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|Language of final thesis:||Slovak|
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|Title of the thesis:||Optimisation of Conditions for Selective Analysis of Substituted Phenols by Gas Chromatography|
|Summary:||The conditions for gas chromatographic analysis of alkylated phenols were investigated in individual single column and dual column setups. New materials for gas chromatography, namely new stationary phases containing the room temperature ionic liquids (RTILs) of mono- or di-cationic character with vinyl-imidazolium cation, were tested throughout the experiments. Two columns were used, one with mixed two-ionic-liquids phase and one with partially crosslinked phase. The outstanding polarity and shape selectivity was proved for the ionic liquid phases towards substituted phenols, expressed by their higher retention in column and interesting retention order in comparison to non-polar and medium polar polysiloxane stationary phases. The basic retention characteristics were measured for 40 individual phenols, and the temperature effects on retention and order of alkyl-phenols eluting from the columns were studied under isothermal conditions. The comparison with polysiloxane type columns enabled to assess the chromatographic characteristics of two ionic liquids. The result are promising for further incorporation of ionic liquid columns in column sets for dual column GC-GC, multidimensional GC or comprehensive GCxGC techniques. Individual columns analysis did not allow complete separation of studied alkyl-phenols in any conditions, but after optimization of analyses quite comparable separation was achieved in column k-4 with cross-linked ionic liquid in isothermal operation and in narrow-bore non-polar column k-1 for fast GC in programmed temperature operation, when 36 different alkyl-phenols were separated in individual peaks. Next experiments were performed with column coupling, the identification of alkyl-phenols was completed in three two-column series in isothermal conditions. The column combinations OV-1701/SPB-1, OV-1701/ionic liquid and ionic liquid/OV-1701 were tested as first and second column, respectively, the second column being 5-9 times shorter than the first one. In all cases the coupled columns provided better peak shapes and higher efficiency. The work has led to further plans of research tasks in use of new chromatographic materials for analysis of polar environment-contaminants. The work was part of research projects by Research and Development Support Agency 20-035205 and Scientific Grant Agency of Ministry of Education 1/0827/08.|
|Key words:||alkylphenols, ionic liquids, gas chromatography|
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