Abstract

The carbonyl-labelled compound, [3.2.1]bicyclo-4-pyrrolidino- N-methyl-octan-8-one triflate ( 13CO-123), has been used as an intensity standard for quantitative 13C cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance (n.m.r.) analysis (including spin counting) of Argonne Premium coals. The cross-polarization time constants, T CH , and the rotating-frame proton spin-lattice relaxation times, T 1 ϱ H , have been determined for each major 13C peak of each coal via a combination of variable contact-time and variable spin-lock experiments. Two or three components of rotating-frame 1H relaxation decay and two or three components of T CH behaviour have been observed for each major 13C peak of each coal. These data have been used to determine the number of carbon atoms detected in each coal; these values are in the range 77–87% of the amount of carbon known to be in each coal from elemental analysis data, except for Pocahontas No. 3, for which only 50% of the carbon was detected.

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