Chemistry

Applied Chemistry at Protein Interfaces by Gould R.F. (ed.)

By Gould R.F. (ed.)

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6 Schematic presentation of events during a rotation sweep. The mixing flowchart presents a two-step relayed mixing process. Original populations along F1 in sites S3, S2 and S1 end up in positions as shown in the top line. The rectangle presents the resulting 2D spectrum, where original populations project to F1 and final populations to F2. 2D correlation is derived from labels of mixing flowchart top line (F1 coordinate) and positions (F2 coordinate). The relayed process of semi-adiabatic polarization transfer renders the cross-peak pattern asymmetric about the diagonal.

For example, a robust broad-band cross-polarization approach was experimentally demonstrated [12]. 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.

References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . E. Vinogradov et al. Abstract We describe radiofrequency (RF) pulse schemes in solid-state NMR applied to samples rotating at the magic angle (MAS) to obtain high-resolution 1 H spectra. Without combined RF schemes and MAS, 1 H spectra are normally severely broadened by the strong homonuclear proton-proton dipolar couplings. This review gives an outline of a representative class of multiple-pulse sequences, designed to work with and without MAS, and commonly used for high-resolution proton spectroscopy in solid-state NMR.

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