New techniques in solid-state NMR by Jacek W. Hennel, Jacek Klinowski (auth.), Jacek Klinowski

By Jacek W. Hennel, Jacek Klinowski (auth.), Jacek Klinowski (eds.)

J. W. Hennel, J. Klinowski: Magic-Angle Spinning: a historic Perspective.-

A. Samoson, T.Tuherm, J. previous, A. Reinhold, T. Anupold, I. Heinmaa: New Horizons for Magic-Angle Spinning NMR.-

E. Vinogradov, P.K. Madhu, S. Vega: options for High-Resolution Proton Spectroscopy within the Solid-State NMR.-

M.J. Potrzebowski, S. Kazmierski: High-Resolution Solid-State NMR reviews of Inclusion Complexes.-

J. Rocha, C.M. Morais, C. Fernandez: development in Multiple-Quantum Magic-Angle Spinning NMR Spectroscopy.-

H. Eckert, S. Elbers, J.D. Epping, M. Janssen, M. Kalwei, W. Strojek, U. Voigt: Dipolar stable nation NMR techniques in the direction of Medium-Range constitution in Oxide Glasses.-

W. Kolodziejski: Solid-State NMR experiences of Bone.-

A.V. Ivanov, O.N. Antzutkin: normal Abundance 15N and 13C CP/MAS NMR on Dialkyldithiocarbamate Compounds with Ni(II) and Zn(II)

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TREV , a simpler version, based on time reversal echoes, was extended to the TREV decoupling scheme [ ]. A combination of three TREV magic-echo sandwiches with a relative phase difference of 120◦ resulted in the MSHOT sequence [ , ]. The TREV and MSHOT sequences are shown in Fig. The basic symmetric magic-echo sandwich can be represented by {τ − 90◦ y − βx − βx¯ − 90◦ y¯ − τ } ( ) where βx and βx¯ correspond to RF irradiation of intensity ω1 /2π and duration 2π/ω1 and τ a delay of length π/ω1 .

The approach is very similar to the single mode Floquet theory (SMFT) approach adapted by others to NMR spectroscopy [ ]. Following Eqs. , and b the RF interaction Hamiltonian can be expressed as Hint (t) = Hnk einωr t eikωc t ( ) n,k where the Fourier operator coefficients Hnk are defined in the same Hilbert space as the Hamiltonian itself. These time independent operator coefficients contain (l) (l) all parameters dmk , gn,a and Gn,ab , as well as the spin operators Tm , and can only be manipulated by changing the RF irradiation scheme.

Generally, efficient thermal contact between two spin species during sample spinning is provided only if the respective rf field amplitudes differ by a single or double rotation speed value. However, the rf field falls across the (regular pitch) solenoidal coil towards the coil ends in proportion to the maximum value, whereas spinning frequency is uniform. Therefore, whole sample cross-polarization is not possible if the two fields and sample spinning are kept constant. Fast acceleration is allowed to ramp the initially stationary sample to a regular high-resolution speed during the cross-polarization process.

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