Dense silica microspheres (density 2.11-2.16 g cm-3) were obtained from a range of molar compositions tetraethyl orthosilicate (TEOS):CH3COOH:H2O = 1 :(0.5-4.0):(1.5-5.0), FTIR spectroscopic studies of the reaction between TEOS and CH3COOH in the presence and absence of water showed that acetic acid readily attacked TEOS and generated Si-OH groups via the formation of Si-OOCCH3 groups; (OH)-(OH) condensation finally led to the formation of silica particles.