PřF:C8102 Special methods - laboratory - Course Information

C8102 Special methods - laboratory

Extent and Intensity

0/0/5. 5 credit(s) (plus extra credits for completion). Type of Completion: z (credit).
In-person direct teaching

Teacher(s)

doc. Mgr. Karel Novotný, Ph.D. (seminar tutor)
Mgr. Aleš Hrdlička, Ph.D. (seminar tutor)
doc. Mgr. Tomáš Vaculovič, Ph.D. (seminar tutor)
RNDr. Marta Farková, CSc. (seminar tutor)
Mgr. Miroslava Bittová, Ph.D. (seminar tutor)
prof. RNDr. Jiří Urban, Ph.D. (seminar tutor)
prof. Mgr. Jan Preisler, Ph.D. (seminar tutor)
Mgr. Lucie Šimoníková (seminar tutor)
Mgr. Antonín Bednařík, Ph.D. (seminar tutor)
RNDr. Mgr. Iveta Třísková, Ph.D. (seminar tutor)

Guaranteed by

doc. Mgr. Karel Novotný, Ph.D.
Department of Chemistry – Chemistry Section – Faculty of Science
Contact Person: doc. Mgr. Karel Novotný, Ph.D.
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science

Prerequisites

Following lectures is appropriate attend before or during exercise: C7021 Separation Methods A, C7031 Analytical Atomic Spectrometry, C7041 Molecular Spectrometry, C7050 Electroanalytical Methods, C7830 Capillary Electrophoresis and C7895 Mass Spectrometry of Biomolecules.

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 9 fields of study the course is directly associated with, display

Abstract

Main objectives can be summarized as practice training in electroanalytical methods, optical spectroscopy, mass spectroscopy, and separation methods. A) Modern electroanalytical methods, potenciometry with ion selective electrode, elimination and stripping voltammetry. B) atomic emission spectrometry with inductively coupled plasma (ICP-OES/MS), laser spectrometry (LA-ICP-OES/MS, LIBS). C) Isotachophoresis, high performance liquid chromatography (HPLC), capillary chromatography on monolithic stationary phases, capillary zone electrophoresis, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS).

Learning outcomes

Obtaining theoretical knowledge and practical skills in selected analytical methods. Students get to know with hi-tech instrumentation used for research and development of advanced analytical techniques.

Key topics

A) Introduction to laboratory exercises: electroanalytical methods, spectroscopy, separation methods. B) ELECTROANALYTICAL METHODS BLOCK: 1. Determination of nitrates by ion-selective electrode in the presence of an interfering ion. Using the Nikolsky relation by the method of separate solutions and the method of constant interferent concentration, determination of the selectivity constant of the interfering ion. 2. Analytical use of the new electrochemical method of elimination voltammetry (EVLS) in conjunction with adsorptive stripping - separation of potential-close signals (reduction and oxidation of selected depolarizers are monitored on different electrodes). C) SPECTRAL METHODS BLOCK 3. ICP OES/MS spectrometry. Sample decomposition methods: cryogenic grinding, microwave decomposition. Solution analysis using ICP OES and ICP MS spectrometry. 4.Analytical methods based on laser ablation (LA-ICP-MS), laser-excited plasma spectrometry (LIBS): surface mapping D) SEPARATION METHODS BLOCK 5. Determination of anions in water by chronopotentiometry and ITP method 6. Liquid chromatography. HPLC - Determination of the content of inosine, adenosine and their 2’-deoxy-forms in a model mixture - optimization and validation of the method. 7. Liquid chromatography coupled with mass detection (LC-MS). Analysis of white wine: determination of organic acids. 8. CE-LIF, capillary zone electrophoresis with laser-induced fluorescence detection. Optimization of the experimental setup. Determination of the detection limit of rhodamine 6G. Separation of rhodamine dyes. 9. Mass spectrometry of proteins and peptides using matrix-assisted laser desorption/ionization (MALDI MS). Selected applications of MALDI MS: instrument calibration, molecular weight determination, enzymatic digestion, peptide mapping, identification of unknown protein.

Study resources and literature

recommended literature
• SKOOG, Douglas A.; Donald M. WEST; F. James HOLLER and Stanley R. CROUCH. Analytická chemie. Translated by Karel Nesměrák - Václav Červený - Tomáš Křížek - Eliška. Vydání první. Praha: Vysoká škola chemicko-technologická v Praze, 2019, xxx, 950. ISBN 9788075920430. info
• SOMMER, Lumír. Analytická spektrometrie. 1. vyd. Praha: Státní pedagogické nakladatelství, 1986, 173 s. info
• KORYTA, Jiří. Současné trendy v elektrochemii. 1. vyd. Praha: Academia, 1986, 128 s. info
• Analytická příručka. Edited by Jaroslav Zýka. 4., upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988, 831 s. info
• CHURÁČEK, Jaroslav and Pavel JANDERA. Separace látek : kapalinová vysokoúčinná kolonová chromatografie. 1. vyd. Praha: SNTL - Nakladatelství technické literatury, 1981, 140 s. info
• CHURÁČEK, Jaroslav. Úvod do vysokoúčinné kapalinové kolonové chromatograrie. Edited by Pavel Jandera. Vyd. 1. Praha: SNTL - Nakladatelství technické literatury, 1984, 188 s. info
• CHURÁČEK, Jaroslav. Nové trendy v teorii a instrumentaci vybraných analytických metod. Vyd. 1. Praha: Academia, 1993, 387 s. ISBN 8020000100. info
• SOMMER, Lumír. Analytical absorption spectrophotometry in the visible and ultraviolet : the principles. Amsterdam: Elsevier, 1989, 310 s. ISBN 0-444-98882-38. info
• KANICKÝ, Viktor; Vítězslav OTRUBA; Lumír SOMMER and Jiří TOMAN. Optická emisní spektrometrie v indukčně vázaném plazmatu a vysokoteplotních plamenech (Optical emission spectrometry in inductiveky coupled plasma and high temperature flames). 1. st. Praha: Academia, 1992, 152 pp. Pokroky chemie 24. ISBN 80-200-0215-4. info
• Analytická příručka. Díl I [Zýka, 1988]. Edited by Jaroslav Zýka. 4. upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988, 678 s. info
• BARTUŠEK, Miloš. Úvod do elektroanalytických metod. 1. vyd. Praha: SPN, 1984, 104 s. : i. info
• DVOŘÁK, Jiří and Jiří KORYTA. Elektrochemie. 3., dopl. a rozš. vyd. Praha: Academia, 1983, 410 s. URL info
• Nové směry v analytické chemii. Edited by Jaroslav Zýka. 1. vyd. Praha: Státní nakladatelství technické literatury, 1983, 199 s. info
• HOLZBECHER, Záviš and Jaroslav CHURÁČEK. Analytická chemie. 1. vyd. Praha: Státní nakladatelství technické literatury, 1987, 663 s. info
• SOMMER, Lumír. Teorie a praxe vybraných optických analytických metod. 1. vyd. Praha: Státní pedagogické nakladatelství, 1978, 285 s. info
• CHURÁČEK, Jaroslav. Analytická separace látek. 1. vyd. Praha: Státní nakladatelství technické literatury, 1990, 384 s. ISBN 80-03-00569-8. info

Approaches, practices, and methods used in teaching

laboratory courses

Method of verifying learning outcomes and course completion requirements

Laboratory exercises take place in three closed cycles: electroanalytical methods, optical methods LIBS, ICP-OES (+LA-ICP MS), separation methods (+MALDI-MSTOF). Tasks are usually performed after individual agreement with the teacher. Credit is awarded after completing all tasks and submitting the protocol and its approval by the teacher who leads the task.

Language of instruction

Czech

Further comments (probably available only in Czech)

Study Materials
The course is taught annually.
The course is taught in blocks.
General note: dle oboru.

Teacher's information

Preparation for the special exercise: Each exercise will begin with a written test or interview. Guarantors of individual blocks: electroanalytical part: RNDr. Třísková, optical part: Doc. Novotný, Dr. Hrdlička, separation part: Prof. Urban Dr. Bittová, MS part: Dr. Bednařík, Prof. Preisler. Criteria for completing the tasks of the special exercise: Theoretical preparation for the exercise (test, interview). Experimental skill and diligence, order and cleanliness at work, proper records in the work diary, high-quality and timely preparation of the protocol, compliance with the deadline for submitting and correcting the protocol, correct experimental results. Required knowledge: master the theory of the given method and study the practical implementation of the task according to the instructions. Electroanalytical part - knowledge of basic physical concepts: electrical quantities and their units, connection of measuring instruments (A, V) to a circuit, Kirchhoff's laws, Ohm's law, voltage divider. Knowledge of basic concepts of electrochemistry: electrode potential, decomposition voltage, terminal voltage, electromotive voltage, types of overvoltage in electrode processes, electrode processes on the cathode and anode of various materials (Pt, Cu) and in various electrolytes (H2SO4, Na2SO4, CuSO4), polarization curves, depolarizer, polarizable and ideally non-polarizable electrode, Nernst equation, Nikolsky equation, Henderson equation, Faraday's law. Spectroscopic part (including mass spectrometry): Instrumentation: monochromator, polychromator, excitation sources in emission spectroscopy, radiation sources in absorption spectroscopy, dispersive elements, detectors. Terms: spectral line, emission and absorption transitions, plasma temperature, electron concentration, singlet, doublet, triplet, resonance spectral line, self-absorption, Boltzmann's law, Sah's equation, Planck's law, Bouguert-Lambert-Beer's law, absorption, emission, fluorescence (atomic and molecular processes). Laser desorption/ionization mass spectrometry: laser principle, mass spectrometry principle, various types of spectrometers, interaction of laser beam with sample and matrix. Separation part: HPLC: retention time, dead time, reduced retention time, zone width at half height, zone width at base, zone height, resolution, capacity ratio, retention ratio, theoretical plate (number of theoretical plates, theoretical plate height, number of effective plates, theoretical plate height equivalent, reduced T.P. height equivalent), gradient elution, isocratic. Isotachophoresis: electrophoretic mobility, electric field intensity, speed of movement of a charged particle in an electric field, buffer solutions, basic electrolytes, electrokinetic sampling, electroosmotic flow.

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