The synthesis and characterization of iron-containing MCM-41 porous silica using the exchange method of the template with the iron salts FeCl3.6H(2)O and (Fe3Ac6O.3H(2)O)NO3 is reported. Proper conditions under which the exchange reactions can be accomplished without destroying the lattice structure of the parent MCM-41 material were examined, Quantitative measurements upon template removal reveal the existence of ion pairs of surfactant molecules as a constituent of the template structure. Mesoporous silica planted with iron exhibits good thermal stability and high surface areas. Reflectance-IR, EPR, and Mossbauer measurements provide clear evidence for the iron grafting into the silicon oxide network of the calcined products.