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The hydrolysis process of bis-1,2-(triethoxysilyl)ethane (BTSE) was studied in aqueous and methanol solutions at pH 4. Nuclear magnetic resonance (NMR) evaluation of different solutions was carried out for 7 days. Unlike other researches, methanol-rich solutions are proven inadequate to reach a complete hydrolysis process. In water-rich solutions, hydrolysis takes place for 3 days, 85% of the silane molecules being transformed into silanols; this amount continues increasing up to the seventh day of hydrolysis.