Two simple and straightforward procedures for determining the organic content of hybrid silica materials by means of conventional NMR and GC/MS techniques are described. The methods involve dissolving the hybrid material either in a concentrated solution of sodium hydroxide in deuterated water containing a suitable reference or in a solution of hydrogen fluoride in water and extracting with methylene chloride. These methods constitute useful routine techniques for obtaining immediate information concerning both the amount and chemical composition of the organic compounds on the silica surface.
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