Preparation of porous titania microspheres for HPLC packing by sol–gel method

Porous micrometer titania microspheres for HPLC packing were prepared by sol–gel method with titanium isopropoxide (Ti(OPri)4) as titanium source. The effects of some factors including H2O, hydrochloric acid (HCl), and acetic acid (HAc) concentrations on the shape, diameter, gelation time, and specific surface area of the titania microspheres were discussed. The obtained titania microspheres were characterized by SEM and BET measurements. The results show that titania microspheres were mostly regular-ball with 5 μm average particle size, 60.31 m2/g surface area, 0.068 mL/g pore volume, and 5.18 nm average pore diameter.

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► Titania packing was prepared via a template-free sol-gel synthetic route.
► Surface area of microspheres is far greater than those of literatures.
► Microspheres have mesoporous texture, relative narrow particle sizes and pore diameter distribution.
► A new way to synthesize titania microspheres for HPLC has been developed.