The frontal cascade ultrafiltration (UF) technique in conjunction with stripping chronopotentiometry (SCP) has been evaluated for determining the colloidal distribution of Cu, Pb and Cd in estuarine waters. Metallic concentrations in seven size fractions (0.45 μm–0.22 μm; 0.22 μm–300 kDa; 300–50 kDa; 50–30 kDa; 30–10 kDa; 10–5 kDa; <5 kDa) were determined with the aim to investigate their changes along the salinity gradient of the Penzé system (NW France). These data, completed by analysis of the total dissolved metals at 10 stations over the whole freshwater–seawater mixing zone, provided some insights in the removal and addition processes that affect Cu, Pb and Cd in estuaries.