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Course, academic year 2023/2024
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Analytical chemistry II - MC230P68
Title: Analytická chemie II (a)
Czech title: Analytická chemie II (a)
Guaranteed by: Department of Analytical Chemistry (31-230)
Faculty: Faculty of Science
Actual: from 2021 to 2023
Semester: summer
E-Credits: 5
Examination process: summer s.:
Hours per week, examination: summer s.:3/2, C+Ex [HT]
Capacity: unlimited
Min. number of students: unlimited
4EU+: no
Virtual mobility / capacity: no
State of the course: taught
Language: Czech
Explanation: v roce 2020/21 výjimečně v obou semestrech (ZS 3. ročník, LS 2. ročník),od 2021/22 pouze v LS
Note: enabled for web enrollment
Guarantor: prof. RNDr. Vlastimil Vyskočil, Ph.D.
Teacher(s): RNDr. Jan Fischer, Ph.D.
doc. RNDr. Tomáš Křížek, Ph.D.
RNDr. Anna Kubíčková, Ph.D.
doc. RNDr. Karolina Schwarzová, Ph.D.
prof. RNDr. Vlastimil Vyskočil, Ph.D.
Incompatibility : MC230P02N
Is incompatible with: MC230P85
Is interchangeable with: MC230P02N
Annotation -
Calibration in instrumental methods. Electrochemical methods: methods based on measuring of potential (equilibrium potentiometry, potentiometric titrations), current (voltammetry and polarography, coulometry, electrogravimetry) and conductivity (conductometry and dielectrometry). Optical methods: methods without exchange of energy (refractometry,
polarimetry, nephelometry); absorption spectral methods (molecular absorption and atomic absorption spectroscopy); emission spectral methods (molecular fluorescence spectroscopy, atomic emission spectroscopy); analytical methods in flowing liquids with optical detection; spectral methods for determination of pollutants in the air. Chromatographic methods: column chromatography (gas and liquid), planar (thin-layer) chromatography. Electromigration methods.

In the scope of the Seminar training in basic calculations used in analytical chemistry (gravimetry; precipitation, complexation, acid-base and redox equilibria) is realized.

Learning Outcomes:
Upon completion of the course, the student will:
1. Explain electrodes, electrochemical cell, transport mechanisms, polarization curve. Describe electrodes: first and second species, membrane electrodes, redox electrodes. Describes the electrochemical cell: indicating (working) and reference electrodes, galvanic cell, electrolyzer, electrode polarization (concentration and activation), transport mechanisms in electrochemical cells (diffusion, convection, migration), polarization curve, depolarizers.
2. Explain equilibrium potentiometry. Defines equilibrium potentiometry direct: pH measurement (glass electrode, pH meter calibration, alkaline and acid error), ion selective electrodes (with glass, crystalline and liquid membrane, selectivity coefficient), gas potentiometric detectors. Defines indirect potentiometry: indication of the end point in volumetric determinations, selection of electrodes.
3. Explain polarography, voltammetry, amperometry. Define voltammetry and polarography: basic circuitry of electrodes in a cell, potentiostat, working electrodes used (solid materials, mercury), voltammetric wave (half-wave potential, limiting current). Explain the use of voltammetry and polarography: direct analysis methods, stripping analysis. Defines amperometry: detection of substances in flowing media, Clark sensor.
4. Explain electrogravimetry, coulometry, conductometry; absolute and comparative analytical methods. Define electrogravimetry and coulometry: performance at constant potential and constant current (coulometric titrations). Defines conductometry: conductivity vessel (two and four electrode), conductivity detectors. Explain the general concepts: absolute and comparative analytical methods.
5. Explain refractometry, polarimetry, nephelometry, presents a general introduction to spectral methods. Define optical methods in which there is no energy exchange when radiation interacts with matter: refractometry, polarimetry, nephelometry. Defines optical methods in which energy exchange occurs when radiation interacts with matter – general introduction to spectral methods: energy of radiation and nature of interaction, absorption (excitation) and emission (relaxation) of energy by atoms and molecules (line and band spectra).
6. Explain absorption spectral methods, introduces calibration methods. Define radiation absorption and related phenomena, Lambert-Beer law, molecular absorption spectrometry, atomic absorption spectrometry. Explain the general concepts: calibration methods – calibration curve, standard addition method.
7. Explain emission spectral methods, present evaluation of analysis results. Explain the method of excitation (electromagnetic radiation – fluorescence spectrometry, thermal energy, electrons), molecular emission spectrometry, atomic emission spectrometry. Explain the general concepts: evaluation of analytical results – error, deviation, accuracy, precision, range, outliers.
8. Explain the basic instrumentation for optical methods. Describe the radiation source, monochromator, sample cell, radiation detector, signal processing and display. Describe the block diagram of absorption and emission (fluorescence) spectral instruments, single and dual channel arrangements. Describes automatic analyzers with optical detection: FIA, CFA.
9. Explain chromatography – separation principles, efficiency, zone expansion, resolution. Defines planar and column chromatography – general basis. Describe the chromatogram: basic parameters (dead time, retention time, retention ratio, peak width, peak height, peak area, peak symmetry). Describes the instrumentation: mobile phase source, dispensing equipment, column, detector, evaluation equipment. Explain the efficiency and optimization of the separation process: column efficiency, resolution, optimization – van Deemter equation.
10. Explain gas chromatography. Describe the experimental setup and performance of gas chromatography: mobile phase, columns, stationary phase, detectors, isothermal elution, temperature program. Explain the use of chromatographic methods: qualitative analysis – separation and identification of compounds, combined methods (GC-MS, GC-IR), quantitative analysis (internal standard, internal standardisation).
11. Explain liquid chromatography (column and planar). Describe the experimental set-up and performance of liquid chromatography: column chromatography – mobile phase, columns, stationary phase, detectors, isocratic and gradient elution; planar chromatography – descending, ascending, two-dimensional elution, retardation factor. Describe the use of chromatographic methods: qualitative analysis – separation and identification of compounds, combined methods (LC-MS), quantitative analysis (internal standard). Explain supercritical fluid chromatography.
12. Explain electromigration methods, explain how to express the result of the analysis. Describe the separation of charged substances in an electric field (migration), zonal and capillary electrophoresis, separation of proteins and amino acids (isoelectric point and choice of pH of the separation medium). Explain the separation modes: capillary zone electrophoresis, micellar electrokinetic chromatography, isotachophoresis, capillary gel electrophoresis. Explain the general concepts: how to express the result of an analysis – arithmetic mean, median, standard deviation, confidence interval, valid digits.
Last update: Vyskočil Vlastimil, prof. RNDr., Ph.D. (27.02.2024)
Literature -

1. F. Opekar a kol.: Základní analytická chemie, skripta, UK, Karolinum, Praha 2002 a 2010.
2. P. Coufal a kol.: Seminář z analytické chemie, skripta, UK, Karolinum, Praha 2001.
3. D. A. Skoog, D. M. West a F. J. Holler: Fundamentals of Analytical Chemistry, 6. Edition, Saunders College Publishing, 1992.
4. Kolektiv: Analytická chemie 2, SNTL Praha, 1980.

Last update: Nesměrák Karel, doc. RNDr., Ph.D. (28.10.2019)
Requirements to the exam -
To pass a credit in analytical chemistry is required to pass both a written credit test and an oral exam (with a written preparation). Requirements for the written tests are given by the extent of the lectures/exercises.
Last update: Vyskočil Vlastimil, prof. RNDr., Ph.D. (13.09.2022)
Syllabus -
Continuation of the lecture C230P01 - Analytical chemistry I.

12. Absolute and comparative analytical methods. Calibration methods (calibration curve method, standard addition method).

13. Basic statistical evaluation of data (accuracy and precision, mean, standard deviation, confidence interval, valid numbers)

14. Electroanalytical methods based on measurement of potential. Equilibrium potentiometry (electrochemical cell, electrodes). Direct potentiometry (measurement of pH, determination of other ions using ISE, selectivity coefficient, gas sensors based on ISE). Indirect potentiometry, potentiometric titrations.

15. Electroanalytical methods based on measurement of current I. Voltammetry and polarography (polarization curve, scheme of electrochemical cell, electrodes, dc, ac and pulse voltammetry. Voltammetric stripping analysys. Amperometry (amperometric detectors).

16. Electroanalytical methods based on measurement of current II. Electrogravimetry and coulometry (potentiostatic and galvanostatic methods, coulometric titrations, colometric analyzers). Conductometry (conductometric analyzers and detectors).

17. Optical methods (the nature of absorption and emission of radiation by atoms and molecules). Atomic and molecular absorption and emission/fluorescence spectra, their utilization in analytical chemistry. Molecular absorption spectrometry in uv/vis range of radiation. Atomic absorption spectrometry.

18. Automatic chemical analysers (FIA, CFA). Nonspectral optical methods (refractometry, polarimetry, nephelometry).

19. Chromatographic methods (fundamentals, classification of chromatographic methods).

Planar chromatography. Column chromatography (general aspects, parameters obtained from chromatogram, separation efficiency, resolution, optimization of separation process). Application of chromatographic methods in quantitative and qualitative analysis (hyphenated methods, GC-MS, LC-MS).

20. Gas chromatography (columns, detectors). Liquid chromatography (selection of mobile phase, classification of LC based on difference in stationary phase - partition, affinity, size-exclusion, ion-exchange chromatography).

21. Electromigration methods. Separation in electric field (zone and capillary electrophoresis). Example of separation - aminoacids and peptides.

Seminar's Syllabus:
1. Acid-base equilibria and pH calculations. Acid-base titrations and stochiometry.

2. Redox equilibria, titrations and stochiometry.

3. Basic principles and calculations in separation methods.

4. Statistics of experimental analytical results.

Last update: FORSTOVA/NATUR.CUNI.CZ (05.04.2013)
 
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