The biosorptive potentials of three aquatics-based biosorbents, including shells of a bivalve mollusk and scales of two fish species for Pb removal from aqueous solutions were evaluated, for the first time. A Box–Behnken design with the response surface methodology was used to investigate the effects of the seven important variables (contact time, temperature, initial concentration, dosage, size, salinity and pH) on the sorption capacity of the sorbents. Among the seven studied factors, the effects of biosorbent dosage, initial concentration and pH were significant for all the response variables, while biosorbent size was not significant for any of the responses. The initial concentration was the most influential factor. The presence of Pb ions on the surfaces of the biosorbents after the adsorption was clearly confirmed by the SEM–EDX and XRF analyses. The maximum sorption capacities of the biosorbents were comparable to the literature and the descending order was as follows: scales of Rutilus kutum and Oncorhynchus mykiss and the shells of Cerastoderma glaucum. The isotherm studies revealed Langmuir model applicability for the Pb adsorption by R. kutum and O. mykiss scales, while Freundlich model was fitted to the adsorption C. glaucum shells.