C8102 Special methods - laboratory course

Faculty of Science
Spring 2011 - only for the accreditation
Extent and Intensity
0/0/5. 5 credit(s) (plus extra credits for completion). Type of Completion: graded credit.
Teacher(s)
RNDr. Marta Farková, CSc. (seminar tutor)
Mgr. Aleš Hrdlička, Ph.D. (seminar tutor)
prof. RNDr. Přemysl Lubal, Ph.D. (seminar tutor)
doc. Mgr. Karel Novotný, Ph.D. (seminar tutor)
prof. Mgr. Jan Preisler, Ph.D. (seminar tutor)
doc. Mgr. Petr Táborský, Ph.D. (seminar tutor)
prof. RNDr. Libuše Trnková, CSc. (seminar tutor)
doc. Mgr. Tomáš Vaculovič, Ph.D. (seminar tutor)
Ing. Blanka Vrbková, Ph.D. (seminar tutor)
Guaranteed by
doc. Mgr. Karel Novotný, Ph.D.
Department of Chemistry - Chemistry Section - Faculty of Science
Contact Person: doc. Mgr. Karel Novotný, Ph.D.
Prerequisites (in Czech)
! C6390 Org. chem. physical methods
Je vhodné absolvovat před cvičením přednášky: Separační metody C7021, Atomová spektrometrie C7031, Molekulová spektrometrie C7041, Elektroanalytické metody C7050. Vhodná je C7830 Kapilární elektroforéza a C7895 Analytická hmotnostní spektrometrie.
Course Enrolment Limitations
The course is only offered to the students of the study fields the course is directly associated with.
fields of study / plans the course is directly associated with
there are 15 fields of study the course is directly associated with, display
Course objectives
Main objectives can be summarized as practice training in optical spectroscopy, mass spectroscopy, electroanalytical methods, separation methods. a) Molecular fluorescence, UV/Vis spectrotphotometry, atomic emission spectrometry with inductively coupled plasma (ICP-AES), laser spectrometry (LA-ICP-OES, LIBS), spark spectrometry. b) Moderne electroanalytical methods. Elimination voltammetry, stripping voltammetry, potentiometry, dielectrimetry. c) High performance liquid chromatography (HPLC), isotachophoresis, gas chromatography, capillary zone electrophoresis, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS).
Syllabus
  • A) Introduction to course, classified test: spectroscopy, separation methods, electroanalytical methods. B) ELECTROANALYTICAL METHODS 1. Determination of dipole moment of cyclohexanone ond/or cyclohexanol. Capacity and permitivity of liquid dielectrics, polarization of dielectrics, Hedestrand method, calculation of DM. 2. Reduction of azide derivative - determination of number of electrons in dependence on pH (coulometry with ISES) 3. Determination of chloride in milk products. Potentiometric titration, calibration curve method, standard addition method, comparison of methods) 4. Analysis of feed salt by anodic stripping difference pulse voltammetry. Determination of heavy metals Cd, Pb, Cu, Zn) 5.Elimination voltammetry in analytical chemistry. HMDE and carbon electrode PIGE, reduction and oxidation of selected depolarizers. Comparison of processes, rate determining step, advantages for analysis. C) SPECTRAL METHODS 6. Analysis of archaeological samples (bones) by inductively coupled plasma - optical emission spectrometry. Method development for ICP-OES instrument Jobin-Yvon 170 Ultrace: analytical line selection, background correction points, calibration curves, analysis of real samples. 7. Diagnostics of ICP - determination of excitation temperature in ICP discharge using Fe emission lines set and two-lines method. Calcualtion of average electron density in ICP discharge using Stark broadening of H 486,1 nm line. 8. Fluorescent determination of quinine and riboflavin. Estimation of excitation and emission maxima of quinine and riboflavin in solution, calibration curve, determination of riboflavin (in tablets) and quinine (in tonic) in real samples 9. UV/VIS molecule spectroscopy. Multicomponent spectroscopic and kinetic analysis (Determination of bichromate and permanganate in mixture; determination of molybdate and tungstate in mixture; determination of Fe(II) and Fe(III) ions in mixture; determination of Co(II) and Cr(III) ions in mixture) 10.Analysis of steel by laser ablation - inductively coupled plasma optical emission spectrometry. Optimization of ablation parameters. Calibration curves and analysis of real steel and soil pelet samples. 11. Analysis of steel using spark spectrometry. Interferences of analytical lines. Calibration and analysis of real steel samples. 12. Using laser-induced breakdown spectrometry in steel samples analysis. Optimization of laser parameters (beam focusing, pulse energy). Calibration curve asnd analysis of real steel and soil pellet samples. D) SEPARATION METHODS 13. High performance liquid chromatography. Determination of inosin, adenosin and their 2’-deoxy-forms in model mixture – optimaliztion and validation method. 14. Isotachophoresis. Determination of glutamic acid in instant soup. ITP instrument EA 100 (Vila Labeco, SR), double-column systém ITP-ITP with preconcentration. Comparison with permitted concentration according to hygiene standard. 15. Gas chromatography. Determination of caffeine derivatives in tea by gas partition chromatograhy GLC using CHROM 5 chromatograph (Laboratorní přístroje Praha, CR). 16. CE-LIF, capillary zone electrophoresis with laser-induced fluorescence detection. Optimization of the experimental setup. Determination of detection limit of rhodamine 6G. Separation of rhodamine dyes and labeled biological peptides. 17. MALDI TOF MS, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Instrument calibration and determination of molecular weight of selected analytes. Ccomparison of TOF analysis of peptides and proteins in linear and reflector modes. Peptide mass fingerprinting and identification of an unknown protein.
Literature
  • CHURÁČEK, Jaroslav. Nové trendy v teorii a instrumentaci vybraných analytických metod. Vyd. 1. Praha: Academia, 1993. 387 s. ISBN 8020000100. info
  • KANICKÝ, Viktor, Vítězslav OTRUBA, Lumír SOMMER and Jiří TOMAN. Optická emisní spektrometrie v indukčně vázaném plazmatu a vysokoteplotních plamenech (Optical emission spectrometry in inductiveky coupled plasma and high temperature flames). 1. st. Praha: Academia, 1992. 152 pp. Pokroky chemie 24. ISBN 80-200-0215-4. info
  • CHURÁČEK, Jaroslav. Analytická separace látek. 1. vyd. Praha: Státní nakladatelství technické literatury, 1990. 384 s. ISBN 80-03-00569-8. info
  • SOMMER, Lumír. Analytical absorption spectrophotometry in the visible and ultraviolet : the principles. Amsterdam: Elsevier, 1989. 310 s. ISBN 0-444-98882-38. info
  • Analytická příručka. Díl I [Zýka, 1988]. Edited by Jaroslav Zýka. 4. upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988. 678 s. info
  • Analytická příručka. Díl II [Zýka, 1988]. Edited by Jaroslav Zýka. 4. upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988. 831 s. info
  • Vysoká škola chemicko-technologická (Pardubice). Katedra analyti. Pokroky v teorii a instrumentaci moderních analytických metod. Edited by Jaroslav Churáček. 2. přeprac. a dopl. vyd. Pardubice: Vysoká škola chemicko-technologická, 1988. 193 s. info
  • HOLZBECHER, Záviš and Jaroslav CHURÁČEK. Analytická chemie [Holzbecher, 1987]. 1. vyd. Praha: Státní nakladatelství technické literatury, 1987. 663 s. info
  • SOMMER, Lumír. Analytická spektrometrie. 1. 1. vyd. Praha: Státní pedagogické nakladatelství, 1986. 173 s. info
  • KORYTA, Jiří. Současné trendy v elektrochemii. 1. vyd. Praha: Academia, 1986. 128 s. info
  • Nové směry v analytické chemii. Svazek II. Edited by Jaroslav Zýka. 1. vyd. Praha: Státní nakladatelství technické literatury, 1984. 218 s. info
  • BARTUŠEK, Miloš. Úvod do elektroanalytických metod. 1. vyd. Praha: SPN, 1984. 104 s. : i. info
  • CHURÁČEK, Jaroslav. Úvod do vysokoúčinné kapalinové kolonové chromatograrie. 1. vyd. Praha: SNTL - Nakladatelství technické literatury, 1984. 188 s. info
  • DVOŘÁK, Jiří and Jiří KORYTA. Elektrochemie [Dvořák, 1983]. 3. dopl. a rozš. vyd. Praha: Academia, 1983. 410 s. info
  • Nové směry v analytické chemii. Svazek I. Edited by Jaroslav Zýka. 1. vyd. Praha: Státní nakladatelství technické literatury, 1983. 199 s. info
  • CHURÁČEK, Jaroslav and Pavel JANDERA. Separace látek : kapalinová vysokoúčinná kolonová chromatografie. 1. vyd. Praha: SNTL - Nakladatelství technické literatury, 1981. 140 s. info
  • SOMMER, Lumír. Teorie a praxe vybraných optických analytických metod. 1. vyd. Praha: Státní pedagogické nakladatelství, 1978. 285 s. info
Teaching methods
laboratory courses
Assessment methods
Three close cycles of laboratory course: optical methods, electroanalytical methods, separation methods (+MALDI - MSTOF). Preliminary annoucement to lector is necessary. Graded credit requirements: completion of all laboratory exercises
Language of instruction
Czech
Further comments (probably available only in Czech)
The course is taught annually.
The course is taught: every week.
General note: dle oboru.
The course is also listed under the following terms Spring 2008 - for the purpose of the accreditation, Spring 2000, Spring 2001, Spring 2002, Spring 2003, Spring 2004, Spring 2005, Spring 2006, Spring 2007, Spring 2008, Spring 2009, Spring 2010, Spring 2011, Autumn 2011, Autumn 2011 - acreditation, Autumn 2012, Autumn 2013, Autumn 2014, Autumn 2015, Autumn 2016, autumn 2017, Autumn 2018, Autumn 2019, Autumn 2020.