In this study, the synthesis of interpenetrated hybrid materials capable of removing arsenic from water is reported. These novel hybrid sorbents consisted of a polymeric matrix with quaternary ammonium groups and zirconium oxide as the organic and inorganic phase, respectively. Furthermore, a coupling agent was used to enhance the compatibility between the polymeric matrix and the metal oxide, creating a covalent bond between them. The hybrid sorbents were prepared by varying the mole ratio of the zirconium oxide precursor and the monomer to provide different surface compositions, and their effect on arsenic sorption was investigated. The hybrids were characterized by spectroscopic analysis such as, Fourier transform infrared spectroscopy (FTIR), C-13, and Si-29 solid-state nuclear magnetic resonance (NMR), thermal analysis (TGA), transmission and scanning electron microscopy (TEM, SEM-EDS), and FTIR microspectroscopy. Arsenite and arsenate sorption experiments were conducted under different experimental conditions (i.e., initial arsenic concentration, kinetics, and selectivity). The hybrids with a higher hydrous zirconium oxide content exhibited greater sorption of arsenite, and the sorbents with the lowest content exhibited greater sorption of arsenate. (C) 2015 Elsevier B.V. All rights reserved.