The sorption capacity of untreated and alkaline-treated coconut shaft biosorbents for the removal of Pb 2+ from aqueous solution was investigated in batch experiments. Effects of contact time, biosorbent dose, initial metal concentration, and pH on the sorption capacity were investigated. Optimum Pb 2+ removal of 17.6 and 22.1 mg/g by untreated and alkaline-treated biomass was achieved at an initial metal concentration of 150 mg/L, a biomass dose of 0.7 g, a contact time of 80 min, and a pH of 4.0. The sorption data fitted well into the Langmuir isotherm, while kinetic modeling of the data from untreated biomass indicated conformity with the Lagergren pseudo-first-order model, whereas data from the treated biomass fit well with the Elovich model. FT-IR results gave indications of possible functional groups on the cell walls of the coconut shaft, including alcohols, amines, carboxylic acids, ester, and ethers. Thus, alkaline treatment of the coconut shafts enhanced the biosorption ability of Pb 2+ onto the coconut shaft biomass.