C7021 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
Contact Person: doc. Mgr. Jan Havliš, Dr.
Supplier department: National Centre for Biomolecular Research – Faculty of Science
Timetable
Tue 13:00–14:50 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
the main objective of the course is to acquaint students with separation methods based on equilibrium separation between two phases.
another objective of the course is to provide this knowledge in english in order to improve students' language skills
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
  • 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. presentations themselves will be available in both, czech & english, 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, and because there are no available textbooks in czech language covering certain parts of the subject.
at the beginning of the course, students will be supplemented in the study materials section with the document containing voluntary running tasks to consolidate the acquired knowledge.
Assessment methods
the examination consists of max 30 min written test of basic knowledge and of an oral examination. the examination will be conducted in czech, eventually, when agreed, in english; 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
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 2016, autumn 2017, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2022, Autumn 2023.
  • Enrolment Statistics (recent)
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