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Spectrometric Methods

Class at Faculty of Science |
MC230P04N

Syllabus

Principle and classification of spectrometric methods: Properties of electromagnetic radiation. Energy states of atoms and molecules. Classification of methods (interaction radiation-mass with the exchange and without exchange of energy).

Basic instrumentation: Radiation sources, dispersion systems, detectors.

Analytical determinations using spectrometric methods: Analyte concentration determination, evaluation of measurement, errors.

Spectral analysis in X-ray range: Theoretical background (origin of X-rays, characteristics of spectrum, basic relationships). The methods based on X-ray emission (primary radiation -EMA, PIXE; secondary radiation - fluorescence spectroscopy), absorption and diffraction. Experimental set-up and analytical application of individual methods.

Atomic emission spectroscopy: Theoretical background (origin of emision spectra, characteristics of spectra, basic relationships). The flame photometry, spectrography, automatic spectrometry, AES-ICP, ICP-MS. Experimental (excitation sources, dispersion systems, detection of radiation and registration of signals) and analytical applications of all methods.

Atomic absorption and fluorescence spectrometry: Theoretical background (principle of methods, basic relationships. Experimental (primary radiation sources, absorption medium, dispersion system, detection of radiation and registration of signals, background correction).

Analytical application, interferences. Comparison of mostly used atomic spectrometric methods.

Molecular absorption spectrometry in UV/VIS range of radiation: Theoretical background (electronic transitions in inorganic and organic compounds, in metal complexes, CT transitions). Static measurement (colorimetry, photometry, spectrophotometry), dynamic measurement (kinetic methods, flow-through methods). Extraction spectrophotometry. Experimental. Analytical applications.

Molecular luminiscent spectrometry: Theoretical background (photoluminiscence - fluorescence, phosphorescence, chemiluminiscence; the effect of structure of compounds, basic relationships). Fluorimetry and spectrofluorimetry, phosphorimetry. Experimental, analytical applications.

Molecular absorption spectrometry in infrared range of radiation: Theoretical background (vibration and rotation of molecules, basic relationships). Experimental - dispersion spectrometers (radiation sources, dispersion system, detection), Fourier-transform spectrometers. Transmission and reflection measurement, the types of measurement according to sample state. Application (structural analysis, quantitative analysis).

Raman spectrometry: Theoretical background (nonelastic scattering of radiation, basic relationships). Experimental - dispersion instruments, Fourier-transform Raman spectrometry. Analytical application.

Nuclear magnetic resonance: Theoretical background (nuclei with magnetic moment, effect of magnetic field, basic relationships; chemical shift, spin interactions). Experimental (continual measurement, FT-NMR). Application.

Electron paramagnetic (spin) resonance: Theoretical background (systems with non paired electrons, basic relationships; g-factor, hyperfine splitting). Experimental, application.

Mass spectrometry: Theoretical background (ionization, molecular ions, the mechanism of fragmentation of molecules, mass spectrum). Experimental (ion sources, mass analyzers, detectors). The connection of MS with separation methods. Analytical applications.

Refractometry, interferometry: Theoretical background (refractive index, molar refraction). Refractometry - principle, experimental. Interferometry-principle, experimental. Analytical applications.

Polarimetry, spectropolarimetry. Theoretical background (polarization of radiation, optical activity of chiral compounds, specific rotation). Optical rotation dispersion, circular dichroism. Experimental, analytical application.

Nefelometry, turbidimetry: Theoretical background (elastic scattering in turbid samples). Experimental, analytical applications.

Annotation

A basic overview in spectrometric methods used for chemical analyses. Principles of methods, interactions between the analyzed compounds and the electromagnetic radiation, instrumentation, typical measurement procedure and evaluation of results are explained in these lectures including listed examples of analytical applications.