617-3023/01 – Advanced analytical methods (PAM)

Gurantor departmentDepartment of ChemistryCredits5
Subject guarantordoc. Ing. Vlastimil Matějka, Ph.D.Subject version guarantordoc. Ing. Vlastimil Matějka, Ph.D.
Study levelundergraduate or graduateRequirementCompulsory
Year1Semesterwinter
Study languageCzech
Year of introduction2019/2020Year of cancellation
Intended for the facultiesFMTIntended for study typesFollow-up Master
Instruction secured by
LoginNameTuitorTeacher giving lectures
MAT27 doc. Ing. Vlastimil Matějka, Ph.D.
VON37 Ing. Jiřina Vontorová, Ph.D.
Extent of instruction for forms of study
Form of studyWay of compl.Extent
Full-time Credit and Examination 2+3

Subject aims expressed by acquired skills and competences

The aim of the lectures and laboratory practice is to introduce the methods of chemical and phase analysis and selected methods of the electron microscopy. The students will acquire the knowledge of the principles of the selected instrumental analytical methods, construction of the instruments and will understand the interpretation of the results obtained with these methods.

Teaching methods

Lectures
Tutorials
Experimental work in labs

Summary

The subject is focused on theoretical and practical education of the advanced methods used for the studies of different types of materials occurring in solid, liquid as well as gas phase.

Compulsory literature:

CHRISTIAN Gary, D., et al. Analytical chemistry. New York: Wiley, 2013. ISBN 978-0-470-88757-8.

Recommended literature:

GUNZLER, Helmut and Alex WILIAMS. Handbook of Analytical Techniques. Weinheim: Wiley-VCH Verlag GmbH, 2008. ISBN: 978527618323.

Way of continuous check of knowledge in the course of semester

Credit test and oral exam.

E-learning

Other requirements

There are no additional requirements.

Prerequisities

Subject has no prerequisities.

Co-requisities

Subject has no co-requisities.

Subject syllabus:

1. Determination of chemical composition of matter using x-ray fluorescence spectroscopy. Origination of x-ray irradiation, interaction of x-rays with matter, energy and wave dispersive spectrometers, sample preparation, qualitative and quantitative analysis. X-ray fluorescence microanalysis. Examples of practical utilization. 2. Optical emission spectroscopy with spark and glow discharge excitation. Excitation and characteristic of emission spectra. Construction of OE spectrometers, sample preparation, qualitative and quantitative analysis. Utilization of GD-OES for analysis of the depth and chemical composition of thin layers. Methods of the elemental chemical analysis for the determination of C, S, N, O and H. Examples of practical utilization. 3. X-ray diffraction method. Interaction of x-ray with crystal and amorphous matter, overview of x-ray diffraction techniques. X-ray powder diffraction methods, elements of the x-ray powder diffractometers, x-ray powder diffraction pattern, qualitative and quantitative analysis. Examples of practical utilization. 4. Electron microscopy techniques. Scanning electron microscopy, interaction of the electrons with matter, secondary and back scattered electrons for surface image reconstruction, construction of scanning electron microscopes, energy and wave dispersive microanalysis. Transmission electron microscopy, reconstruction of the images, sample preparation, construction of microscopes. Examples of practical utilization. 5. IR spectrometry, interaction of IR irradiation with matter, IR spectra, construction of IR spectrometers, evaluation of IR spectra. Raman spectroscopy, origination of Raman spectra, construction of Raman spectrometers, evaluation of Raman spectra. Practical utilization. 6. UV-VIS diffuse reflectance spectroscopy, interaction of UV and VIS irradiation with matter, principle of the UV-VIS-DRS method, band gap energy evaluation, color measurement. Examples of practical utilization. 7. Determination of specific surface area of powder samples using BET method, construction of the instruments, physical sorption, types of isotherms, evaluation of micro- and mezo- pores. Mercury porosimetry and its utilization for determination of macro and mezzo pores, principle of method, construction of the instruments. Determination of particle size distribution of powder samples using laser diffraction method. Examples of practical utilization. 8. Thermogravimetry, principle of the method, construction of instruments, thermogravimetric curves. Differential thermal analysis, principle of the method, construction of instruments, DTA curves. Differential scanning calorimetry, principle of the method, construction of instruments, DSC curves. Examples of practical utilization. 9. The methods for the transformation of samples from solid to liquid phase. Atomic absorption spectroscopy, principle of the method, absorbance, irradiation sources, flame atomization, electrothermal atomization, hydride generation and cold-vapor atomization. Construction of the instruments. Inductively coupled plasma - Atomic emission spectroscopy, principle of the method, construction of the instruments. Examples of practical utilization. 10. Electrochemical analysis. Electrochemical potential, electrodes, potentiometry, conductivity measurement, voltammetry, amperometry. Methods based on the electrolysis, dissolution techniques, electrogravimetry. Examples of practical utilization. 11. Methods based on the migration of ions in electric field. Electrophoresis, types and their principles, construction of the instruments. Isotachophoretic analysis, principle of the method, one and two column set-up, the role of leading and terminating solvent. Examples of practical utilization. 12. Liquid and ion chromatography, principle of the methods (column, ion-exchange, gel-permeation, affinity chromatography, paper chromatography, thin layer chromatography, high pressure liquid chromatography), ion separation principles, construction of the instruments. Evaluation of the data, examples of practical utilization. 13. Gas chromatography, carrier gas, sample injection, kinds of columns, detectors, examples of practical utilization. Spectroscopic method of the gas mixtures analysis. Methods for the evaluation of mass and numbers of particulate matter in atmosphere. Examples of practical utilization. Laboratory practice: 1. Safety in laboratory 2. X-ray fluorescence spectroscopy (measurement of chemical composition of powder samples) 3. X-ray fluorescence spectroscopy (measurement of chemical composition of alloys) 4. Glow discharge optical emission spectroscopy (determination of the chemical composition of alloys, depth profiling of zinc coating). 5. X-ray diffraction analysis (identification of phases in powder samples) 6. X-ray diffraction analysis (quantitative determination of the amount of the phases) 7. Scanning electron microscopy (observation of the microstructure of alloys, chemical microanalysis) 8. Atomic absorption spectroscopy (quantitative analysis of the selected elements in the alloy after its decomposition) 9. Elemental analysis (determination of C, S, N, O and H in alloys, determination of TOC in liquid samples) 10. IR and Raman spectroscopy (study of the powder samples) 11. Determination of the specific surface area using BET method, determination of the density using He pycnometry (determination of specific surface area of the powder samples) 12. Chromatography (determination of the content of organic solvents using gas chromatography) 13. Isotachophoresis (utilization of isotachophoresis for separation of the dyes) 14. Presentation of the results, evaluation of the activity.

Conditions for subject completion

Full-time form (validity from: 2019/2020 Winter semester)
Task nameType of taskMax. number of points
(act. for subtasks)
Min. number of points
Credit and Examination Credit and Examination 100 (100) 51
        Credit Credit 30  16
        Examination Examination 70  35
Mandatory attendence parzicipation: 100% participation in laboratory exercises.

Show history

Occurrence in study plans

Academic yearProgrammeField of studySpec.ZaměřeníFormStudy language Tut. centreYearWSType of duty
2021/2022 (N0712A130004) Chemical and environmental engineering TCH P Czech Ostrava 1 Compulsory study plan
2020/2021 (N0712A130004) Chemical and environmental engineering TCH P Czech Ostrava 1 Compulsory study plan
2019/2020 (N0712A130004) Chemical and environmental engineering TCH P Czech Ostrava 1 Compulsory study plan

Occurrence in special blocks

Block nameAcademic yearForm of studyStudy language YearWSType of blockBlock owner