Iron- and titanium-modified MCM-41 materials, prepared by direct synthesis at ambient temperature or wet impregnation technique, were investigated using X-ray diffraction (XRD), transmission electron microscopy (TEM), temperature-programmed reduction (TPR), UV-vis diffuse reflectance, Mossbauer and FT-IR spectroscopies. Their catalytic behavior was studied in total oxidation of toluene. Materials with high surface area and well-ordered pore structure were obtained. The increase of the titanium content(up to 50%) in the bisubstituted, iron and titanium containing materials leads to partial structure collapse of the silica matrix. Finely dispersed anatase particles were also formed during the impregnation procedure. The catalytic activity of the bisubstituted materials was influenced by the method of their preparation, but higher catalytic stability could be achieved. compared to iron monosubstituted one. The nature of the catalytic active sites is discussed. (C) 2009 Elsevier B.V. All rights reserved.