Hydroxylation/carbonylation carbonaceous microspheres (H/C CMSs) are designed as a "hunter" for lead(II) (Pb2+) in electrochemical detection. Without the need for external functionalization, the carbonyl and hydroxyl groups were introduced to the surface of carbonaceous spheres during hydrothermal synthesis using glucose. The features of H/C CMSs before and after lead adsorption were studied using FTIR and XPS. C=O and O-H vibrations were affected by lead adsorption, which can be attributed to the coordination bonds between oxygen atoms of C=O and O-H and Pb2+. A H/C CMSs modified glassy carbon electrode (GCE) was electrochemically characterized using cyclic voltammetry (CV). Anodic stripping voltammetric performance of bound Pb2+ was evaluated using square wave anodic stripping voltammetry (SWASV) analysis. Linear increases in the stripping peak current were observed for concentrations from 0 to 30 nM, with a sensitivity of 1.9067 mu A/nM. This was almost 260 times higher than the sensitivities to Cu2+ and Hg2+. A limit of detection was found to be 2 nM based on the 3 sigma method. The successive addition of 250 nM Zn2+, Cr3+, Cd2+, Cu2+, and Hg2+ to 25 nM Pb2+ acetate buffer solution did not interfere with the adsorption of Pb2+ and stripping of Pb-0. (C) 2012 Elsevier Ltd. All rights reserved.