Solid state nuclear magnetic resonance quantitative

Harris RK. 1985. Quantitative aspects of high-resolution solid-state nuclear magnetic resonance spectroscopy. Analyst 110 649-655. 

Suryanarayanan, R. and Wiedmann, T. S. (1990). Quantitation of the relative amounts of anhydrous carbamazepine (C15H12N2O) and carbamazepine dihydrate (C15H12N2O H2O) in a mixture by solid-state nuclear magnetic resonance (NMR). Pharm. Res., 1, 184-7. [142]... 

Abstract Modern solid state nuclear magnetic resonance presents new powerful opportunities for the elucidation of medium range order in glasses in the sub-nanometer region. In contrast to standard chemical shift spectroscopy, the strategy presented here is based on the precise measurement and quantitative analysis of internuclear magnetic dipole-dipole interactions, which can be related to distance information in a straightforward manner. The... 

The enantiomer and the racemic compound possess different crystal structures, which correspond to different intermolecular interactions, as mentioned in Sec. 3. Therefore the enantiomer and the racemic compound exhibit different powder x-ray diffraction (PXRD) patterns, different infrared (IR) and Raman spectra, and different solid-state nuclear magnetic resonance (SSNMR) spectra. However, the opposite enantiomers give identical PXRD patterns, and identical IR, Raman, and SSNMR spectra. Consequently, the PXRD patterns and the above spectra of a conglomerate, which is a physical mixture of opposite enantiomers, are identical to that of the pure enantiomers. In contrast, the diffraction pattern and the various corresponding spectra of the racemic compound usually differ significantly from those of the pure enantiomers. Therefore the type of racemate can be easily determined by comparing the diffraction patterns or the various spectra of the racemic species with that of one of the pure enantiomers (Figs. 3 5). The enantiomeric composition in a racemic mixture may be determined by PXRD, or by IR or SSNMR spectroscopy. Quantitative PXRD has been applied to determine the relative... 

Recent developments on acidity characterization of solid acid catalysts, specifically those invoking P solid-state nuclear magnetic resonance (SSNMR) spectroscopy using phosphorus-containing molecules as probes, have been summarized. In particular, various P SSNMR approaches using trimethylphosphine, diphosphines, and trialkylphosphine oxides (R3PO) will be Introduced, and their practical applications for the characterization of important qualitative and quantitative features, namely, type, distribution, accessibility (location/proximity), concentration (amount), and strength of acid sites in various solid acids, will be illustrated. 

The usefulness of XPS in the study of the surface chemistry of carbonaceous materials is well established [120-123]. It is significant, however, that in 1994, while reviewing some aspects of the surface chemistry of carbon blacks and other carbons (in particular, active carbons), Boehm [48] devoted only a few lines to XPS and argued that XPS is not very useful for quantitative determinations. The selected examples included here are meant to give the reader an idea of the use of XPS in the last decade, often in combination with other methods such as FTIR and TPD, and more recently with solid-state nuclear magnetic resonance (NMR), for both qualitative and quantitative characterization of the surface chemistry (i.e., functional groups) either of raw carbonaceous materials or after their treatment (e.g., activation, thermal or chemical treatment, and pyrolysis). 

Gerstein BC, Dybowski CR (1985) Transient techniques in NMR of solids an introduction to theory and practice Academic Press, Orlando, 295 pp Hatcher PG (1987) Chemical structural studies of natural lignin by dipolar dephased solid-state nC nuclear magnetic resonance Org Geochem 11 31-39 Hatfield GR, Maciel GE, Erbatur O, Erbatur G (1987) Qualitative and quantitative analysis of solid lignin samples by carbon-13 nuclear magnetic resonance spectrometry Anal Chem 59 172-179... 

Cody G. D., Alexander C. M. O D., and Tera E. (2002) Solid-state ( H and C) nuclear magnetic resonance spectroscopy of insoluble organic residue in the Murchison meteorite a self-consistent quantitative analysis. Geochim. Cosmochim. Acta 66, 1851-1865. 

Mao J.-D., Hu W.-G., Schmidt-Rohr K., Davies G., Ghabbour E. A., and Xing B. (2000) Quantitative characterization of humic substances by solid-state carbon-13 nuclear magnetic resonance. Soil Sci. Soc. Am. J. 64, 873-884. 

To determine the nature of the silicon moieties in a polymer, clearly the easiest method would be a technique that provides a direct observation of the silicon atom and meaningful, interpretable information on the atom. Nuclear magnetic resonance spectroscopy tuned to the Si isotope ( Si NMR) is a tool of this nature it can directly probe the state of the silicon atom, and with it one can often readily determine the extent to which Si-O-Si crosslinks (fi-om silanol condensation), have formed. One can observe spectra of silicon-containing compounds either dissolved in a solvent or in the solid state. Liquid-state Si NMR, while the most sensitive, cannot be used quantitatively on heterogeneous systems such a latex formulations. Therefore, one must separate the liquid and solid portions of the latex (without heat, which would promote hydrolysis and condensation) and use the solid residue for the Si NMR experiments. 

A 13C nuclear magnetic resonance (NMR) study in solution and in the solid state has been reported for three thermochromic spirooxazines, 29-31.32 From a quantitative analysis of I3C cross-polarization/magic-angle-spinning (CP-MAS) NMR spectra shielding anisotropies were estimated and a correlation of these characteristics with thermochromic activity was suggested. 

It can now be predicted with confidence that machine calculations will lead gradually toward a really fundamental quantitative understanding of the rules of valence and the exceptions to these toward a real understanding of the dimensions and detailed structures, force constants, dipole moments, ionization potentitils, and other properties of stable molecules and equally unstable radicals, anions, and cations, and chemical reaction intermediates toward a basic understanding of activated states in chemical reactions, and of triplet and other excited states which are important in combustion and explosion processes and in photochemistry and in radiation chemistry and also of intermolecular forces further, of the structure and stability of metals and other solids of those parts of molecular wave functions which are important in nuclear magnetic resonance, nuclear quadrupole coupling, and other interaction involving electrons and nuclei and of very many other aspects of the structure of matter which are now understood only qualitatively or semi-empirically. 

Quantitative characterization of humic substances by solid-state carbon-13 nuclear magnetic resonance. 2000 64 873-884. 

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