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The ^Si and ^1H high-resolution liquid-phase NMR has been used to investigate the hydrolysis process of the tetraethyl orthosilicate(TEOS).^1H-NMR spectroscopy shows that the hydrolysis of TEOS in TPA is faster than in TEA.The impacts of TPA and TEA on the TOES hydrolysis process and its hydrolyzed product distribution have been observed by ^29Si-NMR respectively.The influences of water and the isopropyl alcohol on hydrolysis have also been diseussed.The presence of TBOT marks an evident differentiation between TPA and TEA for hydrolysis in ^29Si-NMR spectra.