High-resolution magic-angle-spinning solid state

High-Resolution Magic Angle Spinning and Cross-Polarization Magic Angle Spinning Solid-State NMR Spectroscopy... 

In addition to the standard solid state MAS-NMR methods, Bliimel and co-workers employed high-resolution magic angle spinning NMR of suspensions, which they abbreviated as HRMAS experiments, for the investigation of the structure of phosphine linkers and homogenous catalyst immobilized on the silica surface. The resulting HRMAS NMR... 

High-resolution magic-angle-spinning (HR MAS) solid state NMR was shown to provide compound identification of separated TLC zones without elution (Wilson et al., 1997). Zones were removed by scraping from Cij-bonded plates, slurried with D2O, and placed in a sealed 4-mm zirconia MAS rotor of a Brucker DRX-600 NMR spectrometer for H NMR observation. Spectra were illustrated for 10 J.g of salicylic acid and phenolphthalein glucuronide, which quantity can be obtained from spots on an analytical plate without the need for preparative layer chromatography. 

However, it is found that a combination of techniques, such as proton dipolar decoupling (removes the dipolar interactions), magic angle spinning (reduces the chemical shift tensor to the isotropic chemical shift value), and cross-polarization (increases the sensitivity of rare spins, like 13C) applied to a solid state material, results in sharp lines for 13C nuclei in the solid state10). Thus, the observation of narrow lines or high resolution NMR in the solid state is possible. 

We have in the review described one of the most fascinating, powerful, fundamentally important facets of solid-state NMR spectroscopy, namely the combination of the high-resolution facets of magic-angle-spinning NMR and the informationbearing reintroduction of specific interactions in certain periods of the experiment via recoupling. 

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