Composite SiO2—iron oxide materials were prepared by three experimental procedures. In the first case, the iron oxides were precipitated during a sol-gel process. In the second case, a SiO2 matrix was initially obtained, and the iron oxides were formed by thermal treatment after impregnation of a soluble Fe2+ salt in the previously processed matrix. In the third method, ferrite powders, prepared by wet chemical method, were embedded into a SiO2 based sol-gel matrix. Materials with convenient porosity and nano-sized iron oxide content could be prepared using the mentioned methods. The prepared composite has been tested for arsenic(V) removal.