NMR spectroscopy in the structural elucidation of oligosaccharides and glycosides.

13C NMR spectra of pentacyclic triterpenoids--a compilation and some salient features

The use of 13 carbon nuclear magnetic resonance (NMR) spectroscopy in the molecular characterization of macromolecules has advanced our knowledge into structural areas that have been nearly impossible to measure by other spectroscopic techniques. Innovative applications have led to determinations of polymer configurational distributions, comonomer sequence distributions, average sequence lengths, structure and distribution of short chain branches, and analyses of nonreactive end groups. As a result, the importance of 13C NMR to the field of polymer science cannot be overemphasized. The key to the success of 13C-NMR studies in defining polymer molecular structure has been a structural sensitivity which encompasses more than just a few functional groups or carbon atoms. A sensitivity to polymer repeat unit sequences of lengths from two to as many as five, seven, and even nine contiguous repeat units [1,2] has been observed. Of course, any structural technique that senses a unique response from as f...

A review of high resolution liquid 13carbon nuclear magnetic resonance characterizations of ethylene-based polymers

The introduction of Fourier transform methods has not only remarkably enhanced the sensitivity of high-resolution NMR spectroscopy, thus allowing measurements to be made on less sensitive nuclei of the Periodic Table, but also has paved the way for the development of a large number of new experimental techniques. On the one hand, procedures already known have been improved and can now be performed more rapidly, and, on the other, completely new experimental approaches have become available. This situation resulted mainly from the introduction of programmable pulse transmitters and the separation of the experiment into preparation, evolution, and detection. In particular, the concept of two-dimensional spectroscopy has opened up new possibilities important for the analysis of complicated spectra and is able to provide information previously not accessible. As elsewhere, optimum application of the techniques and correct interpretation of the results require sound understanding of the underlying physical principles. Since a rigorous mathematical treatment is complicated and does not necessarily improve the comprehensibility, this article attempts to give an illustrative presentation of the new pulse techniques within the framework of the Bloch vector model. After a short introduction covering the basic principles, one-dimensional pulse techniques that can be applied using standard experimental equipment are dealt with. The main areas of application are signal assignment, sensitivity enhancement for measurements on less abundant nuclei, and selective excitation of individual resonances. Subsequently, the various techniques of two-dimensional NMR spectroscopy are treated: these enable shift correlations for different types of nuclei to be made, the presentation of spin multiplets without overlap, and the analysis of geometrical relations as well as of chemical exchange phenomena.

James N Shoolery

Papers

Attached proton test for carbon-13 NMR