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The comparison of the temporal development of the X-ray reflection intensities of as-synthesized and calcined MCM-41 materials demonstrates that 90% of the hexagonal channel arrangement is formed after 5-6 h whereas the fully developed mesopore structure requires 72 h. The progress of the reaction can be quantified by reference to the maximum pore volume that can be obtained from adsorption isotherms or from model calculations based on the packing density of the surfactant and the pore wall thickness of ca. 1 nm. For low critical micelle concentrations the maximum amount of MCM-41 formed can be calculated and used as a reference in order to follow quantitatively the progress of the MCM-41 formation.