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Course, academic year 2023/2024
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Electroanalytical Methods - MC230P03N
Title: Elektrochemické metody
Czech title: Elektrochemické metody
Guaranteed by: Department of Analytical Chemistry (31-230)
Faculty: Faculty of Science
Actual: from 2016 to 2023
Semester: summer
E-Credits: 3
Examination process: summer s.:
Hours per week, examination: summer s.:3/0, Ex [HT]
Capacity: unlimited
Min. number of students: unlimited
4EU+: no
Virtual mobility / capacity: no
State of the course: taught
Language: Czech
Note: enabled for web enrollment
Guarantor: prof. RNDr. Vlastimil Vyskočil, Ph.D.
Teacher(s): doc. RNDr. Karolina Schwarzová, Ph.D.
prof. RNDr. Vlastimil Vyskočil, Ph.D.
Annotation -
Basic principles of electroanalytical methods and their classification. Theoretical background and systematic, critical description of the most important methods, i.e., equilibrium (potentiometry), steady-state (polarography, voltammetry, coulometry), non-steady state voltammetry, bulk solution measurements (conductometry, impedance measurements), flow detection and continuous monitoring, combinations of electrochemical measurements with high-performance separations and with other physico-chemical techniques (spectroscopy). Typical examples of applications.

Learning Outcomes:
Upon completion of the course, the student will:
1. Describe the term electroanalytical chemistry, describe the structure of the electrode/electrolyte interphase, explain the electrode potential, describe the electrochemical cell and explain the passage of electric current through the cell, describe the effect of transport on the electrode process, describe the importance of the redox potential.
2. Explain the technique of equilibrium potentiometry, describe the main types of electrodes used in potentiometry, explain the principle of ion selective electrodes and describe their use, explain the selectivity coefficient, explain the principle of pH measurement using a glass electrode, explain the basic principles of potentiometric biosensors, explain the use of indirect potentiometry.
3. Explain the technique of conductometry, explain the term conductivity, describe the principle of conductivity measurement, describe the instrumentation used in conductometry, explain the use of indirect conductometry, explain the technique of dielectrometry and its application.
4. Explain the technique of polarography and describe the main points of its discovery and development, describe the polarograph and the mercury drop electrode, explain the types of electric currents in polarography, describe the static mercury drop electrode and variations of modern polarographic techniques.
5. Explain the technique of voltammetry, describe the electrode materials used, compare electrode surface restoration options, describe the rotating disk and ring electrode and explain the theoretical description of the transport of a substance to the electrode, describe the different types of microelectrodes and explain the theoretical description of the transport of a substance to the microelectrode.
6. Explain the technique of amperometry, describe the working parameters of amperometric detectors, explain the theoretical description of the transport of a substance to an electrode, describe the different types of amperometric sensors and detectors, explain the basic principles of amperometric biosensors.
7. Explain the techniques of electrogravimetry and coulometry, compare their common and different features, describe the geometric arrangement of the cell, compare the performance of constant potential and constant current techniques, describe the different types of coulometric analyzers.
8. Explain the principle of titrations with polarizable electrodes, explain the techniques of amperometric titration and biamperometric titration, describe the determination of water according to Karl Fischer, explain the techniques of potentiometric and bipotentiometric titration.
9. Explain non-stationary voltammetric techniques, describe the principle of chronoamperometry, linear and cyclic voltammetry, pulse voltammetric techniques and electrochemical dissolution analysis.
Last update: Vyskočil Vlastimil, prof. RNDr., Ph.D. (12.02.2024)
Literature -

K. Štulík, J. Barek: Elektrochemické analytické metody, SPN Praha, 1985 (skriptum).
Z. Samec: Elektrochemie, UK, Karolinum, Praha 1999 (skriptum).

Last update: Nesměrák Karel, doc. RNDr., Ph.D. (28.10.2019)
Requirements to the exam -

The course is concluded with an oral examination (with written preparation) with questions on the topics covered throughout the course.

Last update: Vyskočil Vlastimil, prof. RNDr., Ph.D. (06.09.2023)
Syllabus -

1) Introduction: basic principles of electroanalytical methods and their classification.

2) Theoretical background: basic terms, electrochemical properties of solutions, mechanism and rate of electrochemical processes (charge transfer reaction, transport mechanisms, homogeneous and heterogeneous chemical reactions coupled with electrode reactions, adsorption of compounds from solution or produced by electrochemical reaction on the electrode surface).

3) Equilibrium potentiometry: galvanic cell, electrodes, ion-selective electrodes, pH measurement, potentiometric gas sensors. Indirect potentiometry - potentiometric titrations.

4) Polarography: classical polarography, types of polarographic currents, diagnostic criteria, various kinds of mercurial electrodes, analytical applications.

5) Modern polarographic and voltammetric methods: tast polarography, normal pulse and differential pulse polarography, anodic stripping analysis, adsorption stripping analysis.

6) Non-stationary methods: DC voltammetry, cyclic voltammetry.

7) Voltammetry with solid electrodes: properties of electrodes from solid materials, typical polarization curves, electrode history elimination, rotating disk electrode, rotating ring-disk electrode. Microelectrodes and their arrays.

8) Conductometry: low-frequency conductometry, two- and four-electrodes conductometric cells, contactless conductometry, high-frequency conductometry and dielectrometry.

9) Electrochemical methods in flowing systems.

10) Methods based on exhausting electrolysis: potentiostatic coulometry, galvanostatic coulometry, coulometric titrations, coulometry in flowing systems, thin-layer coulometry.

11) Titrations with polarizable electrodes: amperometric titrations, biamperometric titrations, bipotentiometric titrations, potentiometric titrations with one polarizable electrode.

Last update: Vyskočil Vlastimil, prof. RNDr., Ph.D. (03.04.2018)
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