| The technology of stationary phase has been developed quickly in recent years, and themonolithic material as a separation medium has been applied to chromatographic separations. Asa new material of stationary phase, titania has attracted considerable attentions because of itsexcellent pH stability, superior mechanical strength, great thermal stability and amphoteric ionexchanger characteristic. Another unique advantage of using titania as the chromatographicmaterial is its ability to selectively adsorb organophosphate compounds, which can be used toselectively enrich or isolate phosphate compounds. The combination of titania with stationaryphase has exhibited great advantages, which can solve the disadvantage that the silica-basedstationary phases do not withstand high or low pH. Moreover, it can be used to analyze largequantities samples quickly, especially in the field of proteins and peptides. In this paper,monolithic titania materials were prepared through a template-free sol-gel synthesis route, andusing pure TiO2monolith, chromatographic separation of carboxylate compounds wassuccessfully demonstrated, which exhibited the excellent property of chromatography separation.In this paper, there existed four aspects:(1) The materials of titania monolith were prepared through a template-free sol-gel synthesisroute, via using titanium isopropoxide as titania source, while acetate and hydrochloric acid wereused as additives. The synthesized titania monoliths can be controlled by adjusting the content ofacetate、hydrochloric acid and water in the initial reaction solvent. Titania monoliths with morethan10cm in length, the mean mesopore of8.95nm, and the BET surface area of88m2/g, wereobtained after350℃calcination, which can be used as high performance liquid chromatographycolumn.(2) The carboxylate compounds standards were analyzed with the synthesized titaniamonolithic column, evaluating the performance of titania monolithic column by columnefficiency, resolution and so on.(3) The standard of benzoic acid was analyzed with synthesized titania monoliths column,and the factors in the chromatographic condition that could influence benzoic acid on titaniamonolithic column were studied.(4) The compounds of benzoic acid and vanillin were analyzed with synthesized titania monolithic column, in order to fully understand the retention mechanism of benzoic acid andvanillin on titania, acetonitrile percentage, buffer concentration and buffer pH of the mobilephase were investigated. |
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