Advanced instrumental analysis 0600-S2-O-ZAI

Lecture:
Mass spectroscopy in applications for identification and quantitative analysis of chemical compounds. Techniques combined with mass spectroscopy (ESI-MS, HPLC-ICP-MS). Application of laser ablation in chemical analysis. Atomic absorption and emission spectroscopy (ASA, ICP, AES) and X-ray methods (XRF, XRD) used to determine metals in materials. Electrochemical methods: DC polarography, hanging drop, coulometry, field effect transistor-based sensors in chemical analysis. Electron spectroscopy (XPS, Auger) in material research. Electron microscopy (SEM, TEM, STEM) and atomic force microscopy (AFM) in materials testing applications. Methods of thermal analysis in the characteristics of materials (TGA, DTA, DSC).
Laboratory exercises:
1. X-ray diffraction (XRD); Identification of chemical compounds by powder method. Theoretical and practical problems are discussed: elements of symmetry of molecules, crystallographic systems, basic types of crystal structure of inorganic compounds, construction and operation of apparatus, research techniques, interpretation of diffraction patterns.
2. Thermal analysis (TG/DTG/DTA, DSC); Analysis of the reaction course of thermal decomposition of substances, on the example of inorganic salts and complex compounds. Theoretical and practical problems are discussed: the division of thermoanalytical methods, thermal and thermogravimetric analysis (definitions, apparatus, principle of measurement), TG, DTA, DTG curves and their interpretation, phase transitions of the first and higher types, energy effects accompanying chemical reactions, differential scanning calorimetry (definitions, apparatus, principle of measurement, factors influencing the course of measurement), applications of differential scanning calorimetry.
4. Spectrofluorimetry; Determination of B vitamins in pharmaceutical preparations. Theoretical and practical problems discussed: types of luminescence, differences between absorption, fluorescence and phosphorescence, transitions between energy levels, molecules characteristic of fluorescence and phosphorescence, physicochemical parameters affecting the value of fluorescence intensity, fluorescence quenching, construction of a spectrofluorimeter, application, advantages and disadvantages of fluorimetric methods .
5. Scanning electron microscopy and atomic force microscopy (SEM, AFM); Use of electron microscopy and AFM imaging techniques to evaluate various materials. Theoretical and practical problems are discussed: scanning electron microscope - construction and principle of operation, detection methods used in SEM, techniques of work, causes of image distortion, methods of sample preparation; AFM - operating modes, limitations of the method, working environment of the microscope. SEM and AFM methods are compared with each other and with optical microscopy.
6. Polarography, Determination of heavy metals by standard addition method. Theoretical and practical problems discussed: theoretical foundations of AC and DC polarography (formulas, diagrams, graphs), qualitative and quantitative analysis, construction of the measurement system, electrode processes, the role of the basic electrolyte in polarographic analysis, faradaic currents, polarographic maxima.
7. Cyclic, inversion voltammetry; Determination of the concentration of iron in the form [Fe(III)(CN)6]3- by cyclic voltammetry. Determination of heavy metals in water using a hanging drop mercury electrode. Theoretical and practical problems are discussed: Nernst equations, double layer charging phenomenon, Faraday's laws, Faraday and non-Faraday processes, anode and cathode current, electrodes used in voltammetry, parameters of volt amperometric curves, criteria for reversibility of electrode processes, types of volt amperometric methods, hanging droplet mercury electrode, volt-amperometric curves, electrochemical processes, principles of measurement.