Water-pollution problems worldwide have led to an acute shortage of clean and pure water for both domestic and human consumption. Various technologies and techniques are available for water treatment which includes the use of activated carbon. In this study activated carbons used for the removal of lead (II) ions from water samples were prepared from maize tassels (an agricultural waste residue) which were modified using physical and chemical activation. In the physical activation CO2 was used as the activating agent, while in chemical activation H3PO4 with an impregnation ratio ranging from 1 to 4 was employed. The maize tassel was pyrolysed at different temperatures ranging from 300 °C to 700 °C in an inert atmosphere for a period of 60 min and activated at 700 °C for 30 min. The effects of activation temperature, impregnation ratio and duration were examined. The resultant modified tassels were characterised by measuring their particle-size distribution, porosities, pore volume, and pore-size distribution using scanning electron microscopy (SEM). The activated carbon produced by chemical activation had the highest BET surface area ranging from 623 m2 g−1 to 1 262 m2 g−1. The surface chemistry characteristics of the modified tassels were determined by FT–IR spectroscopy and Boehm’s titration method. The experimental data proved that properties of activated carbon depend on final temperature of the process, impregnation ratio and duration of the treatment at final temperature. The adsorption studies showed that chemically prepared activated carbon performed better than physically prepared activated carbon.