Adsorption of lead ions in aqueous solution on gamma-Fe2O3-thiourea complex composite is reported. The adsorbent was characterised by X-ray diffraction (XRD), infrared (IR) and scanning electron micrograph (SEM) studies. The eluent was subjected to atomic absorption spectroscopy to determine the percentage of the adsorbed lead ions onto the complex composite. IR studies of the complex composite showed that the formation of hydrogen bond from the amine group of the thiourea to the surface hydroxyl groups, and lead ions adsorbed on adsorbent shows shift in frequencies and with appearance of some new peaks. SEM studies for pure gamma-Fe2O3 show particles in the range of 100-200 nm with varying shape and size. The adsorbent shows foam net like structure on the surface of the complex composite. Atomic absorption studies showed the decrease of lead ions to 50% after adsorption with the complex composite. Solution conductivity of the eluent is increased to double that of pure lead solution after adsorption. The potential use of gamma-Fe2O3-thiourea complex composite in adsorption study is explained.