C7021 Separation Methods A

Faculty of Science
Autumn 2007 - for the purpose of the accreditation
Extent and Intensity
2/0/0. 2 credit(s) (fasci plus compl plus > 4). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
Teacher(s)
doc. Mgr. Jan Havliš, Dr. (lecturer)
doc. RNDr. Bc. Jiří Pazourek, Ph.D. (lecturer)
Guaranteed by
doc. RNDr. Bc. Jiří Pazourek, Ph.D.
Department of Chemistry – Chemistry Section – Faculty of Science
Prerequisites
C3100 + C4050 Analytical chemistry (at least C1660)
Course Enrolment Limitations
The course is also offered to the students of the fields other than those the course is directly associated with.
fields of study / plans the course is directly associated with
there are 11 fields of study the course is directly associated with, display
Course objectives
Basics of analytical separation methods, transit from liquid-liquid extraction to chromatography. Efficiency of separation methods. Sample preparation for analytical separation. Theory and praxis of Liquid Chromatography (LC). Ion exchange chromatography (IEC) and other variants of LC (SFC, HILIC, etc). Chiral separations. Separation of macromolecules (GPC, HDC, FFF).
Syllabus
  • 1. introduction; 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
  • 2. preanalytical sample preparation: SFE (supercritical fluid extraction); ASE (accelerated solvent extraction); MAE (microwave assisted extraction), TLC (thin-layer chromatography, HPTLC 2D TLC),
  • 3. SPE (solid phase extraction); SPME (solid phase microextraction), HSE (head-space extraction)
  • analytical separation; liquid chromatography (LC) – history, theoretical ground; classification of basic separation mechanisms in LC (liquid-liquid chromatography, LLC, liquid-solid chromatography, LSC, ion chromatography, IC, gel permeation chromatography, GPC),
  • 4. physico-chemical description of LC processes, mass transfer in LC, thermodynamic aspects of separation; kinetic aspects of separation,
  • 5. 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 (diode array detectors, refractometric, fluorescence, amperometric, conductivity, light-scattering, mass spectrometric) 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;
  • basic LC modes: NP-HPLC (normal phase liquid chromatography), RP-HPLC (reverse phase liquid chromatography), ultra-high performance chromatography, high temperature liquid chromatography, elevated-temperature ultra-high performance chromatography,
  • 7. hydrophilic interaction chromatography (HILIC), hydrophobic interaction chromatography (HIC) IEC (ion exchange chromatography) – principles and carry-out, chromatofocusation,
  • 8. affinity chromatography – principles, IMAC (immobilised-metal affinity chromatography); SFC (supercritical fluid chromatography); PC (perfusion chromatography), preparative chromatography – principles and carry-out
  • 9. development of chromatographic method, criteria and optimisation of separation system;
  • study and description of separation; quantitative relations between structure and selectivity in regard to retention;
  • 10. chiral separation: definition of chirality; optical rotation dispersity; chiral selectors and their application in separation methods (HPLC)
  • 11. validation of analytical separation method; why and how, elemental terms –method identity, method precision, calibration, selectivity, robustness
Literature
  • CHURÁČEK, Jaroslav. Analytická separace látek. 1. vyd. Praha: Státní nakladatelství technické literatury, 1990, 384 s. ISBN 80-03-00569-8. info
  • POPL, Milan and Jaroslav KUBÁT. Separace látek. 3. přeprac. vyd. Praha: Vysoká škola chemicko-technologická, 1986, 171 s. info
  • SOMMER, Lumír. Základy teorie analytické chemie. 1. vyd. Praha: Státní pedagogické nakladatelství, 1985, 250 s. info
  • SOMMER, Lumír. Základy teorie analytické chemie. 1. vyd. Praha: Státní pedagogické nakladatelství, 1990, 138 s. ISBN 8021001070. info
  • SOMMER, Lumír. Základy teorie analytické chemie. 1. vyd. Praha: Státní pedagogické nakladatelství, 1991, 185 s. ISBN 8021002158. info
  • Separační metody - Plynová chromatografie
Assessment methods (in Czech)
výuka: přednáška + její verze v PDF (viz. studní materiály); závěrečné hodnocení: ústní zkouška
Language of instruction
Czech
Follow-Up Courses
Further Comments
The course can also be completed outside the examination period.
The course is taught annually.
The course is taught: every week.
Listed among pre-requisites of other courses
The course is also listed under the following terms Autumn 1999, Autumn 2000, Autumn 2001, Autumn 2002, Autumn 2003, Autumn 2004, Autumn 2005, Autumn 2006, Autumn 2007, Autumn 2012, Autumn 2013, Autumn 2014, Autumn 2015, Autumn 2016, autumn 2017, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2022, Autumn 2023, Autumn 2024.