The work presents a study through electroanalytical procedures for the determination of metals in gasoline samples. The determination of metals in fuel is an issue of environmental relevance because it believes that these elements can be released into the atmosphere causing damage to the environment and health. Also when present outside the established acceptable limit, the reactivity of these elements may directly imply the quality of the fuels. Thus, the use of low cost and efficient techniques such as electroanalytic are shown as a viable option for this purpose. The access to the metals by voltammetric techniques was only possible after the acid digestion of the samples and two digestion procedures were evaluated (Digestor Block and Microwaves) in different acid purities. The comparison between the two digestion systems (open and closed) using the same experimental conditions showed that the digestion in the closed system presented better results, due to the lower risk of contamination of the sample. The evaluated procedure presented satisfactory results from an analytical and statistical point of view and, therefore, it was considered adequate for the analyzed matrix.