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Preparation And Evaluation Of Stationary Phase For Capillary Gas Chro Matography

Posted on:2012-12-07Degree:MasterType:Thesis
Country:ChinaCandidate:H J WangFull Text:PDF
GTID:2231330374480815Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Development of novel chromatographic stationary phases is a hot topic in thecapillary gas chromatography. In this paper, two capillary columns with nanopolyelectrolyte particles as stationary phase and two capillary columns coating withPEG-20M modified by derivatives of poly (ethylene-alt-maleic acid). Theperformance of these columns was researched.Drived by electrostatic force between polyanion and polycation, poly(allylaminehydrochloride)(PAH)/poly(acrylic acid)(PAA) and PAH/-phenethylaminederivative of poly(ethylene-alt-maleic acid)(PEMA-PEA) particles were preparedunder the existence of excess PAH and were used to buildup capillary gaschromatographic columns. The properties of the columns were evaluated. The SEMimages show that diameters of PAH/PAA particles are330500nm and the diametersof PAH/PEMA-PEA particles are83115nm. McReynolds constants of columns withPAH/PAA and PAH/PEMA-PEA particles as stationary phases are1006and1049.Efficiencies of PAH/PAA and PAH/PEMA-PEA columns are2093and2799p·m-1forn-hexadecane. Maximum temperatures of PAH/PAA and PAH/PEMA-PEA columnsare260oC. Some non-polar compounds could be baseline resolved on both columns,indicating the nano polyelectrolyte particle has good application prospects for theanalysis of non-polar compounds.By using the reaction between anhydride and amino-or hydroxyl group, twocapillary columns coating with PEG-20M modified by α-phenethylamine (column I)and methionine derivatives of poly (ethylene-alt-maleic acid)(column II) wereprepared and performances of the columns were evaluated. FTIR spectra andelemental analysis data indicated that PEG-20M was modified successfully.McReynolds constants of column I and column II are762and606and Efficiencies ofcolumn I and column II are3066p·m-1and2998p·m-1for n-hexadecane. Maximumtemperatures of column I is260oC. Alkenes and esters could be baseline resolved onboth columns and methyl esters of aliphatic acid in oil and fats could be effectivelyseparated in short-time, indicating these columns have good application prospects forthe analysis of fatty acid composition in oil and fats.
Keywords/Search Tags:gas chromatography, stationary phase, polyelectrolyte, nanoparticle, oil and fats
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