Abstract
Heavy oil derived from coal hydrogenation was separated into saturated fractions, neutral aromatic oil, and asphaltene, and these materials were subsequently fractionated according to the magnitude of their respective molecular sizes by gel-permeation chromatography. These GPC subfractions were analysed by proton and carbon-13 n.m.r. spectroscopy and by an additional procedure using gas chromatography for the paraffinic GPC subfractions. 13C-n.m.r. spectra for the GPC subfraction of saturated material showed typical long straight-chain paraffin spectral patterns accompanied by iso-and cycloparaffinic carbon signals. The results from gas-chromatographic measurement for the paraffinic GPC subfractions agree fairly well with the trends of average carbon numbers and contents of straight-chain paraffins obtained by varying the fraction numbers, estimated from 13C-n.m.r. analyses. The ratios of aromatic carbon to total carbon ( f a ) for aromatic oil and asphaltene GPC subfractions obtained directly from 13C-n.m.r. spectra are slightly lower than the results from the 1H-n.m.r. method assuming x = y = 2 in the Brown—Ladner equation. Peak intensities of the respective carbon species in 13C-n.m.r. spectra were compared with the peak intensities of correspondingly bonded species obtained from 1H-n.m.r. measurement. Some inadequacy was recognized in both measurements. It is assumed that there are two reasons for the discrepancy, one of which is the inaccuracy of 13C-n.m.r. results owing to the long relaxation times and the effect of Nuclear Overhauser Enhancement, and another is the application of unsuitable values of x and y for calculations from the Brown—Ladner equation. New analytical treatments for 13C-n.m.r. results in combination with 1H-n.m.r. analyses are suggested in this study to avoid these uncertainties in structural analyses. From this procedure, it is believed that the actual contents of aromatic and aliphatic carbon and appropriate values of x and y can be derived.
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