A combination of spectroscopy methods (SEM, EDX, XRD, IR, and XPS) was used to study the morphology of Pittsburgh No. 8 Coal after electrolysis in 1.5 M H2SO4/100 mM Fe2+/100 mM Fe3+. The experiments were performed galvanostatically at different operating temperatures (40, 60, and 80 degrees C) in a continuous coal electrolytic cell. Pt-Ir-Rh plated on carbon fibers was used as anode. The results showed that the activity of the coal appears to increase with the temperature. Deactivation of electrooxidized coal seems to be associated with the formation of products on the surface of the coal. Differences in morphology and mineral composition were found in the coal electrolyzed by using SEM-EDX analysis. The minerals identified in the original coal sample by XRD, FTIR, and XPS were quartz, kaolinite, pyrite, and hematite. After electrooxidation illite and siderite were identified on the surface of coal. (c) 2006 Elsevier Ltd. All rights reserved.