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U.S. Department of Energy
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Development of instrumental techniques for coal surface analysis: Functional group analysis in coal by /sup 31/ NMR spectroscopy: Quarterly report, 1 April 1988--30 June 1988

Technical Report ·
OSTI ID:6983518

A selection of phosphorus-containing compounds has been evaluated as potential derivatizing reagents for the analysis, by /sup 31/P NMR spectroscopy, of labile hydrogen functional groups in coal-derived materials. These reagents include dioxaphospholanes (1--5), a diazaphospholane (6), dithiaphospholanes (7--9), and a dithiaphosphorane (10). These reagents have been tested on a large number of model compounds and model compound mixtures for their ability to separate the /sup 31/P chemical shift ranges associated with derivatized functional groups (i.e., phenols, alcohols, carboxylic acids, amines, and thiols) and to resolve within these ranges chemical shifts due to the variety of organic substituents on the functional group. Thus far, reagent 7 has been found to yield the best results. Preliminary screening of a low-temperature coal pyrolysis condensate derivatized with 7 demonstrates the potential of this reagent for the identification and possible quantitation of individual heteroatom components in condensates. 9 refs., 3 figs., 1 tab.

Research Organization:
Ames Lab., IA (USA)
DOE Contract Number:
W-7405-ENG-82
OSTI ID:
6983518
Report Number(s):
IS-4974; ON: DE89003766
Country of Publication:
United States
Language:
English