Solid state nuclear magnetic resonance

Spectral editing in 13C CP/MAS experiments at high magnetic field.

PMID 8784957


We show that the spinning side-bands of protonated and non-protonated carbon atoms can be well separated by means of the standard SCP and LCPD experiments at a relatively slow sample spinning rate or at high magnetic field. These experiments offer a promising way of measuring the principal values of chemical shift anisotropies via spinning side-band analysis in a moderately complex system. General spectral editing in 13C cross-polarization magic-angle spinning (CP/MAS) experiments at high field is achieved by incorporating the total side-band suppression (TOSS) pulse sequence into the standard series of spectral editing pulse sequences. It is confirmed that the relative signal intensity for a certain kind of functional group obtained at different polarization, polarization-inversion and depolarization times is about the same as that obtained at low magnetic field, and that the signal intensity distortion introduced by the TOSS sequence for resonances having different chemical shift anisotropies does not interfere with the spectral editing process. However, quantitative results can only be expected in those cases where full restoration of the intensity of the central band can be achieved by the TOSS sequence. This new strategy at high field is demonstrated by using fumaric acid monoethyl ester as a model compound. A typical application to a Chinese resin is presented, where the relative ratio of each functional group in the aliphatic portion to the total number of aliphatic carbon atoms is determined from only three experimental spectra.

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mono-Ethyl fumarate, 95%