C5440 Separation Methods

Faculty of Science
Autumn 2022
Extent and Intensity
1/0/0. 1 credit(s) (fasci plus compl plus > 4). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
Teacher(s)
doc. RNDr. Ctibor Mazal, CSc. (lecturer)
Guaranteed by
doc. RNDr. Ctibor Mazal, CSc.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science
Timetable
Tue 13:00–13:50 A08/309
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
Main objectives can be summarized as follows: Fundamentals and practice of basic separation methods used in organic chemistry (crystallization, distillation, sublimation, extraction, etc.) with focus on chromatographic methods; membrane separation processes and electromigration methods are mentioned as well.
Learning outcomes
After accomplishing the course students will be able:
- to understand and explain principles of the separation methods frequently used in organic chemistry in particular (e.g. GC, LC, HPLC, TLC and their modifications, crystallization, distillation, sublimation, extraction and electromigration methods);
- to choose appropriate separation method for solution of common analytical or preparative problems;
- to apply the knowledge obtained for setting basic parameters of the mentioned methods for development of simple procedures for sample separation.
Syllabus
  • 1. Chromatography. Introduction, general theory and concepts. Main theoretical models. Retention equation, plate theory and kinetic theory. Elution ratio and resolution.
  • 2. Gas chromatography. Van Deemter equation. GC techniques, block scheme of GC instruments. Carrier gas, sample injection, chomatographic columns, stationary phase. Enantioselective GC.
  • 3. Main methods of GC detection. Flame Ionization Detector (FID), Thermal conductivity detector (TCD), Electron Capture Detector (ECD), GC-MS coupling.
  • 4. Gas chromatography. Qualitative analysis, information from elution data, retention indexes (Kovats etc.). Selective detection. Quantitative analysis, calibration methods.
  • 5. Liquid chromatography. Basic principles. Column chromatography, flash chromatography - main techniques, column preparation, detection, stationary phases. Planar chromatography - paper chromatography and TLC.
  • 6. High performance liquid chromatography (HPLC). Block scheme of HPLC instrument. Mobile phase, pumps, degassing, gradient elution. Sample injection, HPLC columns, stationary phases. Enantioselective HPLC. HPLC detection - UV-Vis and fluorescence detectors, refractive index detector, evaporative light scattering detector. Chiroptical detection.
  • 7. Ion exchange, gel permeation (size exclusion) and affinity chromatography. Ionexchangers and ion equilibria in IEC. Stationary phases and retention in SEC (GPC). Basic principles of affinity chromatography.
  • 8. Sample preparation in chromatographic analysis. Derivatisation methods.
  • 9. Extraction. Countercurrent extraction. Supercritical fluid extraction. MW assisted extraction.
  • 10. Distillation. Basic principles. Rectification. Plate theory, distillation columns. Vacuum distillation, molecular distillation. Steam distillation, azeotropic and extractive distillation.
  • 11. Crystallisation. Crystallisation from solution - nucleation and crystal growth. Crystallisation from melt. Resolution by means of crystallisation.
  • 12. Sublimation. Sublimation techniques - gradient sublimation, lyophylization.
  • 13. Electromigration separation methods. Basic principles, ion mobility, transport processes. Tiselius electrophoresis. Capillary electrophoresis. Isotachophoresis. SDS-PAGE.
  • 14. Membrane permeation separation. Dialysis. Osmosis. Reverse osmosis and ultrafiltration.
Literature
  • SOJÁK, Ladislav. Separačné metódy v organickej chémii. 1. vyd. Bratislava: Univerzita Komenského, 1985, 240 s. info
  • CHURÁČEK, Jaroslav. Analytická separace látek. 1. vyd. Praha: Státní nakladatelství technické literatury, 1990, 384 s. ISBN 80-03-00569-8. info
  • POOLE, Colin F. and Salwa K. POOLE. Chromatography today. Amsterdam: Elsevier, 1991, 1026 s. ISBN 0-444-89161-7. info
  • Kolektiv., Moderní separační metody, ČSAV Praha 1988.
Teaching methods
Lectures
Assessment methods
Oral exam
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.
The course is also listed under the following terms Autumn 2007 - for the purpose of the accreditation, Autumn 1999, Autumn 2010 - only for the accreditation, Autumn 2000, Autumn 2001, Autumn 2002, Autumn 2003, Autumn 2004, Autumn 2005, Autumn 2006, Autumn 2007, Autumn 2008, Autumn 2009, Autumn 2010, Autumn 2011, Autumn 2011 - acreditation, Autumn 2012, Autumn 2013, Autumn 2014, Autumn 2015, Autumn 2016, autumn 2017, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2023, Autumn 2024.
  • Enrolment Statistics (Autumn 2022, recent)
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