C7021 Separation Methods A

Faculty of Science
Autumn 2016
Extent and Intensity
2/0/0. 2 credit(s) (plus extra credits for completion). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
Teacher(s)
doc. Mgr. Jan Havliš, Dr. (lecturer)
Mgr. Pavla Pospíšilová (lecturer)
Guaranteed by
doc. Mgr. Jan Havliš, Dr.
National Centre for Biomolecular Research – Faculty of Science
Contact Person: doc. Mgr. Jan Havliš, Dr.
Supplier department: National Centre for Biomolecular Research – Faculty of Science
Timetable
Mon 19. 9. to Sun 18. 12. Tue 14:00–15:50 C14/207
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
Course objectives
Basics of analytical separation methods, transit from liquid-liquid and liquid-solid 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. Validation of separation methods.
Syllabus
  • 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.
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
Teaching methods
The lecture is based on ppt presentation and its explication. Presentation itself 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 there are no available textbooks in Czech language covering certain parts of the subject.
Assessment methods
oral examination; students are required to understand and to be familiar with the principles and their applications. examination consists of three basic questions, which would be during the examination expanded to let the student demonstrate the extent of topic understanding.
Language of instruction
Czech
Follow-Up Courses
Further Comments
Study Materials
The course can also be completed outside the examination period.
The course is taught annually.
Listed among pre-requisites of other courses
The course is also listed under the following terms Autumn 2007 - for the purpose of the accreditation, 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 2017, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2022, Autumn 2023, Autumn 2024.
  • Enrolment Statistics (Autumn 2016, recent)
  • Permalink: https://is.muni.cz/course/sci/autumn2016/C7021