Two Illinois No. 6 coal liquids (SOH and ASOH) were separated into polar and non-polar fractions and the polar fractions were analyzed to identify the phenols by RP HPLC in tandem with P-31 NMR spectroscopy of samples derivatized with ClPOCMe(2)CMe(2)O (1). The results obtained from both methods complement one another quite well despite numerous cases of more than one phenol displaying equal retention times or the same P-31 chemical shift when derivatized with 1. The total amount of phenolic oxygen was quantitatively determined by P-31 NMR spectroscopy for both coal liquids. The results agree very well with values reported by others by an FTIR method.