This project is about the pre-treatment of South African bituminous coal fines waste using an oxidising agent, hydrogen peroxide (H2O2) in the presence of ultraviolet light. The aim of the pre-treatment is to increase the abundance of solvent-extractable matter in coal so that it can be degraded by microorganisms during coal bioconversion because coal is a bio recalcitrant, complex and insoluble geopolymer, which is not readily degraded by microorganisms during the biogenic production of methane gas. This study characterised the compositional changes of organic compounds released from coal pre-treated with H2O2 at different concentrations: 3, 6 and 9% (v/v). The 3% (v/v) H2O2 pre-treatment has increased the abundance of solvent-extractable matter (oxygen-containing compounds) in the coal and resulted in 20 wt.% solubilisation compared to the other concentrations. Short chain acids were detected in the dissolved fraction, which are known to be good methanogenic substrates. These findings offer a good basis for coal solubilisation as a key starting point for biogenic production of methane gas.