Solids magic angle spinning

Figure 6 Solid state static and magic-angle spinning NMR spectra of a-Mg2V2(>7.

Solid-state Alnmr spectroscopy has been much used in recent years to study the composition and structure of aluminisilcates (pp. 351 -9) and other crystalline or amorphous Al compounds. The technique of magic angle spinning (MAS) must be used in such cases. ... 

J. w. Geus, The interlayer collapse during dehydration of synthetic Na -beidellite a %a solid -state magic-angle spinning NMR study. Clays Clay Minerals. 25 457 (1992). 

As a consequence of restricted internal mobility in molecules in the crystalline state, nuclei in different conformation environments, but identical in other respects, can produce different signals in 13C cross polarization, magic angle spinning (CPMAS) solid-state NMR. This analysis is not necessarily limited to crystalline regions, since signals of different conformations are resolved if the exchange is slow with respect to the time scale of the NMR experiment. 

We used modifications of the standard solid-state CP-MAS (cross-polarisation, magic-angle spinning) experiment to allow the proton relaxation characteristics to be measured for each peak in the C spectrum. It is known that highly mobile, hydrated polymers can not be seen using either usual CP-MAS C spectrum or solution NMR (6). We found, however, that by a combination of a long-contact experiment and a delayed-contact experiment we could reconstruct a C spectrum of the cell-wall components that are normally too mobile to be visible. With these techniques we were able to determine the mobility of pectins and their approximate spatial location in comparison to cellulose. 

NMR of solids is a very diverse collection of methods, and the practice of applying it to chemisorption is changing dramatically as a result of advances in theoretical chemistry including reliable chemical shift calculations. The wide application of NMR to solid state chemistry grew out of the revival of magic angle spinning in the mid 1970 s. This line... 

Synthesis of compounds on solid-phase supports became quite popular in the late 1990s and, though interest might have waned a little more recently, there may still be a demand for it in some establishments. If monitoring reactions carried out on resins is what is required, then a magic angle spinning (MAS) probe is the only way to go. 

Figure 1 Schematic representation of the 13C (or 15N) spin-lattice relaxation times (7"i), spin-spin relaxation (T2), and H spin-lattice relaxation time in the rotating frame (Tlp) for the liquid-like and solid-like domains, as a function of the correlation times of local motions. 13C (or 15N) NMR signals from the solid-like domains undergoing incoherent fluctuation motions with the correlation times of 10 4-10 5 s (indicated by the grey colour) could be lost due to failure of attempted peak-narrowing due to interference of frequency with proton decoupling or magic angle spinning.

Table 1. Structural carbon distribution (%) of the humic acids extracted from soil horizons, adopted from Xing (2001). The distribution was calculated from solid state 13C Cross-Polarization Magic-Angle-Spinning (CP/MAS) NMR spectra. Chemical shift assignment for carbon functional groups alkyl 0-50 ppm O-alkyl 50-117 ppm aromatic 107-165 ppm.

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