PřF:C7021 Separation Methods A - Course Information

C7021 Separation Methods A

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)

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 15:00–16:50 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

• Analytical Chemistry (programme PřF, N-CH)

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; 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
• 2. preanalytical sample preparation: SFE (supercritical fluid extraction); ASE (accelerated solvent extraction); MAE (microwave assisted extraction), TLC (thin-layer chromatography, HPTLC 2D TLC),
• 3. SPE (solid phase extraction); SPME (solid phase microextraction), HSE (head-space extraction)
• analytical separation; liquid chromatography (LC) – history, theoretical ground; classification of basic separation mechanisms in LC (liquid-liquid chromatography, LLC, liquid-solid chromatography, LSC, ion chromatography, IC, gel permeation chromatography, GPC),
• 4. physico-chemical description of LC processes, mass transfer in LC, thermodynamic aspects of separation; kinetic aspects of separation,
• 5. 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 (diode array detectors, refractometric, fluorescence, amperometric, conductivity, light-scattering, mass spectrometric) 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;
• basic LC modes: NP-HPLC (normal phase liquid chromatography), RP-HPLC (reverse phase liquid chromatography), ultra-high performance chromatography, high temperature liquid chromatography, elevated-temperature ultra-high performance chromatography,
• 7. hydrophilic interaction chromatography (HILIC), hydrophobic interaction chromatography (HIC) IEC (ion exchange chromatography) – principles and carry-out, chromatofocusation,
• 8. affinity chromatography – principles, IMAC (immobilised-metal affinity chromatography); SFC (supercritical fluid chromatography); PC (perfusion chromatography), preparative chromatography – principles and carry-out
• 9. development of chromatographic method, criteria and optimisation of separation system;
• study and description of separation; quantitative relations between structure and selectivity with regard to retention;
• 10. chiral separation: definition of chirality; optical rotation dispersity; chiral selectors and their application in separation methods (HPLC)
• 11. validation of analytical separation method; why and how, elemental terms –method identity, method precision, calibration, selectivity, robustness

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

• C8022 Separation Methods B

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

• C8022 Separation Methods B
  C7021  

• Enrolment Statistics (Autumn 2013, recent)
  
• Permalink: https://is.muni.cz/course/sci/autumn2013/C7021