PřF:C7050 Electroanalytical Methods - Course Information

C7050 Electroanalytical Methods

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)

prof. RNDr. Jan Hrbáč, Ph.D. (lecturer)
prof. RNDr. Přemysl Lubal, Ph.D. (lecturer)

Guaranteed by

prof. RNDr. Přemysl Lubal, Ph.D.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science

Timetable

Thu 8:00–9:50 C14/207

Prerequisites

Principles of analytical and physical chemistry in subjects C4050 Analytical Chemistry II, C4020 Physical Chemistry II, C4660 Physical Chemistry I, C5160 Physical Chemistry - laboratory course.

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-CHE)
• Physical Chemistry (programme PřF, N-CHE)

Course objectives

The aim of the course is to give students the overview of electroanalytical methods with the possibilities of their use in analytical practice. In addition to the classification of methods (conductivity, potentiometry, electrogravimetry, coulometry, voltammetric and amperometric methods), the importance is expressed to the explanation of the physico-chemical principles of these methods and their application in chemical analysis. Students will get the knowledge of the fundamentals of electroanalytical methods applicable in basic and applied research laboratories.

Learning outcomes

Students acquire theoretical and practical knowledge in electroanalytical methods.

Syllabus

• 1. Introduction - historical overview, literature. Basic concepts and quantities (charge, voltage, current, resistance and conductivity, capacitance, inductance). Electroactive molecule/particle, electrochemical potential, Nernst equation, cell voltage. Classification of electroanalytical methods.
  2. Conductometry and dielectrometry. Theory - (ion mobility, specific conductance, molar conductivity of electrolyte, dissociation, Kohlrausch's law). Practical implementation - conductivity cell and its circuit. Application of conductometry (water quality monitoring, monitoring of reactions, conductometric titrations). High-frequency conductometry. Dielectrometry.
  3. Electroanalytical separation methods. Electrophoresis, isotachophoresis, isoelectric focusing. Theoretical basis, instrumentation.
  4. Potentiometry I. Theory - Galvanic cell, half-cell, electrode potential, Nernst equation, liquid junction potential, Donnan potential, cell voltage. Practical implementation – Indicator and reference half-cells (electrodes - I, II, III types). Measurement of cell voltage, pH- and pX-meters.
  5. Potentiometry II. Ion-selective electrodes - ISE. Definition and classification of ISE, membrane materials, construction of ISE, selectivity of ISE. Nikolsky-Eisenman equation, methods for determination of selectivity coefficient. Practical applications of ISE. Measurement of pH. Modern potentiometric sensors - "solid contact" ISE, ISFET, LAPS.
  6. Electrogravimetry and coulometry. Faraday's laws of electrolysis. Electrogravimetry - working and auxiliary electrodes, potenciostat, galvanostat, electrogravimetry at constant electric voltage or current, electrolytic separations, internal electrolysis. Coulometry - principle of the method, comparison of coulometry and electrogravimetry. Classification of coulometric methods according to working mode, determination of the number of transferred electrons, determination of the thickness of galvanic coatings. Coulometric titrations.
  7. Voltammetry and amperometry I. Theory - electrode bilayer, capacitive and Faraday current, Butler-Volmer and Tafel equations, semi-infinite linear diffusion, diffusion overvoltage and IR gradient. Cyclic voltammetry - three-electrode circuit, electrode materials and their potential window. Reversibility of the voltammogram - Randles-Shevchik and Delahaye equations. Basic mechanisms of cyclic voltammetry - EC notation. Amperometry - Cottrell equation.
  8. Voltammetry and amperometry II. Voltammetry with dropping mercury electrode - polarography, pulse and AC methods, tast-polarography, stripping analysis. Normal pulse voltammetry/polarography, differential pulse voltammetry/polarography, square wave voltammetry/polarography, AC voltammetry. Stripping analysis. Pulse amperometry.
  9. Voltammetry and amperometry III. Voltammetry with rotating disc electrode, hydrodynamic voltammogram, Levic equation, use of RDE in studying kinetics of electrochemical reactions etc. Voltammetry with microelectrodes - radial diffusion. Galvanostatic techniques - chronopotentiometry. Amperometric sensors with membrane (Clark electrode, biosensors, gas sensors).
  10. Impedance methods. Real and imaginary value of impedance, Nyquist and Bode diagrams, equivalent circuit of electrochemical vessel, electrochemical impedance spectrum (EIS), evaluation of impedance data.
  11. Combined techniques. Electrochemical detection in liquid chromatography and capillary electrophoresis, electrogenerated chemiluminescence, electrochemical microbalance (EQCM), scanning electrochemical microscopy, spectroelectrochemistry (UV-VIS, IR, Raman, EPR, MS), sonoelectrochemistry, bipolar electrochemistry.
  12. Application of electroanalytical methods in chemical research. Potentiometric titrations, titration curves and several ways of their evaluation. Use of electroanalytical methods for the determination of various physico-chemical parameters (e.g. equilibrium/rate constants, diffusion coefficient, etc.). Speciation analysis.

Literature

• Analytická příručka. Díl I [Zýka, 1988]. Edited by Jaroslav Zýka. 4. upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988, 678 s. info
• ČERMÁKOVÁ, Ludmila and Jaroslav ZÝKA. Analytická chemie méně běžných prvků. 1. vyd. Praha: Státní pedagogické nakladatelství, 1990, 176 s. ISBN 80-7066-050-3. info
• BRETT, Christopher M. A. and Ana Maria Oliviera BRETT. Electroanalysis. Oxford: Oxford University Press, 1998, 88 s. ISBN 0198548168. info
• BARD, Allen J. and Larry R. FAULKNER. Electrochemical methods : fundamentals and applications. 2nd ed. New York: John Wiley & Sons, 2001, xxi, 833. ISBN 0471043729. info
• Bard, A.J., Stratman, M. Encyclopedia of Electrochemistry, Instrumentation and Electroanalytical Chemistry, Vol.3, Wiley-VCH,2001
• WANG, Joseph. Analytical electrochemistry. 3rd ed. Hoboken, N.J.: Wiley-VCH, 2006, xvi, 250. ISBN 0471678791. info
• Electroanalytical methods : guide to experiments and applications. Edited by Fritz Scholz - A. M. Bond - R. G. Compton - Dirk A. Fiedler - György. Second, revised and extended. Heidelberg: Springer, 2010, xxvii, 359. ISBN 9783642425318. info
• JANATA, Jiří. Principles of chemical sensors. 2nd ed. Dordrecht: Springer, 2009, xv, 373. ISBN 9780387699301. info
• DVOŘÁK, Jiří and Jiří KORYTA. Elektrochemie. 3., dopl. a rozš. vyd. Praha: Academia, 1983, 410 s. URL info
• BAREK, Jiří, František OPEKAR and Karel ŠTULÍK. Elektroanalytická chemie. 1. vyd. Praha: Karolinum, 2005, 188 s. ISBN 8024611465. info
• Electromigration techniques : theory and practice. Edited by Boguslaw Buszewski - Ewelina Dziubakiewicz - Michal Szumski. Heidelberg: Springer, 2013, xxi, 357. ISBN 9783642350429. info

Teaching methods

Lecture. The emphasis is placed on physico-chemical principles of electroanalytical methods and their application in chemical analysis.

Assessment methods

Presentation, written and oral examination.

Language of instruction

Czech

Further Comments

Study Materials
The course can also be completed outside the examination period.
The course is taught annually.

• Enrolment Statistics (recent)
  
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