As today the 137 Cs fallout peak, in sediment cores, corresponds only to 25% of its initial concentration, alternatives to the use of 137 Cs as a 210 Pb sediment dating validation tool are proposed. In highly industrialized bays, such as Guanabara Bay in the Rio de Janeiro metropolitan region, several chemical/compounds from the surrounding industry releases may be applied as validation tools. Chromium and copper profiles in a sediment core adequately fit the expected pattern due to the implementation of a chemical plant in 1958, reaching their maximum discharge in 1982 and subsequently decreasing due to the operation of a new wastewater treatment plant. A diffuse source such, as the PCB-based mixture Askarel, was also applied as an alternative validation tool, and the observed concentration profile reproduced the expected behavior, with increasing concentration after the Second World War and a decrease after the ban of this product in 1981. The observed Aroclor 1254 and 1260 mixture chlorination rates fit the most widely distributed PCB-based products in the country.