Advanced Instrumental Analysis 0600-S2-EN-AIA

Lecture:
Raman and IR spectroscopy methods in applications to the identification and quantitative analysis of chemical compounds.
Mass spectroscopy in applications for the identification and quantitative analysis of chemical compounds. Combined analytical techniques with mass spectroscopy (ESI-MS, HPLC–ICP-MS, GC-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 various matrices.
Electron spectroscopy (XPS, Auger) in materials research.
Electron microscopy (SEM, TEM, STEM) and atomic force microscopy (AFM) in various applications.
Combined analytical techniques in the analysis of works of art, biological material and material research.
Application of XRF in forensic and food analysis.

Laboratory exercises:

1. X-ray diffraction (XRD); Identification of chemical compounds using the powder method. Theoretical and practical problems are discussed: elements of molecular symmetry, crystallographic systems, basic types of crystal structure of inorganic compounds, structure and operation of equipment, research techniques, interpretation of diffractograms.

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: division of thermoanalytical methods, thermal and thermogravimetric analysis (definitions, equipment, measurement principle), TG, DTA, DTG curves and their interpretation, phase transformations of the first and higher types, energy effects accompanying chemical reactions, differential scanning calorimetry (definitions, equipment, measurement principle, factors influencing the measurement process), applications of differential scanning calorimetry.
3. Infrared spectroscopy (IR, TG/IR); Quantitative spectroscopic analysis of a multi-component mixture. Application of vibrational spectroscopy for qualitative analysis of thermal decomposition products. Theoretical and practical problems discussed: absorption laws and their practical application in qualitative and quantitative analysis, methods of quantitative determinations using infrared spectroscopy (standard curve, arithmetic, internal standard), vibrational spectrum, parameters describing the absorption band (the problem of intensity and integral intensity of the absorption band) and their importance for quantitative measurements (transmittance, absorbance), 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 affecting the fluorescence intensity value, fluorescence quenching, spectrofluorimeter construction, applications, advantages and disadvantages of fluorimetric methods.

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