study of condensed phases is particularly studied nowadays and the data obtained are for a lot of fields as acute as those obtained at the liquid state. (O.M.)

  3. Uses of 1H NMR and 13C NMR spectroscopy in studies of phenylenedioxydiacetamides complexation with the cations of calcium and potassium in solution

    The complexation abilities and the coordination sites of 12 derivatives using infrared, 1HNMR and 13C NMR spectroscopy are analyzed. The spectroscopic results indicate that only the 1,2-phenylenedioxydiacetamides are suitable ligands; the 1,3 derivatives did not react. These ionophors 1-8 represent fourdentale chelating ligands where all four oxygen atmos are involved in bonds to the metal. Independent from its charge one cations is coordinate by two ionophors. (M.J.C.)

  4. Recent Advances in Solution NMR: Fast Methods and Heteronuclear Direct Detection

    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)

  5. Online T5 learning model to enhance chemistry students’ understanding of NMR spectroscopy

    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.

  6. High-resolution magic-angle-spinning NMR spectroscopy for metabolic profiling of intact tissues.

    Beckonert, Olaf; Coen, Muireann; Keun, Hector C; Wang, Yulan; Ebbels, Timothy M D; Holmes, Elaine; Lindon, John C; Nicholson, Jeremy K

    2010-06-01

    Metabolic profiling, metabolomic and metabonomic studies require robust study protocols for any large-scale comparisons and evaluations. Detailed methods for solution-state NMR spectroscopy have been summarized in an earlier protocol. This protocol details the analysis of intact tissue samples by means of high-resolution magic-angle-spinning (HR-MAS) NMR spectroscopy and we provide a detailed description of sample collection, preparation and analysis. Described here are (1)H NMR spectroscopic techniques such as the standard one-dimensional, relaxation-edited, diffusion-edited and two-dimensional J-resolved pulse experiments, as well as one-dimensional (31)P NMR spectroscopy. These are used to monitor different groups of metabolites, e.g., sugars, amino acids and osmolytes as well as larger molecules such as lipids, non-invasively. Through the use of NMR-based diffusion coefficient and relaxation times measurements, information on molecular compartmentation and mobility can be gleaned. The NMR methods are often combined with statistical analysis for further metabonomics analysis and biomarker identification. The standard acquisition time per sample is 8-10 min for a simple one-dimensional (1)H NMR spectrum, giving access to metabolite information while retaining tissue integrity and hence allowing direct comparison with histopathology and MRI/MRS findings or the evaluation together with biofluid metabolic-profiling data. PMID:20539278

  7. Spectroscopically Unlocking Exoplanet Characteristics

    Lewis, Nikole

    2016-05-01

    Spectroscopy plays a critical role in a number of areas of exoplanet research. The first exoplanets were detected by precisely measuring Doppler shifts in high resolution (R ~ 100,000) stellar spectra, a technique that has become known as the Radial Velocity (RV) method. The RV method provides critical constraints on exoplanet masses, but is currently limited to some degree by robust line shape predictions. Beyond the RV method, spectroscopy plays a critical role in the characterization of exoplanets beyond their mass and radius. The Hubble Space Telescope has spectroscopically observed the atmospheres of exoplanets that transit their host stars as seen from Earth giving us key insights into atmospheric abundances of key atomic and molecular species as well as cloud optical properties. Similar spectroscopic characterization of exoplanet atmospheres will be carried out at higher resolution (R ~ 100-3000) and with broader wavelength coverage with the James Webb Space Telescope. Future missions such as WFIRST that seek to the pave the way toward the detection and characterization of potentially habitable planets will have the capability of directly measuring the spectra of exoplanet atmospheres and potentially surfaces. Our ability to plan for and interpret spectra from exoplanets relies heavily on the fidelity of the spectroscopic databases available and would greatly benefit from further laboratory and theoretical work aimed at optical properties of atomic, molecular, and cloud/haze species in the pressure and temperature regimes relevant to exoplanet atmospheres.

  8. Microscopic Structure of Contact Ion Pairs in Concentrated LiCl- and LiClO4-Tetrahydrofuran Solutions Studied by Low-Frequency Isotropic Raman Scattering and Neutron Diffraction with (6)Li/(7)Li Isotopic Substitution Methods.

    Kameda, Yasuo; Ebina, Saki; Amo, Yuko; Usuki, Takeshi; Otomo, Toshiya

    2016-05-26

    Low-frequency isotropic Raman scattering and time-of-flight neutron diffraction measurements were carried out for (6)Li/(7)Li and H/D isotopically substituted *LiCl- and *LiClO4-tetrahydrofuran (*THF) solutions in order to obtain microscopic insight into solvated Li(+), Li(+)···Cl(-) and Li(+)···ClO4(-) contact ion pairs formed in concentrated THF solutions. Symmetrical stretching vibrational mode of solvated Li(+) in LiCl and LiClO4 solutions was observed at ν = 181-184 and 140 cm(-1), respectively. The stretching vibrational mode of Li(+)···Cl(-) and Li(+)···ClO4(-) solvated contact ion pairs formed in 4 mol % (6)LiCl-THF-h8 and (7)LiCl-THF-h8 solutions was found at ν = 469 and 435 cm(-1), respectively. Detailed structural properties of solvated Li(+) and the contact ion pairs were derived from the least-squares fitting analyses of the first-order difference function, ΔLi(Q), obtained from neutron diffraction measurements on (6)Li/(7)Li isotopically substituted THF-d8 solutions. It has been revealed that Li(+) takes 4-fold coordination in the average local structure of Li(+)X(-)(THF)3, X = Cl and ClO4. The nearest neighbor Li(+)···O(THF) distance was determined to be 2.21 ± 0.01 Å and 2.07 ± 0.01 Å for 4 mol % *LiCl- and 10 mol % *LiClO4-THF-d8 solutions, respectively. The Li(+)···anion distances for Li(+)···Cl(-) and Li(+)···O(ClO4(-)) contact ion pairs were determined to be 2.4 ± 0.1 Å and 2.19 ± 0.01 Å, respectively. The nearest neighbor Li(+)···THF interaction is significantly modified by the anion in the first solvation shell. PMID:27157529

  9. Two dimensional solid state NMR

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

  10. Observation of a stuffed unmodified network in beryllium silicate glasses with multinuclear NMR spectroscopy

    The structure of BeO-SiO2 glasses with up to 20 mol % BeO has been studied with 9Be and 29Si NMR spectroscopic techniques. The NMR results are consistent with a glass structure consisting of nanoclusters of corner-shared BeO4 tetrahedra that occupy the interstices of an unmodified and highly strained corner-shared SiO4 network. The complete absence of nonbridging oxygens in these glasses contradicts the conventional wisdom of oxide glass structures based on the modified random-network-type models. This structure type may have important implications in understanding and designing glasses with unusual properties

  11. Studies on the Interactions between Potassium oxalato oxodiperoxovanadate and Histidine by NMR and MS

    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.

  12. NMR for chemists and biologists

    Carbajo, Rodrigo J

    2013-01-01

    This book intends to be an easy and concise introduction to the field of nuclear magnetic resonance or NMR, which has revolutionized life sciences in the last twenty years. A significant part of the progress observed in scientific areas like Chemistry, Biology or Medicine can be ascribed to the development experienced by NMR in recent times. Many of the books currently available on NMR deal with the theoretical basis and some of its main applications, but they generally demand a strong background in Physics and Mathematics for a full understanding. This book is aimed to a wide scientific audie

  13. Annual reports on NMR spectroscopy

    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

  14. Cluster model of A=7 nuclei revisited, and the astrophysical S factors for 3 He(α, γ)7 Be and 3 H(α, γ)7 Li at zero energy

    A elementary cluster model that visualizes an alpha particle interacting with a 3 H of 3 He cluster via a local potential is employed. An assurance is made that the major requirements of the Pauli principle are satisfied by choosing relative motion quantum numbers N (Principal Quantum Number) and L to correspond to the microscopic situation in which the 3 H or 3 He nucleons occupy shell-model orbitals above the (O)- orbitals filled by the alpha particles. The So factor for the capture reactions 3 He (α,γ)7 Be and 3 H (α,γ)7 Li is calculated by considering only electric dipole capture from incident s-waves as follows. (author)

  15. The S(E) factor of 7Li(p,γ)8Be and consequences for S(E) extrapolation in 7Be(p,γ0)8B

    Excitation functions and forward-backward anisotropies have been measured for the 7Li(p, γ)8Be capture reaction over the proton energy range Ep = 100 to 1500 keV, using a 4π summing crystal and Ge(Li) detectors, respectively. The data show at all energies the presence of E1 and M1 capture amplitudes arising from the direct capture (DC) process and the ER = 441 and 1030 keV resonances, respectively. Due to the observed DC process, the present data increase significantly the reaction rates (up to a factor of 110) compared to values given in the compilation. The data and their analyses remove the recent criticism on DC model calculations, which had implied a significant reduction in the extrapolated S(E) factor for 7Be(p, γ)8B and thus in the predicted flux of high-energy solar neutrinos; thus, the solar neutrino problem is still with us. (orig.)

  16. 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.

    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. PMID:24387907

  17. Quasi-monoenergetic neutron energy spectra for 246 and 389 MeV {sup 7}Li(p,n) reactions at angles from 0{sup o} to 30{sup o}

    Iwamoto, Yosuke, E-mail: iwamoto.yosuke@jaea.go.j [Japan Atomic Energy Agency, 2-4 Shirakatashirane, Tokai, Naka, Ibaraki 319-1195 (Japan); Hagiwara, Masayuki [High Energy Accelerator Research Organization (KEK), 1-1 Oho, Tsukuba, Ibaraki 305-0801 (Japan); Satoh, Daiki [Japan Atomic Energy Agency, 2-4 Shirakatashirane, Tokai, Naka, Ibaraki 319-1195 (Japan); Iwase, Hiroshi [High Energy Accelerator Research Organization (KEK), 1-1 Oho, Tsukuba, Ibaraki 305-0801 (Japan); Yashima, Hiroshi [Research Reactor Institute, Kyoto University, 2-1010 Asashiro-nishi, Kumatori-cho, Sennnan-gun, Osaka 590-0494 (Japan); Itoga, Toshiro [RIKEN, 1-1-1 Kouto, Sayo-cho, Sayo-gun, Hyogo 679-5148 (Japan); Sato, Tatsuhiko; Nakane, Yoshihiro; Nakashima, Hiroshi; Sakamoto, Yukio [Japan Atomic Energy Agency, 2-4 Shirakatashirane, Tokai, Naka, Ibaraki 319-1195 (Japan); Matsumoto, Tetsuro; Masuda, Akihiko; Nishiyama, Jun [National Institute of Advanced Industrial Science and Technology, 1-1-1 Higashi, Tsukuba, Ibaraki 305-8561 (Japan); Tamii, Atsushi; Hatanaka, Kichiji [Research Center for Nuclear Physics (RCNP), 10-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan); Theis, C.; Feldbaumer, E.; Jaegerhofer, L. [CERN, CH-1211 Geneve 23 (Switzerland); Pioch, C.; Mares, V. [German Research Center for Environmental Health, Institute of Radiation Protection, Ingolstaedter Landstr. 1, 85764 Neuherberg (Germany)

    2011-02-11

    The authors measured the neutron energy spectra of a quasi-monoenergetic {sup 7}Li(p,n) neutron source with 246 and 389 MeV protons set at seven angles (0{sup o}, 2.5{sup o}, 5{sup o}, 10{sup o}, 15{sup o}, 20{sup o} and 30{sup o}), 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{sup o} and 10 MeV at other angles. The cross-sections of the peak neutron production reaction at 0{sup o} 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 DARWIN and Wendi-2, the authors showed the subtractions of H*(10) obtained at larger angles (10{sup o}, 15{sup o}, 20{sup o} and 30{sup o}) from the 0{sup o} data in the continuum part for the 246 and 389 MeV {sup 7}Li(p,n) reactions. It was found that subtracting the dose equivalent at about 20{sup o} from the 0{sup o} data almost eliminates the continuum component. This method has potential to eliminate problems associated with continuum correction for high-energy neutron monitors.

  18. Integrative NMR for biomolecular research.

    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 ). PMID:27023095

  19. Optical pumping and xenon NMR

    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.

  20. Optical pumping and xenon NMR

    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. Optical pumping and xenon NMR

    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

  2. Spectroscopic Studies of Amino Acid Ionic Liquid-Supported Schiff Bases

    Paula Ossowicz; Ewa Janus; Grzegorz Schroeder; Zbigniew Rozwadowski

    2013-01-01

    Amino acid ionic liquid-supported Schiff bases, derivatives of salicylaldehyde and various amino acids (L-threonine, L-valine, L-leucine, L-isoleucine and L-histidine) have been investigated by means of various spectroscopic techniques (NMR, UV-Vis, IR, MS) and deuterium isotope effects on 13C-NMR chemical shifts. The results have shown that in all studied amino acid ionic liquid-supported Schiff bases (except the L-histidine derivative) a proton transfer equilibrium exists and the presence o...

  3. NMR spectroscopy of proteins encapsulated in a positively charged surfactant.

    Lefebvre, Brian G; Liu, Weixia; Peterson, Ronald W; Valentine, Kathleen G; Wand, A Joshua

    2005-07-01

    Traditionally, large proteins, aggregation-prone proteins, and membrane proteins have been difficult to examine by modern multinuclear and multidimensional solution NMR spectroscopy. A major limitation presented by these protein systems is that their slow molecular reorientation compromises many aspects of the more powerful solution NMR methods. Several approaches have emerged to deal with the various spectroscopic difficulties arising from slow molecular reorientation. One of these takes the approach of actively seeking to increase the effective rate of molecular reorientation by encapsulating the protein of interest within the protective shell of a reverse micelle and dissolving the resulting particle in a low viscosity fluid. Since the encapsulation is largely driven by electrostatic interactions, the preparation of samples of acidic proteins suitable for NMR spectroscopy has been problematic owing to the paucity of suitable cationic surfactants. Here, it is shown that the cationic surfactant CTAB may be used to prepare samples of encapsulated anionic proteins dissolved in low viscosity solvents. In a more subtle application, it is further shown that this surfactant can be employed to encapsulate a highly basic protein, which is completely denatured upon encapsulation using an anionic surfactant. PMID:15949753

  4. Computational Analysis of Solvent Effects in NMR Spectroscopy.

    Dračínský, Martin; Bouř, Petr

    2010-01-12

    Solvent modeling became a standard part of first principles computations of molecular properties. However, a universal solvent approach is particularly difficult for the nuclear magnetic resonance (NMR) shielding and spin-spin coupling constants that in part result from collective delocalized properties of the solute and the environment. In this work, bulk and specific solvent effects are discussed on experimental and theoretical model systems comprising solvated alanine zwitterion and chloroform molecules. Density functional theory computations performed on larger clusters indicate that standard dielectric continuum solvent models may not be sufficiently accurate. In some cases, more reasonable NMR parameters were obtained by approximation of the solvent with partial atomic charges. Combined cluster/continuum models yielded the most reasonable values of the spectroscopic parameters, provided that they are dynamically averaged. The roles of solvent polarizability, solvent shell structure, and bulk permeability were investigated. NMR shielding values caused by the macroscopic solvent magnetizability exhibited the slowest convergence with respect to the cluster size. For practical computations, however, inclusion of the first solvation sphere provided satisfactory corrections of the vacuum values. The simulations of chloroform chemical shifts and CH J-coupling constants were found to be very sensitive to the molecular dynamics model used to generate the cluster geometries. The results show that computationally efficient solvent modeling is possible and can reveal fine details of molecular structure, solvation, and dynamics. PMID:26614339

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

    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. PMID:26728075

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

    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.

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

    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. 1H) and low-γ (e.g. 13C) 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

  8. NMR study of water solution actinide behaviour with a view to separate them by liquid-liquid extraction from fuel reprocessing solutions

    Actinides (V I) are very well studied, but complementary studies are necessary. Actinides (V): the complexing is less studied, so supplementary studies are very useful. The NMR is a spectroscopic method allowing to study the solution ions, with a quantitative and dynamic method, possessing besides one multi nucleus character, so the NMR will allow to obtain answers to these problems, in the topics of: speciation, structure, dynamics of the molecules in solution

  9. Characterization of reactive intermediates by multinuclear diffusion-ordered NMR spectroscopy (DOSY).

    Li, Deyu; Keresztes, Ivan; Hopson, Russell; Williard, Paul G

    2009-02-17

    Nuclear magnetic resonance (NMR) is the most powerful and widely utilized technique for determining molecular structure. Although traditional NMR data analysis involves the correlation of chemical shift, coupling constant, and NOE interactions to specific structural features, a largely overlooked method introduced more than 40 years ago, pulsed gradient spin-echo (PGSE), measures diffusion coefficients of molecules in solution, thus providing their relative particle sizes. In the early 1990s, the PGSE sequence was incorporated into a two-dimensional experiment, dubbed diffusion-ordered NMR spectroscopy (DOSY), in which one dimension represents chemical shift data while the second dimension resolves species by their diffusion properties. This combination provides a powerful tool for identifying individual species in a multicomponent solution, earning the nickname "chromatography by NMR". In this Account, we describe our efforts to utilize DOSY techniques to characterize organometallic reactive intermediates in solution in order to correlate structural data to solid-state crystal structures determined by X-ray diffraction and to discover the role of aggregate formation and solvation states in reaction mechanisms. In 2000, we reported our initial efforts to employ DOSY techniques in the characterization of reactive intermediates such as organolithium aggregates. Since then, we have explored DOSY experiments with various nuclei beyond (1)H, including (6)Li, (7)Li, (11)B, (13)C, and (29)Si. Additionally, we proposed a diffusion coefficient-formula weight relationship to determine formula weight, aggregation number, and solvation state of reactive intermediates. We also introduced an internal reference system to correlate the diffusion properties of unknown reactive intermediates with known inert molecular standards, such as aromatic compounds, terminal olefins, cycloolefins, and tetraalkylsilanes. Furthermore, we utilized DOSY to interpret the role of aggregation number

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

    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

  11. NMR Dynamic Studies in Living Systems

    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.

  12. Quantitative analysis of sugars in wood hydrolyzates with 1H NMR during the autohydrolysis of hardwoods.

    Mittal, Ashutosh; Scott, Gary M; Amidon, Thomas E; Kiemle, David J; Stipanovic, Arthur J

    2009-12-01

    The focus of this work was to determine the utility of (1)H NMR spectroscopy in the quantification of sugars resulting from the solubilization of hemicelluloses during the autohydrolysis of hardwoods and the use of this technique to evaluate the kinetics of this process over a range of temperatures and times. Yields of residual xylan, xylooligomers, xylose, glucose, and the degraded products of sugars, i.e., furfural and HMF (5-hydroxymethyl furfural), were determined. The monosaccharide and oligomer contents were quantified with a recently developed high resolution (1)H NMR spectroscopic analysis. This method provided precise measurement of the residual xylan and cellulose remaining in the extracted wood samples and xylose and glucose in the hydrolyzates. NMR was found to exhibit good repeatability and provided carbohydrate compositional results comparable to published methods for sugar maple and aspen woods. PMID:19674893

  13. NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

    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.

  14. Metabolic profiling, metabolomic and metabonomic procedures for NMR spectroscopy of urine, plasma, serum and tissue extracts.

    Beckonert, Olaf; Keun, Hector C; Ebbels, Timothy M D; Bundy, Jacob; Holmes, Elaine; Lindon, John C; Nicholson, Jeremy K

    2007-01-01

    Metabolic profiling, metabolomic and metabonomic studies mainly involve the multicomponent analysis of biological fluids, tissue and cell extracts using NMR spectroscopy and/or mass spectrometry (MS). We summarize the main NMR spectroscopic applications in modern metabolic research, and provide detailed protocols for biofluid (urine, serum/plasma) and tissue sample collection and preparation, including the extraction of polar and lipophilic metabolites from tissues. 1H NMR spectroscopic techniques such as standard 1D spectroscopy, relaxation-edited, diffusion-edited and 2D J-resolved pulse sequences are widely used at the analysis stage to monitor different groups of metabolites and are described here. They are often followed by more detailed statistical analysis or additional 2D NMR analysis for biomarker discovery. The standard acquisition time per sample is 4-5 min for a simple 1D spectrum, and both preparation and analysis can be automated to allow application to high-throughput screening for clinical diagnostic and toxicological studies, as well as molecular phenotyping and functional genomics. PMID:18007604

  15. NMR imaging and spectroscopy of the mammalian central nervous system after heavy ion radiation

    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

  16. Diffusion NMR spectroscopy for the characterization of the size and interactions of colloidal matter: the case of vesicles and nanoparticles.

    Valentini, Massimiliano; Vaccaro, Andrea; Rehor, Annemie; Napoli, Alessandro; Hubbell, Jeffrey A; Tirelli, Nicola

    2004-02-25

    We report the application of the pulse gradient spin-echo (PGSE) NMR technique (PGSE NMR) to the analysis of large colloidal materials, specifically vesicles formed from macromolecular amphiphiles and nanoparticles. Measurements of size and size distribution were demonstrated to be comparable to those obtained through dynamic light scattering or hydrodynamic chromatography. In comparison to these more common analytical methods, the use of PGSE NMR is particularly advantageous in that, as a spectroscopic technique, it adds chemical selectivity to the study of physical dimensions. In this way, chemically different species contemporarily present in a sample may be individually studied. In addition, we demonstrate the use of PGSE NMR to probe the existence of equilibria between macroamphiphiles present in solution and those present in vesicles or on the surface of nanoparticles. This feature in particular opens exciting possibilities for the characterization of the phase behavior and of the surface adsorption phenomena of colloids. PMID:14971949

  17. TU-F-BRE-07: In Vivo Neutron Detection in Patients Undergoing Stereotactic Ablative Radiotherapy (SABR) for Primary Kidney Cancer Using 6Li and 7Li Enriched TLD Pairs

    Lonski, P; Kron, T [Physical Sciences, Peter MacCallum Cancer Centre, East Melbourne, Victoria (Australia); RMIT University, Melbourne, Victoria (Australia); Franich, R; Keehan, S [RMIT University, Melbourne, Victoria (Australia); Siva, S [Radiation Oncology and Cancer Imaging, Peter MacCallum Cancer Centre, Melbourne, Victoria (Australia); Taylor, M [Australian Federal Police, Canberra, ACT (Australia)

    2014-06-15

    Purpose: Stereotactic ablative radiotherapy (SABR) for primary kidney cancer often involves the use of high-energy photons combined with a large number of monitor units. While important for risk assessment, the additional neutron dose to untargeted healthy tissue is not accounted for in treatment planning. This work aims to detect out-of-field neutrons in vivo for patients undergoing SABR with high-energy (>10 MV) photons and provides preliminary estimates of neutron effective dose. Methods: 3 variations of high-sensitivity LiF:Mg,Cu,P thermoluminescent dosimeter (TLD) material, each with varying {sup 6}Li / {sup 7}Li concentrations, were used in custom-made Perspex holders for in vivo measurements. The variation in cross section for thermal neutrons between Li isotopes was exploited to distinguish neutron from photon signal. Measurements were made out-of-field for 7 patients, each undergoing 3D-conformal SABR treatment for primary kidney cancer on a Varian 21iX linear accelerator. Results: In vivo measurements show increased signal for the {sup 6}Li enriched material for patients treated with 18 MV photons. Measurements on one SABR patient treated using only 6 MV showed no difference between the 3 TLD materials. The out-of-field photon signal decreased exponentially with distance from the treatment field. The neutron signal, taken as the difference between {sup 6}Li enriched and {sup 7}Li enriched TLD response, remains almost constant up to 50 cm from the beam central axis. Estimates of neutron effective dose from preliminary TLD calibration suggest between 10 and 30 mSv per 1000 MU delivered at 18 MV for the 7 patients. Conclusion: TLD was proven to be a useful tool for the purpose of in vivo neutron detection at out-of-field locations. Further work is required to understand the relationship between TL signal and neutron dose. Dose estimates based on preliminary TLD calibration in a neutron beam suggest the additional neutron dose was <30 mSv per 1000 MU at 18 MV.

  18. NMR and dynamics of biopolymers

    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

  19. Two-dimensional NMR spectrometry

    This article is the second in a two-part series. In part one (ANALYTICAL CHEMISTRY, May 15) the authors discussed one-dimensional nuclear magnetic resonance (NMR) spectra and some relatively advanced nuclear spin gymnastics experiments that provide a capability for selective sensitivity enhancements. In this article and overview and some applications of two-dimensional NMR experiments are presented. These powerful experiments are important complements to the one-dimensional experiments. As in the more sophisticated one-dimensional experiments, the two-dimensional experiments involve three distinct time periods: a preparation period, t0; an evolution period, t1; and a detection period, t2

  20. Solid state NMR investigation of a novel Li ion ceramic electrolyte. Li doped BPO sub 4

    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...

  1. Advanced NMR characterization of zeolite catalysts

    Welsh, L. B.

    1985-04-01

    The program discussed in this report is a two-year two-phase joint UOP-University of Illinois study of the application of improved high resolution solid state nuclear magnetic resonance (NMR) techniques to the characterization of zeolite catalysts. During the first phase of this program very pure, and in some cases isotopically enriched faujasites will be prepared and studied by magic angle sample spinning NMR (MASS NMR) and variable engine sample spinning NMR (VASS NMR) on 500 and 360 MHz (proton frequency) NMR spectrometers. The NMR techniques that will be emphasized are the measurement and analysis of the (17)O NMR properties, (27)Al NMR intensity quantitation, and (27)Al and (29)Si NMR relaxation rates. During the second phase of this program these NMR techniques will be used to study the effects of impurity concentration, dealumination treatments and cation exchange on the NMR properties of faujasites. The initial emphasis of this program during Phase I is on the preparation and measurement of the NMR properties of (17)O enriched Na-Y faujasties.

  2. Radiofrequency and magnet technology in medical NMR

    Nuclear magnetic resonance (NMR) is briefly described, particularly its rf and magnet aspects. Particular attention is given to the duplexer, the rf coils, and new kinds of magnets for remote sensing NMR

  3. Spectroscopic Investigations of the Fouling Process on Nafion Membranes in Vanadium Redox Flow Batteries

    Vijayakumar, M.; Sivakumar, Bhuvaneswari M.; Nachimuthu, Ponnusamy; Schwenzer, Birgit; Kim, Soowhan; Yang, Zhenguo; Liu, Jun; Graff, Gordon L.; Thevuthasan, Suntharampillai; Hu, Jian Z.

    2011-01-01

    The Nafion-117 membrane used in vanadium redox flow battery (VRFB) is analyzed by X-ray photoelectron spectroscopy (XPS) and nuclear magnetic resonance (NMR) spectroscopy. The XPS study reveals the chemical identity and environment of vanadium cations accumulated at the surface due to their low diffusivity. On the other hand, the 17O NMR spectrum explores the diffused vanadium cation from the bulk part of Nafion and shows the chemical bonding of cation and the host membrane. The 19F NMR shows the basic Nafion structure is not altered due to the presence of diffused vanadium cation. Based on these spectroscopic studies, the chemical environment of diffused vanadium cation in the Nafion membrane is discussed. This study also shed light into the possible cause for the high diffusivity of certain vanadium cations inside the Nafion membranes.

  4. High resolution NMR theory and chemical applications

    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,

  5. Cancer metastasis detected by NMR

    A narrow NMR line originating from the plasma membrane of a cancer cell is unexpected. The behaviour of these lines is explained in terms of fundamental physics and chemistry. There is biochemical evidence to support the presence of neutral lipid domains in the plasma membrane. T2 relaxation and clinical implications are briefly discussed

  6. Spectroscopic Detection of Pathogens

    ALAM,M. KATHLEEN; TIMLIN,JERILYN A.; MARTIN,LAURA E.; HJELLE,DRIAN; LYONS,RICK; GARRISON,KRISTIN

    2000-11-01

    The goal of this LDRD Research project was to provide a preliminary examination of the use of infrared spectroscopy as a tool to detect the changes in cell cultures upon activation by an infectious agent. Due to a late arrival of funding, only 5 months were available to transfer and setup equipment at UTTM,develop cell culture lines, test methods of in-situ activation and collect kinetic data from activated cells. Using attenuated total reflectance (ATR) as a sampling method, live cell cultures were examined prior to and after activation. Spectroscopic data were collected from cells immediately after activation in situ and, in many cases for five successive hours. Additional data were collected from cells activated within a test tube (pre-activated), in both transmission mode as well as in ATR mode. Changes in the infrared data were apparent in the transmission data collected from the pre-activated cells as well in some of the pre-activated ATR data. Changes in the in-situ activated spectral data were only occasionally present due to (1) the limited time cells were studied and (2) incomplete activation. Comparison of preliminary data to infrared bands reported in the literature suggests the primary changes seen are due an increase in ribonucleic acid (RNA) production. This work will be continued as part of a 3 year DARPA grant.

  7. The use of enriched 6Li and 7Li LiF: Mg, Cu, P glass-rod thermoluminescent dosemeters for linear accelerator out-of-field radiation dose measurements

    6Li:Mg, Cu, P and 7Li: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 6Li:Mg, Cu, P TLDs at various distances from the iso-centre. With cadmium filters employed, slow neutrons (< 0.5 eV) were distinguished from fast neutrons. The average in-air photon dose equivalents per monitor unit (MU) ranged from 1.5±0.4 to 215.5±94.6 uμSv at 100 and 15 cm from the iso-centre, 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 uμSv at 100 and 15 cm from the iso-centre, respectively. Contribution of thermal neutrons to total neutron dose equivalent was small: 3.1±7.2 uμSv per MU at 15 cm from the iso-centre. (authors)

  8. The use of enriched 6Li and 7Li Lif:Mg,Cu,P glass-rod thermoluminescent dosemeters for linear accelerator out-of-field radiation dose measurements.

    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 (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. PMID:21873634

  9. 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

    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...

  10. Proton NMR studies of functionalized nanoparticles in aqueous environments

    Tataurova, Yulia Nikolaevna

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

  11. Spectroscopic and structural elucidation of alanyl-containing dipeptides and their hydrogensquarates

    Koleva, Bojidarka B.; Kolev, Tsonko M.; Spiteller, Michael

    2008-04-01

    The hydrogensquarates of alanyl-containing dipeptides glycylalanine ( H-Gly-Ala-OH) and alanylalanine ( H-Ala-Ala-OH) are characterized structurally by means of quantum chemical ab initio calculations, solid-state linear-dichroic infrared (IR-LD) spectroscopy, 1H and 13C NMR data, ESI-MS, HPLC-MS/MS, TGV and DSC methods. The structures consist in positive charged peptide moiety and negative hydrogensquarate anion (HSq -), stabilizing by strong intermolecular hydrogen bonds. The theoretical and IR-LD spectroscopic data are compared with corresponding ones of zwitterion dipeptides with a view to understanding the structural and conformational changes as well as the IR-spectroscopic ones as a result of hydrogensquarates formation. The strong overlapped and complicated IR-spectroscopic bands typical for hydrogensquarates in solid-state are assigned supporting with the presented vibrational analysis of the dipeptides and of the hydrogensqauarate anion.

  12. The ABC exporter MsbA probed by solid state NMR – challenges and opportunities.

    Kaur, Hundeep; Lakatos, Andrea; Spadaccini, Roberta; Vogel, Ramona; Hoffmann, Christian; Becker-Baldus, Johanna; Ouari, Olivier; Tordo, Paul; Mchaourab, Hassane; Glaubitz, Clemens

    2015-09-01

    ATP binding cassette (ABC) transporters form a superfamily of integral membrane proteins involved in translocation of substrates across the membrane driven by ATP hydrolysis. Despite available crystal structures and extensive biochemical data, many open questions regarding their transport mechanisms remain. Therefore, there is a need to explore spectroscopic techniques such as solid state NMR in order to bridge the gap between structural and mechanistic data. In this study, we investigate the feasibility of using Escherichia coli MsbA as a model ABC transporter for solid state NMR studies. We show that optimised solubilisation and reconstitution procedures enable preparing stable and homogenous protein samples. Depending on the duration of solubilisation, MsbA can be obtained in either an apo- or in a native lipid A bound form. Building onto these optimisations, the first promising MAS-NMR spectra with narrow lines have been recorded. However, further sensitivity improvements are required so that complex NMR experiments can be recorded within a reasonable amount of time. We therefore demonstrate the usability of paramagnetic doping for rapid data acquisition and explore dynamic nuclear polarisation as a method for general signal enhancement. Our results demonstrate that solid state NMR provides an opportunity to address important biological questions related to complex mechanisms of ABC transporters. PMID:25849794

  13. 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

    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…

  14. Magic-angle-spinning solid-state NMR of membrane proteins.

    Baker, Lindsay A; Folkers, Gert E; Sinnige, Tessa; Houben, Klaartje; Kaplan, Mohammed; van der Cruijsen, Elwin A W; Baldus, Marc

    2015-01-01

    Solid-state NMR spectroscopy (ssNMR) provides increasing possibilities to examine membrane proteins in different molecular settings, ranging from synthetic bilayers to whole cells. This flexibility often enables ssNMR experiments to be directly correlated with membrane protein function. In this contribution, we discuss experimental aspects of such studies starting with protein expression and labeling, leading to membrane protein isolation or to membrane proteins in a cellular environment. We show that optimized procedures can depend on aspects such as the achieved levels of expression, the stability of the protein during purification or proper refolding. Dealing with native membrane samples, such as isolated cellular membranes, can alleviate or entirely remove such biochemical challenges. Subsequently, we outline ssNMR experiments that involve the use of magic-angle-spinning and can be used to study membrane protein structure and their functional aspects. We pay specific attention to spectroscopic issues such as sensitivity and spectral resolution. The latter aspect can be controlled using a combination of tailored preparation procedures with solid-state NMR experiments that simplify the spectral analysis using specific filtering and correlation methods. Such approaches have already provided access to obtain structural views of membrane proteins and study their function in lipid bilayers. Ongoing developments in sample preparation and NMR methodology, in particular in using hyperpolarization or proton-detection schemes, offer additional opportunities to study membrane proteins close to their cellular function. These considerations suggest a further increase in the potential of using solid-state NMR in the context of prokaryotic or eukaryotic membrane protein systems in the near future. PMID:25950971

  15. NMR Studies of Inclusion Compounds

    Nikkhou Aski, Sahar

    2008-01-01

    This thesis presents the application of some of the NMR methods in studying host-guest complexes, mainly in solution. The general focus of the work is on investigating the reorientational dynamics of some small molecules that are bound inside cavities of larger moieties. In the current work, these moieties belong to two groups: cryptophanes and cyclodextrins. Depending on the structure of the cavities, properties of the guest molecules and the formed complexes vary. Chloroform and dichloromet...

  16. Measurement of deformations by NMR

    Bytchenkoff, Dimitri; Rodts, Stéphane

    2015-12-01

    Two NMR data acquisition protocols together with corresponding data processing algorithms for locating macroscopic objects, measuring distances between them or monitoring their displacements or deformations with microscopic precision are presented and discussed. The performance of the methods is demonstrated by applying them to the measurement of deformations of a freely supported beam under loading. We believe that our methods will find their applications in mechanics, civil engineering and medicine.

  17. RECENT PROGRESS IN BIOMOLECULAR NMR

    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.

  18. NMR-Based Milk Metabolomics

    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.

  19. NMR-Based Milk Metabolomics.

    Sundekilde, Ulrik K; Larsen, Lotte B; Bertram, Hanne C

    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 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. PMID:24957988

  20. Structural proteomics by NMR spectroscopy.

    Shin, Joon; Lee, Woonghee; Lee, Weontae

    2008-08-01

    Structural proteomics is one of the powerful research areas in the postgenomic era, elucidating structure-function relationships of uncharacterized gene products based on the 3D protein structure. It proposes biochemical and cellular functions of unannotated proteins and thereby identifies potential drug design and protein engineering targets. Recently, a number of pioneering groups in structural proteomics research have achieved proof of structural proteomic theory by predicting the 3D structures of hypothetical proteins that successfully identified the biological functions of those proteins. The pioneering groups made use of a number of techniques, including NMR spectroscopy, which has been applied successfully to structural proteomics studies over the past 10 years. In addition, advances in hardware design, data acquisition methods, sample preparation and automation of data analysis have been developed and successfully applied to high-throughput structure determination techniques. These efforts ensure that NMR spectroscopy will become an important methodology for performing structural proteomics research on a genomic scale. NMR-based structural proteomics together with x-ray crystallography will provide a comprehensive structural database to predict the basic biological functions of hypothetical proteins identified by the genome projects. PMID:18761469

  1. 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

    Highlights: ► Electro-chemical Al deposition is industrially relevant for barrier formation. ► Al scales have to be converted into protective layers by heat treatments. ► Morphology of scales depend on deposition parameters. ► Solid state diffusion step at 640 °C avoids critical Al melting and activates steel surface. ► Al2O3 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 Al2O3 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.

  2. 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

    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.

  3. NMR spectroscopy: structure elucidation of cycloelatanene A: a natural product case study.

    Urban, Sylvia; Dias, Daniel Anthony

    2013-01-01

    The structure elucidation of new secondary metabolites derived from marine and terrestrial sources is frequently a challenging task. The hurdles include the ability to isolate stable secondary metabolites of sufficient purity that are often present in conversions and/or degradations. Immediately after purification, the next step is to rapidly acquire all analytical spectroscopic data in order to complete the characterization of the isolated secondary metabolite(s), prior to any possible decomposition. The final hurdle in this multiple step process, especially in the acquisition of the NMR spectroscopic and other analytical data (mass spectra, infrared and ultra-violet spectra, optical rotation, etc.), is to assemble the structural moieties/units in an effort to complete the structure elucidation. Often ambiguity with the elucidation of the final structure remains when structural fragments identified are difficult to piece together on the basis of the HMBC NMR correlations or when the relative configuration cannot be unequivocally identified on the basis of NOE NMR enhancements observed. Herein, we describe the methodology used to carry out the structure elucidation of a new C16 chamigrene, cycloelatanene A (5) which was isolated from the southern Australian marine alga Laurencia elata (Rhodomelaceae). The general approach and principles used in the structure determination of this compound can be applied to the structure elucidation of other small molecular weight compounds derived from either natural or synthetic sources. PMID:23963906

  4. A spectroscopic assignment technique for membrane proteins reconstituted in magnetically aligned bicelles

    Oriented-sample NMR (OS-NMR) has emerged as a powerful tool for the structure determination of membrane proteins in their physiological environments. However, the traditional spectroscopic assignment method in OS NMR that uses the “shotgun” approach, though effective, is quite labor- and time-consuming as it is based on the preparation of multiple selectively labeled samples. Here we demonstrate that, by using a combination of the spin exchange under mismatched Hartmann-Hahn conditions and a recent sensitivity-enhancement REP-CP sequence, spectroscopic assignment of solid-state NMR spectra of Pf1 coat protein reconstituted in magnetically aligned bicelles can be significantly improved. This method yields a two-dimensional spin-exchanged version of the SAMPI4 spectrum correlating the 15N chemical shift and 15N–1H dipolar couplings, as well as spin-correlations between the (i, i ± 1) amide sites. Combining the spin-exchanged SAMPI4 spectrum with the original SAMPI4 experiment makes it possible to establish sequential assignments, and this technique is generally applicable to other uniaxially aligned membrane proteins. Inclusion of an 15N–15N correlation spectrum into the assignment process helps establish correlations between the peaks in crowded or ambiguous spectral regions of the spin-exchanged SAMPI4 experiment. Notably, unlike the traditional method, only a uniformly labeled protein sample is required for spectroscopic assignment with perhaps only a few selectively labeled “seed” spectra. Simulations for the magnetization transfer between the dilute spins under mismatched Hartmann Hahn conditions for various B1 fields have also been performed. The results adequately describe the optimal conditions for establishing the cross peaks, thus eliminating the need for lengthy experimental optimizations.

  5. Contributions of excited {sup 6}Li and {sup 7}Li nuclei to the production of {sup 4}He+{sup 2}H and {sup 4}He+{sup 3}H systems in {sup 16}O{sub p} collisions at a momentum of 3.25 GeV/c per nucleon

    Olimov, K., E-mail: olimov@uzsci.net [Uzbek Academy of Sciences, Physical-Technical Institute, Fizika-Solntse Research and Production Association (Uzbekistan); Glagolev, V. V. [Joint Institute for Nuclear Research (Russian Federation); Gulamov, K. G.; Lutpullaev, S. L.; Kurbanov, A. R.; Olimov, A. K.; Petrov, V. I.; Yuldashev, A. A. [Uzbek Academy of Sciences, Physical-Technical Institute, Fizika-Solntse Research and Production Association (Uzbekistan)

    2013-07-15

    New experimental data on the cross sections for the yield of excited {sup 6}Li* and {sup 7}Li* nuclei and on their contributions to the production of {sup 4}He + {sup 2}H and {sup 4}He+{sup 3}H light dinuclear systems in {sup 16}O{sub p} collisions at a momentumof 3.25 A GeV/c per nucleon are presented.

  6. Spectroscopic analysis of optoelectronic semiconductors

    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. Effects of the Fluorine-Substitution and Acid Treatment on the Electrochemical Performances of 0.3Li2MnO3·0.7LiMn0.60Ni0.25Co0.15O2 Cathode Material for Li-Ion Battery

    The 0.3Li2MnO3·0.7Li[Mn0.60Ni0.25Co0.15]O1.975F0.025 cathode materials were synthesized by using a co-precipitation process in a Couette-Taylor reactor. Fluorine was substituted to facilitate the movement of lithium ions by forming more compact SEI layer and reduce the dissolution of transition metals, and lower internal impedance with charging/discharging cycling. In order to chemically remove the Li2O, the 0.3Li2MnO3·0.7Li [Mn0.60Ni0.25Co0.15]O1.975F0.025 composites was preconditioned by a HNO3 solution. The acid-treated 0.3Li2MnO3·0.7Li[Mn0.60Ni0.25Co0.15]O1.975F0.025 was showed the low initial irreversible capacity and the higher discharge capacity. The acid-treated and fluorine-substituted materials delivered the low initial discharge capacities, but it gradually increased during cycles

  8. Integrated analysis of spectroscopic data

    Spectroscopic data are analysed by fitting a collisional-radiative model to the emission spectrum of a low-temperature plasma in the wavelength range of visible light. The inference procedure employs Bayesian probability theory and accounts for all measurement and model uncertainties. This allows for the validation of model parameters, such as atomic data obtained in recent close-coupling calculations, which are ore only partly or not at all accessible by beam-type experiments. Initial results indicate that the spectroscopic data contain significant information about some Einstein coefficients for spontaneous emission of less prominent spectral lines. (author)

  9. Detection of Potential TNA and RNA Nucleoside Precursors in a Prebiotic Mixture by Pure Shift Diffusion-Ordered NMR Spectroscopy

    Islam, S

    2013-01-01

    In the context of prebiotic chemistry, one of the characteristics of mixed nitrogenous-oxygenous chemistry is its propensity to give rise to highly complex reaction mixtures. There is therefore an urgent need to develop improved spectroscopic techniques if onerous chromatographic separations are to be avoided. One potential avenue is the combination of pure shift methodology, in which NMR spectra are measured with greatly improved resolution by suppressing multiplet structure, with diffusion-...

  10. A DVD Spectroscope: A Simple, High-Resolution Classroom Spectroscope

    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…

  11. Effect of paramagnetic impurities on NMR in superionic conductors

    Relaxation of mobile 7Li nuclei in LiAlSiO4 and other Li+ conductors is shown by the high temperature T1 : T2 ratio to be caused by paramagnetic impurities. The stationary 27Al, however, is relaxed by quadrupole coupling

  12. Quality assessment of protein NMR structures

    Rosato A.; Montelione G.T.; Tejero R.

    2013-01-01

    Biomolecular NMR structures are now routinely used in biology, chemistry, and bioinformatics. Methods and metrics for assessing the accuracy and precision of protein NMR structures are beginning to be standardized across the biological NMR community. These include both knowledge-based assessment metrics, parameterized from the database of protein structures, and model versus data assessment metrics. On line servers are available that provide comprehensive protein structure quality assessment ...

  13. NMR INVESTIGATIONS OF HYDROGENATED AMORPHOUS SILICON

    J. Reimer

    1981-01-01

    A review is presented of the N.M.R. (Nuclear Magnetic Resonance) studies to date of hydrogenated amorphous silicon-hydrogen films. Structural features of proton N.M.R. lineshapes, dynamics of hydrogen containing defect sites, and the promise of quantitative determinations of local silicon-hydrogen bonding environments are discussed in detail. Finally, some comments are given on future directions for N.M.R. studies of hydrogenated thin films.

  14. An Inversion Recovery NMR Kinetics Experiment

    Williams, Travis J.; Kershaw, Allan D.; Li, Vincent; Wu, Xinping

    2011-01-01

    A convenient laboratory experiment is described in which NMR magnetization transfer by inversion recovery is used to measure the kinetics and thermochemistry of amide bond rotation. The experiment utilizes Varian spectrometers with the VNMRJ 2.3 software, but can be easily adapted to any NMR platform. The procedures and sample data sets in this article will enable instructors to use inversion recovery as a laboratory activity in applied NMR classes and provide research students with a conveni...

  15. NMR studies of isotopically labeled RNA

    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.

  16. Ligand-receptor Interactions by NMR Spectroscopy

    Novak. P.

    2008-04-01

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

  17. NMR exposure sensitizes tumor cells to apoptosis.

    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. PMID:16528477

  18. Spin-Exchange Pumped NMR Gyros

    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.

  19. Advance reservoir evaluation by using NMR logging

    Based on brief explanation of the measurement principle for nuclear magnetic resonance (NMR) logging, this paper illustrates the importance of NMR logging in reservoir evaluation through typical case examples. These case examples include: Reservoir characterization and productivity evaluation by using NMR logging, determination of reservoir porosity in complex lithology, identification of oil, water and gas zones under complex reservoir conditions where resistivity log data give poor indication, guiding the implementation of completion and drilling programs, etc. Excellent application results indicate that NMR logging has its special features and advantages in comparison with conventional logging techniques. It is a very practical and very promising logging technology

  20. NMR characterization of pituitary tumors

    Twelve patients (5 male, 7 female, mean age 37.9 +- 20) with pituitary tumors were extensively evaluated with NMR imaging using a 1.5K gauss resistive magnet. Saturation recovery (SR), inversion recovery (IR) and spin echo (SE) pulse sequences were used for qualitative characterization of the lesions. T/sub 1/ calculations were also performed for brain and pituitary. Tumor histology and endocrine status were correlated with NMR data. All tumors were large with suprasellar extension (6 with prolactin secretion, 6 without). Pituitary T/sub 1/'s ranged from .2 to .64, the mean T/sub 1/ being longer than that of brain (Brain = .4 +- .04; Pit = .48 +- .14). 3 patients with histological evidence of homogeneous adenomas had long T/sub 1/'s (0.58 +- .05). 3 patients with evidence of recent or old hemorhage into the pituitary had much shorter T/sub 1/'s (0.29 +- .12). There was no relationship between prolactin secretion and T/sub 1/. Qualitative T/sub 1/ and T/sub 2/ information can be obtained by using a combination of SR, IR, and SE images. Using this method in the patients, homogeneous adenomas had similar T/sub 1/'s and longer T/sub 2/'s compared to the brain, while patients with bleeds had shorter T/sub 1/'s and T/sub 2/'s. Image T/sub 1/ characteristics correlated well with the calculated T/sub 1/ values. The range of T/sub 1/ (and potentially T/sub 2/) values which occur in apparently similar lesions are most likely due to anatomical and pathophysiological variations in these lesions. It may be ultimately possible to separate different types of pathological processes based on NMR image T/sub 1/ and T/sub 2/ characteristics after careful comparative studies of NMR and histological data are completed. The combination of calculated T/sub 1/ and T/sub 2/ with image T/sub 1/ and T/sub 2/ information may also be useful in further characterization of lesions