1. Introduction to instrumental methods, their advantages, disadvantages, the distribution of instrumental methods, their qualitative and quantitative use. Defining the problem. Basic terms. Processes of obtaining information. Absolute and comparative analytical methods. Calibration methods. Developments in instrumental methods of analysis.
2. Evaluating results of analysis and their expression. Statistical evaluation of analytical results. Reference material, a circular test. Fundamentals of chemometric approaches and methods. Testing the metrological characteristics of results.
3. - 5. Electroanalytical methods: their classification and principles, cells, electrode potential, Nernst and Peterson equation.
Methods based on measuring potential: Principles, instrumentation layout, uses, advantages and disadvantages. Electrodes and specific cells. Glass pH electrode, experimental approach to measure pH. Ion-selective electrodes. The choice of the electrode system. Nikolsky-Eisenman equation. Electrodes with additional membranes. Specific cell sets for potentiometric titration, evaluation of titration curves. Direct potentiometry, the method of calibration line, the method of standard additions, potentiometric titration, evaluation of titration curves, examples of use.
Methods based on current measurement: Voltammetry and polarography: Fundamentals of polarografic measurements: principle, instrument layout, qualitative and quantitative analysis, use. Mercury drop electrode and its properties. Currents, maximum. Sample treatment for polarographic measurements. Types of titration curves, their interpretation, applications. DC, AC, pulse, differential, inverse; curves shapes, evaluation, and charging the electrolytic current apparatus, calibration methods, examples of use. Current trends in voltammetry.
Amperometry, biamperometry - principles of methods, forms and evaluation of titration curves, examples of use. Electrogravimetry - electrolysis. Faraday's law, elimination of products on the cathode and anode, apparatus, examples of use. Coulometry: principles, coulometry at a constant potential, coulometry at a constant current, coulometric titration, evaluation, chronopotentiometry. Conductometry: mobility of ions, Kohlrausch law, specific and molar conductivity, direct conductometry, calibration, conductometric titration, shapes and evaluation of titration curves, examples of use. Principles, instrumentation, analytical applications, advantages and disadvantages.
6. - 9. Optical methods, interaction of matter and radiation, the classification of optical methods, principles, fundamentals of luminescence analysis, use of optical methods. Optical analytical methods: theoretical basics. Optical spectral apparatus. Non-spectroskopic methods - methods without enery changes between the substance and radiation, a) refractometry- refraction, method principle, apparatus, application examples, b) polarimetry - polarized light, optically active substance, the principle of the method, apparatus, examples of use.
Spectroscopic methods: absorption and emission of radiation, the energy levels of atoms and molecules, degradation of polychromatic radiation by prism and grating, monochromators, interference filters. Emission methods - excitation, electron spectrum a) atomic emission spectroscopy - principles, equipment, registration of spectra, the qualitative and quantitative evaluation, usage examples, b) flame emission spectroscopy - principles, equipment, calibration methods, examples of use.
Absorption methods - absorption of light by atoms and molecules: theory basics, instrumentation, qualitative and quantitative aspects, applications, analytical applications. Atomic absorption spectrometry: principle, flame and flameless atomization, apparatus, calibration methods, examples of use. Molecular absorption spectrometry: principle, transmittance, absorbance, Lambert-Beer law, apparatus, calibration methods, examples of use. Automatic analyzers with optical detection: FIA, CFA. Infrared spectroscopy: Principle, apparatus, instrumentation, evaluation of molecular absorption spectra, analytical use. Raman spectrum - the principle of the method, analytical recovery. Absorption of radio waves and microwaves. Nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR).
10. Separation and concentration steps: theory. Separation methods: separation based on the principle and according to the experimental design, the effectiveness of separation process. Extraction.
11. Membrane separation. Mass spectrometry. Basic theory, instrumentation, qualitative and quantitative aspects of application.
12. Chromatographic methods. Planar Chromatography: Thin layer sorbent chromatography, theory basics, instrumentation, qualitative and quantitative aspects of application.
13. Column chromatography: Liquid chromatography. Gas chromatography. Theory, basic instrumentation, qualitative and quantitative characteristics, analytical use.
14. Electromigration methods: theory, zonal and capillary electrophoresis, electrophoresis on medium and isotachophoresis. Basics of instrumentation, qualitative and quantitative characteristics, analytical use.
Exercise syllabus
Lectures and exercises are conceived as a one-block course for students of combined from of study.
2. Evaluating results of analysis and their expression. Statistical evaluation of analytical results. Reference material, a circular test. Fundamentals of chemometric approaches and methods. Testing the metrological characteristics of results.
3. - 5. Electroanalytical methods: their classification and principles, cells, electrode potential, Nernst and Peterson equation.
Methods based on measuring potential: Principles, instrumentation layout, uses, advantages and disadvantages. Electrodes and specific cells. Glass pH electrode, experimental approach to measure pH. Ion-selective electrodes. The choice of the electrode system. Nikolsky-Eisenman equation. Electrodes with additional membranes. Specific cell sets for potentiometric titration, evaluation of titration curves. Direct potentiometry, the method of calibration line, the method of standard additions, potentiometric titration, evaluation of titration curves, examples of use.
Methods based on current measurement: Voltammetry and polarography: Fundamentals of polarografic measurements: principle, instrument layout, qualitative and quantitative analysis, use. Mercury drop electrode and its properties. Currents, maximum. Sample treatment for polarographic measurements. Types of titration curves, their interpretation, applications. DC, AC, pulse, differential, inverse; curves shapes, evaluation, and charging the electrolytic current apparatus, calibration methods, examples of use. Current trends in voltammetry.
Amperometry, biamperometry - principles of methods, forms and evaluation of titration curves, examples of use. Electrogravimetry - electrolysis. Faraday's law, elimination of products on the cathode and anode, apparatus, examples of use. Coulometry: principles, coulometry at a constant potential, coulometry at a constant current, coulometric titration, evaluation, chronopotentiometry. Conductometry: mobility of ions, Kohlrausch law, specific and molar conductivity, direct conductometry, calibration, conductometric titration, shapes and evaluation of titration curves, examples of use. Principles, instrumentation, analytical applications, advantages and disadvantages.
6. - 9. Optical methods, interaction of matter and radiation, the classification of optical methods, principles, fundamentals of luminescence analysis, use of optical methods. Optical analytical methods: theoretical basics. Optical spectral apparatus. Non-spectroskopic methods - methods without enery changes between the substance and radiation, a) refractometry- refraction, method principle, apparatus, application examples, b) polarimetry - polarized light, optically active substance, the principle of the method, apparatus, examples of use.
Spectroscopic methods: absorption and emission of radiation, the energy levels of atoms and molecules, degradation of polychromatic radiation by prism and grating, monochromators, interference filters. Emission methods - excitation, electron spectrum a) atomic emission spectroscopy - principles, equipment, registration of spectra, the qualitative and quantitative evaluation, usage examples, b) flame emission spectroscopy - principles, equipment, calibration methods, examples of use.
Absorption methods - absorption of light by atoms and molecules: theory basics, instrumentation, qualitative and quantitative aspects, applications, analytical applications. Atomic absorption spectrometry: principle, flame and flameless atomization, apparatus, calibration methods, examples of use. Molecular absorption spectrometry: principle, transmittance, absorbance, Lambert-Beer law, apparatus, calibration methods, examples of use. Automatic analyzers with optical detection: FIA, CFA. Infrared spectroscopy: Principle, apparatus, instrumentation, evaluation of molecular absorption spectra, analytical use. Raman spectrum - the principle of the method, analytical recovery. Absorption of radio waves and microwaves. Nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR).
10. Separation and concentration steps: theory. Separation methods: separation based on the principle and according to the experimental design, the effectiveness of separation process. Extraction.
11. Membrane separation. Mass spectrometry. Basic theory, instrumentation, qualitative and quantitative aspects of application.
12. Chromatographic methods. Planar Chromatography: Thin layer sorbent chromatography, theory basics, instrumentation, qualitative and quantitative aspects of application.
13. Column chromatography: Liquid chromatography. Gas chromatography. Theory, basic instrumentation, qualitative and quantitative characteristics, analytical use.
14. Electromigration methods: theory, zonal and capillary electrophoresis, electrophoresis on medium and isotachophoresis. Basics of instrumentation, qualitative and quantitative characteristics, analytical use.
Exercise syllabus
Lectures and exercises are conceived as a one-block course for students of combined from of study.