This paper aims to evaluate the cylinder head carbon deposit from diesel engine fuelled by four samples of diesel fuel emulsions containing 0%; 5%; 10% and 15% vol. water and 20% Palm Oil Methyl Ester (POME) were subjected to thermogravimetric analysis (TGA/DSC) in air medium. The deposit build up processes were performed on a single-cylinder direct-injection diesel engine for period of 25 h for each set of test fuel under constant speed 2500 rpm. The TGA system was used and then correlated with elemental analysis as well as infrared spectra for microscopic observations. It has been found that, as the water increases in fuel, less aromatic and less reactive of deposits would be formed. Therefore, such method of analyses can be used as an indicator to verify the stability of carbon deposit inside the combustion chamber that could substantiate the applicability of a particular fuel to be accepted. (C) 2008 Elsevier Ltd. All rights reserved.