C7023 Separation methods A

Přírodovědecká fakulta
podzim 2023
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
the 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 the following phase systems - liquid-liquid, solid-liquid, solid-gas, liquid-gas
to describe and explain principles and practical aspects 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. presentations themselves will be available as study materials (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.
the subject is usually practically merged with subject C7021 to be lectured together. the C7021 is originally for czech students, but taught in english and examined in czech. students of C7023 will benefit from the lecturing in english, and then they will be, of course, examined in english.
at the beginning of the course, the document containing voluntary running tasks to consolidate the acquired knowledge will be uploaded to the study materials section.
Metody hodnocení
the examination consists of max 30 min written test of basic knowledge and of an oral examination. students are required to understand and to be familiar with the principles and their applications. the oral examination consists of three basic questions, which would be during the examination expanded to let the student demonstrate the extent of topic understanding.
Vyučovací jazyk
Angličtina
Navazující předměty
Informace učitele
the lecture is going to be merged with subject C7021 and taught in the same time slot - every tuesday 11:00-12:50 in C14-207
Další komentáře
Předmět je dovoleno ukončit i mimo zkouškové období.
Předmět je vyučován každoročně.
Výuka probíhá každý týden.
Nachází se v prerekvizitách jiných předmětů
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 2017, podzim 2018, podzim 2019, podzim 2020, podzim 2021, podzim 2022, podzim 2024.