Fast Acquisition of <Superscript>13</Superscript>C NMR Spectra using the Steady-state Free Precession Sequence

In this paper, we show that the steady-state free precession sequence can be used to acquire ¹³C high-resolution nuclear magnetic resonance spectra and applied to qualitative analysis. The analysis of brucine sample using this sequence with 60o flip angle and time interval between pulses equal to 300 ms (acquisition time, 299.7 ms; recycle delay, 300 ms) resulted in spectrum with twofold enhancement in signal-to-noise ratio, when compared to standard ¹³C sequence. This gain was better when a much shorter time interval between pulses (100 ms) was applied. The result obtained was more than fivefold enhancement in signal-to-noise ratio, equivalent to more than 20-fold reduction in total data recording time. However, this short time interval between pulses produces a spectrum with severe phase and truncation anomalies. We demonstrated that these anomalies can be minimized by applying an appropriate apodization function and plotting the spectrum in the magnitude mode.     

Distribution of <Superscript>28</Superscript>Si, <Superscript>29</Superscript>Si,and <Superscript>30</Superscript>Si isotopes under plastic deformation in subsurface layers of Si: B crystals

The redistribution of ²⁸Si, ²⁹Si, and ³⁰Si isotopes in subsurface layers of Si: B single crystals after their plastic deformation has been revealed. It has been found that the distribution profile of ²⁸Si and ²⁹Si isotopes becomes smoother after deformation, whereas the ³⁰Si isotope distribution remains unchanged. A change in the subsurface profile of the ²⁹SiO oxide is observed, which indicates the migration of the ²⁹Si isotope in the composition of oxygen complexes during plastic deformation.     

<Superscript>29</Superscript>Si, <Superscript>27</Superscript>Al, <Superscript>1</Superscript>H and <Superscript>23</Superscript>Na MAS NMR Study of the Bonding Character in Aluminosilicate Inorganic Polymers

²⁹Si, ²⁷Al, ¹H and ²³Na solid-state magic-angle spinning (MAS) nuclear magnetic resonance (NMR) has been used to relate nominal composition, bonding character and compressive strength properties in aluminosilicate inorganic polymers (AIPs). The ²⁹Si chemical shift varies systematically with Si-to-Al ratio, indicating that the immediate structural environment of Si is altering with nominal composition. Fast ¹H MAS and ²⁹Si T _SiH/T _1ρ relaxation measurements demonstrated that occluded pore H₂O mobility within the disordered cavities is slow in comparison with H₂O mobility characteristics observed within the ordered channel structures of zeolites. The ²⁷Al MAS NMR data show that the Al coordination remains predominantly 4-coordinate. In comparison with the ²⁹Si MAS data, the corresponding ²⁷Al MAS line shapes are relatively narrow, suggesting that the AlO₄ tetrahedral geometry is largely unperturbed and the dominant source of structural disorder is propagated by large distributions of Si–O bond angles and bond lengths. Corresponding ²³Na MAS and multiple-quantum MAS NMR data indicate that Na speciation is dominated by distributions of hydration states; however, more highly resolved ²³Na resonances observed in some preparations supported the existence of short-range order. New structural elements are proposed to account for the existence of these Na resonances and an improved model for the structure of AIPs has also been proposed. Authors' address: John V. Hanna, NMR Facility, Institute of Materials and Engineering Science, Lucas Heights Research Laboratories, Australian Nuclear Science and Technology Organisation, Private Mail Bag 1, Menai, NSW 2234, Australia     

Perturbative role in the inelastic electron scattering from <Superscript>29</Superscript>Si

Inelastic electron scattering form factors away from the closed sd -shell are investigated. This investigation covers the low-lying states in ²⁹Si , which is considered according to the many-particle configuration mixing shell model as the ¹⁶O core, plus thirteen nucleons distributed over the entire sd -shell orbits. The investigation concentrates on the perturbative role of the core, which is called core polarization effects, on the inelastic electron scattering form factors. Core polarization effects are taken into consideration through the excitation of nucleons from 1s and 1p core orbits, and also from the 2s -1d valence orbits into higher shells, with 2ℏω excitations. Core polarization matrix elements are calculated with the M3Y effective interaction. For the sd -shell model space, a new Hamiltonian, based on a renormalized G -matrix, USDB, is used. All calculations are performed without adjusting any parameters.     

Determination of Enantiomeric Excess of Leucine by <Superscript>13</Superscript>C CP-MAS Solid-State NMR

The enantiomeric excess can be determined by many methods. One of them is nuclear magnetic resonance in solid state (SS-NMR). In this study we used the SS-NMR experiment of one-dimensional exchange spectroscopy by sideband alteration for determination of the enantiomeric excess of leucine. The density functional theory gauge-including atomic orbital calculations were used to assign all signals in ¹³C cross polarization magic-angle spinning spectra for two different molecules in the crystal lattice of L-leucine. Authors' address: Elżbieta J. Tadeusiak, Department of Structural Studies, Center of Molecular and Macromolecular Studies, Polish Academy of Sciences, Sienkiewicza 112, 90-363 Lodz, Poland     

<Superscript>2</Superscript>H and <Superscript>13</Superscript>C NMR investigation of deuterofullerites C<Subscript>60</Subscript>D<Subscript>x</Subscript>

Deuterofullerites C₆₀D_x have been studied by ²H and ¹³C NMR. These fullerites have two types of carbon–deuterium bonds: C–D terminal bonds, characterized by the quadrupole coupling constant (QCC) of 171 kHz, and –C ··· D ··· C– bridging bonds with a QCC of 56 kHz. The latter is responsible for the rigid lattice found in these fullerites, which is untypical of fullerenes. PACS 81.05.Tp; 82.56.Fk; 61.48.+c; 61.18.Fs; 61.10.Nz     

<Superscript>29</Superscript>Si nuclear spin relaxation in microcrystals of plastically deformed Si: B samples

Single crystals and microcrystals Si: B enriched with ²⁹Si isotopes have been studied using nuclear magnetic resonance and electron paramagnetic resonance (EPR) in the temperature range from 300 to 800 K. It has been found that an increase in the temperature from 300 to 500 K leads to a change in the kinetics of the relaxation of the saturated nuclear spin system. At 300 K, the relaxation kinetics corresponds to direct electron–nuclear interaction with inhomogeneously distributed paramagnetic centers introduced by the plastic deformation of the crystals. At 500 K, the spin relaxation occurs through the nuclear spin diffusion and electron–nuclear interaction with an acceptor impurity. It has been revealed that the plastic deformation affects the EPR spectra at 9 K.     

Raman spectroscopy of isotopically pure (<Superscript>12</Superscript>C, <Superscript>13</Superscript>C) and isotopically mixed (<Superscript>12.5</Superscript>C) diamond single crystals at ultrahigh pressures

The Raman scattering by isotopically pure ¹²C and ¹³C diamond single crystals and by isotopically mixed ^12.5C diamond single crystals is studied at a high accuracy. The studies are performed over a wide pressure range up to 73 GPa using helium as a hydrostatic pressure-transferring medium. It is found that the quantum effects, which determine the difference between the ratio of the Raman scattering frequencies in the ¹²C and ¹³C diamonds and the classical ratio (1.0408), increase to 30 GPa and then decrease. Thus, inversion in the sign of the quantum contribution to the physical properties of diamond during compression is detected. Our data suggest that the maximum possible difference between the bulk moduli of the ¹²C and ¹³C diamonds is 0.15%. The investigation of the isotopically mixed ^12.5C diamond shows that the effective mass, which determines the Raman frequency, decreases during compression from 12.38 au at normal pressure to 12.33 au at 73 GPa.     

Evolution of Airy structure in <Superscript>12</Superscript>C(<Superscript>12</Superscript>C, <Superscript>12</Superscript>C)<Superscript>12</Superscript>C between 5 and 10 MeV/A

We investigate the properties of a global optical potential, which describes the ¹²C + ¹²C elastic-scattering data between 70 and 130 MeV, within the nearside/farside and barrier-wave/internal-wave decomposition techniques. Particular emphasis is laid on the discussion of the incomplete absorption features of this system, and especially on the properties of the Airy minima which are observed in the experimental excitation function. The complicated angular and energy evolution of the data is explained in terms of the interference of a small set of scattering subamplitudes with a much simpler behavior.Received: 2 September 2003, Revised: 25 September 2003, Published online: 5 February 2004PACS: 24.10.-i Nuclear reaction models and methods - 24.10.Ht Optical and diffraction models - 25.70.Bc Elastic and quasielastic scattering     

<Superscript>1</Superscript>H and<Superscript>13</Superscript>C chemical shift assignments and stereochemistry of matrine and oxymatrine

Matrine and oxymatrine were extracted fromSophora flavescens, and their¹H and¹³C nuclear magnetic resonances (NMR) were unambiguously assigned by a combination of different two-dimensional 2-D¹H-¹³C and¹H-¹H correlation experiments of HMQC, HMQC-TOCSY and MAXY. The technique of using those experiments to make the assignment of the heavily overlapped spectrum is demonstrated. The coupling constants of matrine were measured by 2-DJ-resolved spectrum and 1-D spectra extracted from the slices of 2-D MAXY spectrum. The stereochemistry of the titled compounds was established from the NMR spectroscopy.     

Study of the Involvement of <Superscript>8</Superscript>Be and <Superscript>9</Superscript>B Nuclei in the Dissociation of Relativistic <Superscript>10</Superscript>C, <Superscript>10</Superscript>B,and <Superscript>12</Superscript>C Nuclei

The results obtained by estimating the contribution of 8Be and 9B nuclei to the coherent dissociation of ¹⁰C, ¹⁰B, and ¹²C relativistic nuclei in nuclear track emulsions (“white” stars) are presented. The selection of white stars accompanied by 9B leads to a distinct peak appearing in the distribution of the excitation energy of 2α2p ensembles and having a maximum at 4.1 ± 0.3 MeV. A 8Be nucleus manifests itself in the coherent-dissociation reaction ¹⁰B → ²He + H with a probability of (25 ± 5)%, (14 ± 3)% of it being due to 9B decays. The ratio of the branching fractions of the ⁹B + n and ⁹Be + p mirror channels is estimated at 6 ± 1. An analysis of the relativistic dissociation of ¹²C nuclei in a nuclear track emulsion revealed nine 3α events corresponding to the Hoyle state.     

Comparison of halo of <Superscript>11</Superscript>Be, <Superscript>15</Superscript>C,and <Superscript>19</Superscript>C

We have compared the halo of ¹¹Be, ¹⁵C, and ¹⁹C nuclei by analyzing the one-neutron stripping reaction data on the Be target at 60-, 54-, and 57-MeV/A beam energies, respectively, within the framework of the eikonal approximation approach. The determination of effective range through the comparison of the total cross section data and prediction has revealed that the halo of ¹⁹C is the well developed, while that of ¹⁵C is the least and that of ¹¹Be lies in between these two. The longitudinal momentum distribution data also strengthen these observations. The text was submitted by the authors in English.     

Simulation of NMR spectra of <Superscript>31</Superscript>P in the spinless <Superscript>28</Superscript>Si matrix and problems of the design of a solid-state quantum computer

The problem of numerical simulation of NRM spectra of the donor impurity in silicon is solved in the context of the fact that the system of nuclear spins of ³¹ P is planned to be used to organize working registers of a solid-state quantum computer. The proposed simulation method is shown to be applicable in the case of a quantitative increase of the NMR register and its topological complication. A scheme of readout of the results of “quantum counting” at a level allowing determination (with the help of SQUID) of the state of an individual spin is proposed.     

Features of <Emphasis Type="Italic">E</Emphasis>1 resonances in <Superscript>28</Superscript>Si and <Superscript>30</Superscript>Si nuclei

The structure of the E1 resonance in ²⁸Si and ³⁰Si isotopes is calculated within the particle–core coupling (PCC) version of the multiparticle shell model using experimental data on direct pickup reactions.     

<Superscript>23</Superscript>Na and <Superscript>27</Superscript>Al NMR Study of Structure and Dynamics in Mordenite

Temperature dependencies of ²⁷Al and ²³Na nuclear magnetic resonance spectra and spin–lattice relaxations in mordenite have been studied in static and magic angle spinning regimes. Our data show that the spin–lattice relaxations of the ²³Na and ²⁷Al nuclei are mainly governed by interaction of nuclear quadrupole moments with electric field gradients of the crystal, modulated by translational motion of water molecules in the mordenite channels. At temperatures below 200 K, the dipolar interaction of nuclear spins with paramagnetic impurities becomes an important relaxation mechanism of the ²³Na and ²⁷Al nuclei.     

Proton halo in the <Superscript>13</Superscript>N nucleus

We demonstrate that the radii of excited nuclear states can be estimated using the (³He, t) charge-exchange reaction and relying on the modified diffraction model. The radius of the N excited state with an excitation energy of E*=2.73 MeV, which lies in a continuous spectrum, is determined. The radius of this state proves to be close to that of the mirror 3.09-MeV state of the ¹³С nucleus, which possesses a neutron halo but lies in a discrete spectrum. Thereby, we demonstrate that the 2.37-MeV state of the ¹³N nucleus has a proton halo. The analysis is based on published measurements of differential cross sections for relevant reactions.