C7023 Separation methods A

Přírodovědecká fakulta
podzim 2017
Rozsah
2/0/0. 2 kr. (plus ukončení). Doporučované ukončení: zk. Jiná možná ukončení: k.
Vyučující
doc. Mgr. Jan Havliš, Dr. (přednášející)
Garance
doc. Mgr. Jan Havliš, Dr.
Národní centrum pro výzkum biomolekul – Přírodovědecká fakulta
Dodavatelské pracoviště: Národní centrum pro výzkum biomolekul – Přírodovědecká fakulta
Předpoklady
basic knowledge of physical and analytical chemistry is prerequisited.
Omezení zápisu do předmětu
Předmět je otevřen studentům libovolného oboru.
Cíle předmětu
main objective of the course is to acquaint students with separation methods based on equilibrium separation between two phases.
Výstupy z učení
at the end of the course students should be able:
to manage general principles of analytical separation and its description to manage principles of equilibrium separation between two phases to describe and explain basic separation modes using following phase systems - liquid-liquid, solid-liquid, solid-gas, liquid-gas to describe and explain principles and practical spects of liquid and gas chromatography.
Osnova
  • 1. introduction to separation: separation of two ideally miscible compounds, separation limits, separation methods classification – preparative, analytical, basic principles of separation – molecular equilibrium, intermolecular interactions, entropy.
  • 2. extraction: description of extraction equilibria in system liquid-liquid and in system liquid-solid; choice of extraction system, carry-out of extraction, influence of analyte-solvent interaction, repeated extraction
  • 3. preanalytical sample preparation: CCE (counter-current extraction), SFE (supercritical fluid extraction); ASE (accelerated solvent extraction); MAE (microwave assisted extraction), SPE (solid phase extraction); SPME (solid phase microextraction), HSE (head-space extraction)
  • 4. analytical separation: chromatography, basic techniques (frontal, displacement, elution), theoretical principles – column equilibrium, physico-chemical description of processes on LC, kinetic and thermodynamic aspects of separation.
  • 5. study and description of separation; quantitative relations between structure and selectivity in regard to retention; liquid chromatography (LC) – history, theoretical ground; classification of basic separation mechanisms in LC (LLC, LSC, IEC), LC arrangement: mobile phase delivery, elution and elution force (isocratic and gradient); injection devices; separation column, types of stationary phases (particle, monolithic, on-chip), overview of sorbents;
  • 6. detectors photometric (DAD), refractometric, fluorescence, amperometric, conductivity, light-scattering, mass spectrometric, derivatisation and sample collection. description and evaluation of separation results: defining the chromatographic system, analytical information in chromatogram (qualitative, quantitative); precision, accuracy, limits of analysis (MDL, LOD, LOQ); evaluation of separation efficiency, testing of the system and its “good” behaviour;
  • 7. basic LC modes: CCC (counter-current chromatography), NP-HPLC (normal phase liquid chromatography), RP-HPLC (reverse phase liquid chromatography), TLC (thin-layer chromatography, HPTLC 2D TLC), ultra-high performance chromatography, high temperature liquid chromatography, elevated-temperature ultra-high performance chromatography, hydrophilic interaction chromatography (HILIC), ERLIC, hydrophobic interaction chromatography (HIC),
  • 8. IEC (ion exchange chromatography) – principles and carry-out, IXC (ion exclusion chromatography), chromatofocusation; affinity chromatography – principles, IMAC (immobilised-metal affinity chromatography); SFC (supercritical fluid chromatography); PC (perfusion chromatography);
  • 9. multi-dimensional chromatography: interface and principles; hyphenated separation techniques; preparative chromatography: methods (system scale-up, system overloading), fraction collection,
  • 10. gas chromatography (GC): history, differences between LC and GC (isotherms, gas compressibility, retention quantities), GC arrangement, mobile phase delivery; injection device (split, splitless); separation column, stationary phase types (WCOT, FSOT, SCOT, PLOT), column thermostat, detectors (flame ionisation, chemiluminescence, mass spectrometric detectors, etc.), GC system definition, GC evaluation and testing.
Literatura
  • MEYER, Veronika R. Practical High-Performance Liquid Chromatography. 3. vyd. Chichester: J. Wiley & Sons, 1999, 338 s. ISBN 0-471-98372-1. info
  • A practical approach to chiral separations by liquid chromatography. Edited by Ganapathy Subramanian. Weinheim: VCH Verlagsgesellschaft, 1994, 405 s. ISBN 3-527-28288-2. info
Výukové metody
the lecture is based on ppt presentation and its explication. presentation it-self will be available as a study material (black-and-white printable pdf with high resolution and restricted access rights). it is recommended to attend the lecture, because of the explication, which significantly extends the presentation and because of limited availability of textbooks in english covering certain parts of the subject. Subject will be eventually lectured if the number of enrolled students exceeds number 5, otherwise students will be given the chance to pass the subject combining study materials and tuition.
Metody hodnocení
written examination; students are required to understand and be familiar with the principles and their applications. examination consists of three basic questions.
Vyučovací jazyk
Angličtina
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Předmět je zařazen také v obdobích podzim 2010 - akreditace, podzim 2008, podzim 2009, podzim 2010, podzim 2011, podzim 2011 - akreditace, podzim 2012, podzim 2013, podzim 2014, podzim 2015, podzim 2016, podzim 2018, podzim 2019, podzim 2020, podzim 2021, podzim 2022, podzim 2023, podzim 2024.