Course: Instrumental Methods

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Course title Instrumental Methods
Course code ACH/IME
Organizational form of instruction Lecture
Level of course Bachelor
Year of study not specified
Semester Winter
Number of ECTS credits 4
Language of instruction Czech
Status of course Compulsory, Compulsory-optional, Optional
Form of instruction Face-to-face
Work placements This is not an internship
Recommended optional programme components None
Lecturer(s)
  • Milde David, doc. Ing. Ph.D.
  • Jirovský David, doc. RNDr. Ph.D.
  • Papoušková Barbora, RNDr. Ph.D.
Course content
Liquid chromatography - paper and thin-layer chromatography, column chromatography. Instrumentation - solvent delivery systems, injection devices, columns, detectors, auxiliary devices. Retention in HPLC, principles of separation (normal-phase and reversed-phase liquid chromatography, ion-pair chromatography, liquid-liquid chromatography, separation of chiral compounds, ion-exchange chromatography, size-exclusion and affinity chromatography). Hyphenation of separation and spectral techniques (GC/MS, GC/IR, HPLC/MS, HPLC/FTIR, HPLC/NMR, CE/MS).Electromigration methods (electrophoretic mobility, electroosmotic flow, capillary electrophoresis, isotachophoresis). Mass spectrometry- origin of mass spectra; a scheme of mass spectrometer, resolution. Selected ion sources (electron ionization - EI, chemical ionization - CI, atmospheric pressure chemical ionization - APCI, electrospray ionization - ESI, desorption electrospray ionization - DESI, direct analysis in real time - DART, fast atom (ion) bombardment - FAB, FIB, laser desorption ionization - LDI, matrix assisted laser desorption ionization - MALDI). Mass analyzers - sector instruments, quadrupole, ion trap, time of flight, ion cyclotron resonance, orbitrap. Tandem mass spectrometry. Detection and registration of ions, vacuum systems. Mass spectrometry in a structural analysis. Quantitative analysis. Mass spectrometry of inorganic compounds. Spectrometry. Electromagnetic radiation. Absorption, emission and luminescence of radiation. Fundamental parts of spectrometers: radiation sources, monochromators, detectors. Atomic spectrometry - atomic absorption and fluorescence spectrometry, optical emission spectrometry (flames, plasma and electrical discharges). X-ray fluorescence. Application of atomic spectrometry.Molecular spectrometry - UV/Vis absorption spectrometry (theory, instrumentation, application). Fluorescence and phosphorescence of molecules. IR spectrometry (molecular vibrations and rotations, instrumentation, application). Raman spectrometry. NMR: principle, NMR spectrometer, NMR spectrum, analytical applications. Methods without energy exchange between radiation and matter: refractometry, polarymetry, turbidimetry, nephelometry. Electroanalytical Methods Classification of Electrochemical Methods. Electrochemical Cells, Electrodes. Potentiometric Methods of Analysis - Instrumentation, Ion-Selective Electrodes, Measurement of pH. Potentiometric Titrations. Voltammetry - Instrumentation, Electrode Process, Current-Potential Curves. Basic Voltammetric Techniques - DC Polarography and Voltammetry, Normal and Differential Pulse Voltammetry, Electrochemical Stripping Analysis. Titrations with Polarized Electrodes. Coulometry and Electrogravimetry - Instrumentation, Controlled-Potential and Controlled-Current Techniques. Conductometric Methods of Analysis - Conductometric Titrations, Measurement of Specific Electric Inductive Capacity.

Learning activities and teaching methods
Lecture
  • Attendace - 52 hours per semester
  • Homework for Teaching - 39 hours per semester
  • Preparation for the Course Credit - 89 hours per semester
Learning outcomes
The course provides the introduction to the field of instrumental techniques used in analytical chemistry
Explain the principles of instrumental methods of chemical analysis, interpret a problem, describe the solution of analytical problems
Prerequisites
The knowledge of basics of general, organic, anorganic, physical and analytical chemistry is recommended.

Assessment methods and criteria
Mark, Written exam

written final test, it is necessary to achieve at least 50% of all the points.
Recommended literature
  • Atomová spektroskopie- T. Černohorský, P. Jandera, Univerzita Pardubice 1997.
  • Barek J., Opekar F., Štulík K.: Elektroanalytická chemie (skriptum). Karolinum, Praha 2004.
  • de Hoffmann E., Stroobant, V.: Mass Spectrometry. Principles and Applications. John Wiley and sons, Chichester, 2002..
  • Foret F., Křivánková L., Boček P.: Capillary Electrophoresis (Radola B. J., ed.), VCH Verlagsgesellschaft Weinheim, 1993..
  • Harris D. C.: Quantitative Chemical Analysis. W. H. Freeman and Company, New York 2003.
  • Harvey D.: Modern Analytical Chemistry. McGraw-Hill, New York 2000.
  • Heiger D. N.: High Performance Capillary Electrophoresis - An Introduction, Hewlett-Packard GmbH Waldbronn, 1992..
  • Holčapek M. (editor): Spojení vysokoúčinné kapalinové chromatografie a hmotnostní spektrometrie, Spektroskopická společnost Jana Marca Marci a Univerzita Pardubice, Pardubice, 2001..
  • Churáček J. a kol.: Analytická separace látek, SNTL Praha, 1990..
  • I. Wilson, C. Poole, M. Cooke: Encyclopedia of separation science. Academic Press, San Diego, London, Boston, New York, Sydney, Tokyo, Toronto 2000..
  • Jandera P.: Molekulová spektroskopie v organické analýze. Univerzita Pardubice, Pardubice, 1999..
  • Kellner R., Mermet J.-M., Otto M., Valcárcel M., Widmer, H. M.(eds.): Analytical Chemistry. A Modern Approach to Analytical Science. Wiley-VCH, Weinheim 2004.
  • Li S. F. Y.: Capillary Electrophoresis, Journal of Chromatography Library 52, Elsevier Amsterodam, 1993..
  • Modern Analytical Chemistry, D. Harvey, The Mc Graw Hill 2000.
  • Modern Practice of Gas Chromatography Ed. R.L. Grob, E.F. Barry, Wiley-Interssience , 2004.
  • Niessen W.M.A.: Liquid Chromatography-Mass Spectrometry, Marcel Dekker, New York, 1999..
  • Opekar F. a kol.: Základní analytická chemie (skriptum). Karolinum, Praha 2003..
  • Poole C., F., Poole S., K.: Chromatography Today, Elsevier, Amsterdam, 1991..
  • Principles of Instrumental Analysis, D.A.Skoog, F.J. Holler, T.A. Nieman , Brooks/cole Thomson Learning 1997.
  • R. E. Ardrey: Liquid Chromatography - Mass Spectrometry: An Introduction. John Wiley & Sons, Chichester 2003..
  • Štulík K. a kol: Analytické separační metody, Karolinum UK Praha 2004.
  • Ubik K.: Fyzikálně-chemické metody, část 2, Hmotnostní spektrometrie, Ústav organické chemie a biochemie AV ČR, Praha, 2000..
  • Vřešťál J. (editor): Hmotnostní spektrometrie, Masarykova Univerzita, Brno, 1998.


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