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Liquid Chromatographic Stationary Phase Tio < Sub > 2 < / Sub > The Preparation And Application Of Research

Posted on:2013-10-29Degree:MasterType:Thesis
Country:ChinaCandidate:Y ZhouFull Text:PDF
GTID:2241330395990075Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Nowadays silica is the most widely used chromatographic stationary phase because of its high mechanical strength, the large specific surface area and the suitable pore volume. Meanwhile the good permeability and pore structure of silica are suitable for the chromatographic separation. While the silica will dissolve when pH<2or pH>8and some matters can cause the irreversible adsorption and also cause a smearing of the alkaline compounds in the separation. Thus the nature of silica limits the application in some important areas. Recent years TiO2can be used as the liquid chromatographic packings due to the good chemical stability and mechanical strength. TiO2is more stable in strong acid and strong alkali thus it can make up for the narrow pH range of silica. So TiO2is a good liquid chromatography packings for separating the alkaline samples, especiallysamples, especially for the biological macromolecules.There are several methods of synthesis the titanium oxide, such as the sol-gel, polymerization-induced colloid aggregation, microemulsion, hydrothermal, ethanol thermal, the chemical co-precipitation. In this paper, we choose the sol-gel method and hydrothermal method that are relatively simple to prepare the titania. The tetrabutyl titanate [Ti(OC4H9)4] and titanium tetrachloride (TiCl4) are separately used as the titanium source. And in order to seek the optimal condition, the synthesis was investigated by different methods and different conditions to test the impact of the preparation of TiO2microspheres. Through a series of experiments, the TiO2microspheres have a homogeneous particle size distribution with an average diameter of5μm and the pore volume of0.25cm/g, specific surface area of276.0m2/g. Titanium dioxide and C18-TiO2which was prepared based on TiO2microspheres were made into the normal phase chromatography packings and reversed phase columns. The normal phase chromatography was separated the mixture of benzene, nitrobenzene and nitro-anisole. Meanwhilie the reverse phase column was used to separate the mixture of p-nitroaniline, p-phenylenediamine, o-nitroaniline. The two columns both have better separation of two sets of mixture.
Keywords/Search Tags:titania, liquid chromatogram, stationary phase, sol-gel, hydrothermal treatmen
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