The optimization of acid digestion of sediment samples was studied with the purpose of determining the metals (Al, Fe, Mn, Cr, Ni, V, Cu, Zn and Pb) using closed microwaves sisteem. For that, the recovery of these metals was noticed using certified reference materials: MESS-3, marine sediment, from the National Research Council of Canada (NRCC) and SRM 1645, river sediment, from the National Institute of Standards and Technology (NIST), with the determination performed by inductively coupled plasma optic emission spectrometry (ICP-OES). The acid digestion process with closed microwave system was optimized using factorial planning with three variables and two levels. As a result, the following operational conditions were achieved: maximum power of 600W, total digestion time of 40 minutes, and an acid mixture of 2 mL HNO3 + 6 mL HCl for 250 mg of sample digestion. Determination of these elements in 163 sediment samples from in the oil region of Bacia de Campos in the state of Rio de Janeiro, Brazil, was based on the methodology developed. The results were evaluated employing univariate and multivariate statistical techniques such as: linear regression, multiple regressions, Principal Component Analysis (PCA) and Cluster Analysis (CA). The data were compared with the results from the environmental diagnosis of oil exploration and production areas in Bacia de Campos, Santos and Espírito Santo (2002) by laboratory contracting by Petrobras.