the sequential extraction procedure proposed by tessier and total digestion were applied for the analysis of sediment samples from tubar？o river. the recoveries were between 93.5 and 102.5% for cu and 99.2 and 111% for pb. the precision was tipically better than 6% for cu and 3% for pb. comparison of the values obtained for the total digest with the sum of the extracted fractions showed that there were no significant losses in the extraction steps so that the method can be used for the monitoring availability and mobility of these analytes. according to ten points of sampling, was possible to determined the average of labiles phases (fractions 1 and 4) for pb and cu: 33.70% and 18.18%, respectively; and the inert phases (fraction 5- residual): 66.30% for pb and 81.82% for cu.