This work reports the optimization of a focused microwave assisted procedure for the wet acid dissolution of diesel oil in order to allow the determination of metals in the samples by inductively coupled plasma optical emission spectrometry (ICP-OES). The dissolution process was monitored by measuring residual carbon content (RCC), also by ICP-OES, in the final solutions obtained after application of digestion program. All experimental work was performed using a commercial sample of diesel oil containing 85.74 +/- 0.13% of carbon. The initial dissolution program comprised three steps: (i) carbonization with H2SO4; (ii) oxidation with HNO3 and (iii) final oxidation with H2O2. During work it was verified that the first step played an important role on the dissolution process of this kind of sample. It is therefore, necessary to give a detailed optimization of such step. Employing the optimized conditions it was possible to digest 2.5 g of diesel oil with a 40 min-heating program. At these conditions, residual carbon content was always lower than 5%. Optimized methodology was applied in the determination of metals in three diesel oil samples by ICP-OES. Recovery tests were also performed by adding 10 jig of metals, as organic standards, to the samples before digestion. Recovery percentages always higher than 90% were obtained for the metals of interest (Al, Cu, Fe and Ni), except for Zn, which presented recoveries between 70 and 78%. (C) 2007 Elsevier B.V. All rights reserved.