(in Polish) Zaawansowane metody instrumentalne 0600-S2-CM-ZAI

Lecture:

Mass spectroscopy in applications for identification and quantitative analysis of chemical compounds. Techniques combined with mass spectroscopy (ESI-MS, HPLC–ICP-MS, LDI). Application of laser ablation in chemical analysis. Atomic absorption and emission spectroscopy (ASA, ICP, AES). Methods using X-rays (XRF, XRD, TEM, XPS) as a source of information about the tested sample. Electrochemical methods: DC polarography, hanging drop, coulometry, field effect transistor-based sensors in chemical analysis. Sensors and biosensors. Electron (Auger) spectroscopy in materials research. Electron microscopy (SEM, TEM, STEM) and atomic force microscopy (STM, 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 the powder method. Theoretical and practical problems are discussed: elements of symmetry of molecules, crystallographic systems, basic types of the crystal structure of inorganic compounds, structure and operation of apparatus, research techniques, and interpretation of diffraction patterns.

2. Thermal analysis (TG / DTG / DTA, DSC); Analysis of the course of the thermal decomposition of substances, on the example of inorganic salts and complex compounds. Theoretical and practical problems are discussed: division of thermoanalytical methods, thermal and thermogravimetric analysis (definitions, apparatus, measurement principle), 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, measurement principle, factors influencing the course of measurement), applications of differential scanning calorimetry.

3. Infrared spectroscopy (IR, TG / IR); Spectroscopic quantitative analysis of a multicomponent mixture. Application of vibrational spectroscopy to qualitative analysis of thermal decomposition products. Discussed theoretical and practical problems: absorption laws and their practical application in qualitative and quantitative analysis, quantification methods using infrared spectroscopy (standard curve, arithmetic curve, internal standard), oscillation spectrum, parameters describing the absorption band (the problem of intensity and intensity of the integral band absorption) and their importance for quantitative measurements (transmittance, absorbance), the accuracy of the method and causes of errors.

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 influencing the value of fluorescence intensity, fluorescence quenching, spectrofluorimeter structure, application, advantages and disadvantages of fluorimetric methods.

5. Scanning electron microscopy and atomic force microscopy (SEM, AFM); The use of imaging techniques by electron microscopy and AFM to evaluate various materials. Theoretical and practical problems are discussed: scanning electron microscope - structure and principle of operation, detection methods used in SEM, techniques of work of the cause of image disturbances, sample preparation methods AFM - operating modes, method limitations, microscope work environment. SEM and AFM methods are compared with each other and with optical microscopy.

6. Polarography, Determination of heavy metals by the 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 measuring system, electrode processes, the role of the primary electrolyte in polarographic analysis, Faraday currents, polarographic maxima.

7. Cyclic, inverse voltammetry; Determination of iron concentration in the form of [Fe(III)(CN)6]3- by cyclic voltammetry method, 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 currents, electrodes used in voltammetry, parameters of amperometric volt curves, criteria for reversibility of electrode processes, types of volt amperometric methods, hanging drip mercury electrode, amperometric volt curves, electrochemical techniques, measurement principles.