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Preparation And Characterization Of Complex-Functional Porous Silica Matrix Separation Medium

Posted on:2013-11-12Degree:MasterType:Thesis
Country:ChinaCandidate:B Y YuanFull Text:PDF
GTID:2231330374996556Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Chromatographic column is the key for Chromatographic separation, research anddevelopment on high performance stationary phase are therefore always the most active andpopular subjects in liquid chromatography. In high performance liquid chromatography andcapillary electro-chromatography variety of separation of materials have been used for avariety of different separation objects and separation mode. For the feature of narrow poresize distribution, large surface area of silica mesoporous separation materials, and suchmaterials can bring us the better separation effect, it is one of the most widespread use ofliquid chromatographyIn this paper, using (3-aminopropyl) triethoxysilane (APTES) and tetraethylorthosilicate (TEOS) as the silica sources,and using ammonia to regulate the pH value of thereaction solution, the functionalized porous hybrid silica as a separation medium wassynthesized in the presence of cetyltrimethyl ammonium bromide (CTAB) which was cationicsurfactant under the reaction conditions of80℃for80h. The synthesized materials werecharacterized by Fourier-Transform FTIR, SEM, nitrogenadsorption-desorptionmeasurements and pore structure measurements, and researched the affect regularity ofmaterial structure of the major product’s proportion and pH. The results of the experimentindicated that under the best preparation conditions of that pH=10,when the quality ofAPTES and TEOS are1.88g and2.50g, The best dosage pf CTAB is1.50g, add theamino into the silica gel skeleton in the materials for preparation, control its size range of0.5~2μm and pore size between3.8and~6.7nm. The column made by this porous silicahas been applied to separate hybrid. The results of HPLC shows that the synthesized materialshave good recognition of hybrid. The baseline separation of samples was achieved in6min.
Keywords/Search Tags:silica, separation medium, preparation, Liquid chromatography
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