C5440 Separation Methods

Faculty of Science
Autumn 2019
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
Wed 9:00–9:50 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
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 2020, autumn 2021, Autumn 2022, Autumn 2023, Autumn 2024.
  • Enrolment Statistics (Autumn 2019, recent)
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