A solvent-insoluble fraction from three Arogonne Premium coals as reactants is used as reactants and the release of organic halogens (OHs) from the residues during noncatalytic and Ni-catalyzed hydrotreatments under relatively mild conditions is examined. The residues used as reactants are tetrahydrofuran/carbon disulfide insoluble fractions from three coals. After exhaustive extraction, THF and CS2 remaining in the residues were removed by extraction with acetone. Result of the study showed that some organic chlorines and organic iodines are released from coal residues during noncatalytic and Nickel catalyzed hydrotreatment at 300°C. The OHs may be a moiety of organic macromolecular species in the Arogonne premium coals.