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Terminated in academic year 2021/2022

Methods of Instrumental Analysis

Type of study BachelorFollow-up Master
Language of instruction Czech
Code 617-2007/01
Abbreviation MIA
Course title Methods of Instrumental Analysis
Credits 6
Coordinating department Department of Chemistry
Course coordinator prof. Ing. Petr Praus, Ph.D.

Subject syllabus

Lectures
1. Properties of light, interaction of light with matter , refractive index (Cauchy equation)., light reflection and refraction, diffraction and interference of light refraction. Refractometry, interferometry and polarimetry.

2. Model of the atom, quantum numbers, Boltzmann law, the width of spectral lines. Dispersion of light, detection of electromagnetic radiation.

3. Atomic emission spectrometry, equipments, detectors, practical use.

4. Atomic absorption spectrometry, Lambert-Beer Law, methods of atomization, detectors, equipments, practical use.

5. Interaction of X-rays with matter, X-ray spectra, Auger effect, X-ray fluorescence spectrometry, sample preparation, X-ray dispersion, detectors, practical use.

6. X-ray diffraction, crystalline planes, Müller indexes, Debye-Scherrer method, evaluation of diffractograms, practical use. Electron Spectroscopy: Wehnelt cylinder, analyzers of electrons. Electron spectroscopy for chemical analysis (ESCA), Auger spectroscopy.

7. Interaction of molecules and electromagnetic irradiation, molecular spectra, LCAO theory, ligand field theory, charge -transfer complexes. UV-VIS absorption spectroscopy, luminescence spectroscopy, practical use.

8. Vibration of molecules, infrared spectrometry, equipments, FTIR spectroscopy, practical use.

9. Core in external magnetic field, NMR spectroscopy, equipments. Mass spectroscopy: ionization of molecules, fragmentation, separation of ions in the magnetic and electric field, the detection of ions, practical use.

10. Electrochemical potential (Peters and the Nernst equation), types of electrodes, direct potentiometry and potentiometric titration, practical use. Conductivity of strong and weak electrolytes, direct conductometry and conductometric titration, use in practice.

11. Electrolysis, Ilkovicova equation, polarography, AC-DC methods, voltammetry, practical use.

12. Separation methods in analytical chemistry, chromatography: principles of separation, van Deemterova and Giddings curve. Gas chromatography, liquid chromatography, practical use.

13. Migration of ions in electric field, ion electrophoretic mobility, electroosmotic flow. Plate and capillary electrophoresis, capillary isotachophoresis, isoelectric focusing, practical use.

14. Statistical treatment of analytical results, type of errors, normal distribution and its parameters, confidence intervals , statistical tests, reference materials.

Laboratory exercises
• Determination of resin exchange capacity •
• Spectrophotometric study (determination of manganese and chromium in VIS region
• Polarographic studies (determination of cadmium, nickel and zinc)
• Potentiometric determination of chromium and vanadium in steel
• Determination of cadmium and lead by atomic absorption spectrometry
• Determination of sulphate by conductometric titration
• Identification of simple organic compounds by gas chromatography
• Determination of nitrate in waters by UV spectrophotometry
• Refractometric determination of the Fridex concentration
• Conductometric determination of specific electrolytic conductivity of water
• Validation of methods for the determination of chromium in water - VIS spectrophotometry
• Potentiometric determination of pH
• Determination of nitrite in water - VIS spectrophotometry
• Determination of chloride ion selective electrode
• Determination of lead by amperometric titration
• Identification of simple organic compounds by FT-IR spectroscopy (using the ATR technique)
• Determination of elements in coal by X-ray fluorescence analysis

Literature

[1] G. D. Christian, Analytical Chemistry (5 th Ed.). New York ,
Wiley, 1994, 812 s.
[2]D. Kealay, P.J: Haines, Analytical Chemistry. Oxford, BIOS Scientific Publishers, 2002, 342 s.
[3]J. Kenkel, Analytical Chemistry for Technicians (4th Ed.). Boca Raton, CRC Press, 2014, 507 s.

Advised literature

1. Sommer L. a kol., Základy analytické chemie I. Skriptum, Brno, VUTIUM, 1998, 199 s.
2. Sommer L. a kol. Základy analytické chemie II. Skriptum, Brno, VUTIUM, 2000, 347 s.
3. Tomík B., Poljak B., Jirkovský R. Analytická chemie pro hutníky. Praha, SNTL, 1988, 264 s.
4. Vláčil F. a kol., Příklady z chemické a instrumentální analýzy Praha, SNTL, 1983, 432 s.
5. Churáček J. a kol., Analytická separace látek. Praha, SNTL, 1990, 384 s.