This short paper highlights the unusual properties of the high-mass material of coal liquids isolated by their insolubility in pyridine and solubility in NMP. The separation has been achieved by a column chromatography method. One gram quantity have been processed and near quantitative recovery of the sample as fractions has been achieved. This fractionation permitted recourse to a broad range of analytical methods, including some (e.g. C-13 NMR), which require large sample sizes. Multiple macro analyses have been undertaken, using elemental analysis, TGA proximate analysis, NMR and FT-ir in addition to the micro-analytical methods used previously-pyrolysis-gc-ms, SEC, UV-fluorescence, probe-ms and MALDI-ms. The fractions show increasing concentrations of large molecular mass material with increasing polarity of successive eluents used in the fractionation. Evidence from solid-state 13C NMR and UV-fluorescence spectroscopy show progressive structural changes with increasing apparent molecular mass. (C) 2003 Elsevier Science Ltd. All rights reserved.