A phosphonate-rich organosilica layered hybrid material (PSLM) made of 3-(trihydroxysilyl)propyl methylphosphonate, monosodium salt, as the single silica source, has been obtained from its aqueous solution through a xerogel process and mild thermal aging. The method is simple, affording bulk quantities of powdered PSLM in a single-step. The hybrid is stable in water and possesses a high content of phosphonate groups fixed on the solid matrix. In addition, PSLM shows good thermal stability, which exceeds 300 degrees C in air. The material was characterized using SEM, TEM, XRD, FT-IR and TGA techniques. Potentiometric titrations show that PSLM bears high-surface density of phosphonate groups (3 mmol g-1). As a result, the material displays high metal uptake capacity for heavy metal ions such as Cu2+ (2.72 mmol g-1), pb2, (1.67 mmol g-1) and Cd2+ (1.00 mmol g-1) at neutral pH values e.g. the pH of natural waters. Detailed theoretical modeling using a Surface Complexation Model combined with Electron Paramagnetic Resonance (EPR) spectroscopy shows that the surface distribution of surface bound Cu2+ ions is rather homogeneous e.g. copper-binding phosphonate sites are arranged in average distances 5-8 A. 2014 Elsevier B.V. All rights reserved.