C7023 Separation Methods A

Faculty of Science
Autumn 2024
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).
In-person direct teaching
Teacher(s)
doc. Mgr. Jan Havliš, Dr. (lecturer)
Guaranteed by
doc. Mgr. Jan Havliš, Dr.
National Centre for Biomolecular Research – Faculty of Science
Supplier department: National Centre for Biomolecular Research – Faculty of Science
Prerequisites
basic knowledge of physical and analytical chemistry is prerequisited.
Course Enrolment Limitations
The course is offered to students of any study field.
Course objectives
the main objective of the course is to acquaint students with separation methods based on equilibrium separation between two phases.
Learning outcomes
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.
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
  • MEYER, Veronika R. Practical High-Performance Liquid Chromatography. 3rd ed. Chichester: J. Wiley & Sons, 1999, 338 pp. 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
Teaching methods
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.
Assessment methods
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.
Language of instruction
English
Follow-Up Courses
Further comments (probably available only in Czech)
Study Materials
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
Teacher's information
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
The course is also listed under the following terms Autumn 2010 - only for the accreditation, 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 2022, Autumn 2023.
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