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Lecturer(s)
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Jandera Pavel, prof. Ing. DrSc.
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Fischer Jan, doc. Ing. CSc.
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Course content
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Basic criterions of optimization of separation - quality of separation, sensitivity, amount of samples, time required for separation - and their influence on selection of optimization approach. Overview of working parameters determining quality of separation. Quality of separation evaluation criterions and their measurement - resolution, Kaiser separation criterion, peak capacity, chromatographic optimization function. Influence of sample composition structure on separation, its characterisation and prediction. Basic optimization strategies. Empiric and systematic approach to optimization of separation. One-parametric optimization of separation conditions. Window diagram method. Predictive methods of retention and separation selectivity optimization. Simultaneous multiparametric optimization - sequention and simultaneous strategy. Simplex method. Overlap resolution mapping method. Calculation of simultaneous optimization. Optimization of separation performance in gas and high-performance liquid chromatography with emphasis on time and pressure. Optimization of column dimensions, bed composition and mobile phase flow. Optimization of temperature of separation. Optimization of temperature gradient and gradient elution in chromatography. Multidimensional separation techniques. Optimization of separation conditions in capillary electrophoresis and micellar electrokinetic chromatography. Trace analysis - influence of working conditions in chromatography and electrophoresis on sensitivity and limit of detection and quantification, their optimization. Selectivity and sensitivity of detection and their optimization. Miniaturised separation systems - influence of miniaturisation on quality of separation, applications and instrumental limitations. Comparison of advantages and disadvantages of capillary chromatography, capillary electrophoresis and electrochromatography. Expert systems for optimization of chromatographic separations. Overview of commercial systems for automatic optimization of separation processes.
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Learning activities and teaching methods
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Monologic (reading, lecture, briefing)
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Learning outcomes
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The aim of the course is to obtain an overview of basic approaches and relevant knowledge of optimization of the analytical separation techniques. The use of basic knowledge in the field of chromatographic separation and electromigration analytical techniques for the design of the working conditions for the solution of individual separation problems and their systematic optimization is emphasised.
Graduate of the course is able to design the optimal separation conditions for the analysis of specific samples.
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Prerequisites
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Course of Analytical separation methods.
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Assessment methods and criteria
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Home assignment evaluation
Seminar project, written examination.
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Recommended literature
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Churáček J. a kol. Analytická separace látek, 1990, SNTL Praha..
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Churáček J. a kol. Nové trendy v teorii a instrumentaci vybraných analytických metod. Praha, 1993.
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Schoenmakers P.J. Optimization of Chromatographic Selectivity, 1986, Elsevier, Amsterdam.
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Snyder L. R. a kol. Practical HPLC method development. New York, 1997.
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