Analytical Chemistry (N-bBCH-013/15 and N-bENS-022/15)

Chemistry students will become familiar with the information about recent state of quantitative observation - measurement within the system of scientific cognition of material reality; about generation of analytical signal and classification of analytical principles and methods, about analytical process, principles, procedures and techniques; about approach to solution of identification problems, about characterization and quantification of chemical substances in science and technology. Students become familiar also with the possibility to reveal and search for solution of material based research, production and social practice with the aid of chemical analyses as tools of analytical chemistry. The objective involves also calculus in analytical chemistry and solution of model situation from social practice that are discussed in daily press and information media. Student will solve case tasks from biochemistry, biotechnology and the other natural sciences. Current use of analytical chemistry methods and their future potential and outline of their development trends will be discussed. The objective is taught in three forms. Theoretical aspects and calculus basics are taught in lectures and seminars, respectively. Inevitable part of the objective is also instrumental experimental work in the laboratory.

Syllabus

  1. Definition, matter of interest and resources of analytical chemistry. History of analytical chemistry in the context with society development. Relations of knowledge – signal – information dealing with fundamental aspects of material world around us. Method of scientific cognition; methodology of scientific work in analytical chemistry; observation, measurement, experiment, hypothesis, theory, correction functions in science. Relations of science and technology from the point-of-view of current possibilities of analytical chemistry. Trace analysis and microanalysis.
  2. Measurement. Analytical signal and its properties. Generation of analytical signal. Classification of analytical signals and noise. Comprehensive principles of measurement and evaluation of quality and quantity of chemical substances. Potential and restrictions of measurement and detection analytical methods.
  3. Classification of analytical principles according to selectivity, type and properties of analytical signal: qualitative tests and reactions, gravimetry, volumetry. Important chemical concepts, amount and concentration. Importance of quantity, units, measures and mass. International system of quantities (SI). Solutions and concentration.  Chemical stoichiometry . Solution of chemical equilibrium. Volumetry - titration. Some general aspects of volumetry.  Standard solutions. Calculus. Titration curves. Principles and analytical utilization of neutralization, precipitation, oxidation-reduction, complex forming titrations.
  4. Classification of analytical principles according to selectivity, type and properties of analytical signal – electroanalytical methods. Electrogravimetry: weighing of electrochemically deposited substance. Coulometric analytical methods. Voltamperometry. Polarography. Potentiometry: determination of ions and molecules concentration. General principles. Electrodes. Direct potentiometry, pH-metry, ion-selective electrodes. Potentiometric titrations. Conductometry and conductometric detection.
  5. Spectroscopic analytical methods, measurement of chemical substances by use of electromagnetic radiation (or light) properties. Interaction of radiation and mater. Atomic absorption spectroscopy. Instrumentation for measurement of light emission or absorption. Atomic emission spectrometers, spectrofluorimeters, UV-VIS photometers, spectrophotometers. Infra-red spectrometers. Analytical utilization of molecular and atomic spectroscopic methods. Analytical molecular fluorescence spectroscopy. Analytical methods based on light scattering by ions and molecules (ELSD, etc). Analytical applications of optical methods.
  6. Introduction to analytical separation methods. Classification of separation principles and methods. Masking and demasking reactions. Precipitation and filtration. Separation of volatile substances by distillation. Isolation and separation of substances by extraction. Ion-exchange.
  7. Chromatographic separation. Generalised outline of chromatography. Classification of chromatographic methods. Gas chromatography (GC) - principles. Instrumentation of gas chromatography. Carrier gas and auxiliary gas. GC columns and stationary phases.  Application of GC for chemical analysis of substances. High-performance liquid chromatography (HPLC). HPLC instrumentation. Separation mechanism: distribution , adsorption, ion-exchange, affinity based LC. Normal phase vs. reversed phase systems. Gel chromatography. Supercritical fluid chromatography (SFC).
  8. Electroseparation methods. Capillary electrophoresis vs planar techniques. Instrumentation. Basic principles of electrophoretic methods. Zone electrophoresis, isotachophoresis, isoelectric focusing. Application of capillary electrophoresis in chemical analysis.
  9. Mass spectrometry (MS) basic principles. Basic scheme of mass spectrometer. Variables and conditions of measurement by MS. Output signal of MS. MS instrumentation. Basic ionization techniques in MS. Identification and confirmation of identity. Automation of analytical methods in QC/QA laboratories. Application of combined techniques for solution of selected analytical problems.
  10. Automation in analytical laboratories. The combined application of analytical methods to solve selected analytical problems.
  11. Practical examples of analytical methods usage in procedures of chemical analysis for solution of actual practical problems I.
  12. Practical examples of analytical methods usage in procedures of chemical analysis for solution of actual practical problems II.
  13. Practical examples of analytical methods usage in procedures of chemical analysis for solution of actual practical problems III.
  14. Final thinking about new trends in analytical chemistry.

Course evaluation

    There will be two running written tests, each for 10 points, during the semester on seminars, in summary maximum 20 points. Only student obtaining from both tests minimum 50% will pass to final exam test. Experimental laboratory work will be graded as follows: continuous compounding will be evaluated by 20 points maximum involving theoretical preparation for laboratory work, activity and quality of results in the experimental work summarized in laboratory protocol. Final test from topics of laboratory will be enabled only to student who submitted protocols from all done laboratory experiments - student can get maximum 20 points, in summary max. 40 points for experimental laboratory work. Only those students will be admitted to final examination who achieve at least 50% of the points from seminar tests and laboratory work evaluation. Final exam related to lecture topics will consist of 40-point test. For clarification of boundary test results it is possible to require additional oral answer to the question for maximum 4 points included. Overall grade will consist of summary evaluation of final exam, seminar tests and experimental work according to formula (0.4 x % final exam) + (0.2 x % seminar tests) + (0.4 x % laboratory work) = resulting %. 

    Overall Course Evaluation

    92 - 100 % A
    84 - 91 % B
    76 - 83 % C
    68 - 75 % D
    60 - 67 % E
    0 - 59 % FX

    Laboratory exercises

    Laboratory experiments

    1. TITRATION METHODS
    2. OPTICAL METHODS
    3. CHROMATOGRAPHY METHODS
    4. ELECTROSEPARATION METHODS

    Suggested readings

    • Skoog, West , Holler , Crouch : Analytical Chemistry , An Introduction , 7th Edition, Thomson Learning, 2000, London, United Kingdom
    • Ján Labuda a kol., Analytická chémia, STU v Bratislave, 2014
    • Ján Labuda a kol., Príručka vybraných pojmov v analytickej chémii, STU v Bratislave, 2014
    • Poznámky z prednášok predmetu Analytical Chemistry.
    • G . Schwedt : The Essential Guide to Analytical Chemistry , Wiley , New York, 1997
    • P . Klouda , Moderní analytické metody , Nakl . P. Klouda Ostrava, 2.vyd. 2002
    • R . Kellner , J-M. Mermet , M. Otto , Analytical Chemistry , John Wiley & Sons Australia , Ltd , 2013
    • J . Lehotay ., Separačné metódy v analytickej chémii, STU v Bratislave, 2009
    • E . Plško , Všeobecná analytická chémia, 2 THETA, Český Těšín , 2011
    • J . Sádecká , A. Purdešová , Úprava vzorky v analytickej chémii, Slovenská technická univerzita v Bratislave, 2012
    • P . Májek ( Ed .), e-Analytická chémia, ÚACH FCHPT, STU v Bratislave, 2006
    • P . Tarapčík , Elektronická zbierka príkladov a úloh z analytickej chémie, ÚACH FCHPT, STU v Bratislave, 2006
    • Halko R. a Žemberyová : Atómová spektrometria a možnosti jej kombinácie s kvapalinovou chromatografiou , Kartprint , Bratislava, 2010

    Grading policy

    • ak študent príde na cvičenie nepripravený (VP UK č.8/2015, Článok 15, odsek 3, písmeno g a Článok 24, odsek 4) alebo v priebehu cvičenia sa bude chovať neadekvátne (VP UK č.8/2015, Článok 15, odsek 3, písmeno h), poruší bezpečnosť pri práci a ohrozí tým svoje zdravie alebo zdravie svojich kolegov (VP UK č.8/2015, Článok 47), vyučujúci ho môže vylúčiť z cvičenia bez nároku na náhradné odcvičenie úlohy
    • študent musí absolvovať všetky laboratórne cvičenia (VP UK č.8/2015, Článok 21, odsek 9),
    • v prípade neúčasti študenta na cvičeniach, musí študent dokladovať dôvod svojej neúčasti, inak mu vyučujúci nemusí uznať zápočet a študent následne nebude pripustený ku skúške (VP UK č.8/2015, Článok 21, odsek 9 a Článok 24, odsek 4),
    • ak študent vymešká cvičenie a vyučujúci uzná jeho dôvody ako opodstatnené, docvičovanie úloh resp. získanie bodov stratených kvôli neúčasti sa bude riešiť individuálne na základe okolností a písomnej dohody medzi študentom a vyučujúcim (VP UK č.8/2015, Článok 21, odsek 9),
    • študenti majú nárok na jeden náhradný termín (spravidla v 13. týždni semestra), počas ktorého si môžu docvičiť vymeškané úlohy (okrem prípadov menovaných v prvom bode) (VP UK č.8/2015, Článok 21, odsek 9).
    • študent je povinný nahlásiť ešte pred absolvovaním cvičenia každú skutočnosť, ktorá by mohla ohroziť bezpečnosť a zdravie ľudí v laboratóriu alebo spôsobiť materiálne škody (VP UK č.8/2015, Článok 15, odsek 3, písmeno b a Článok 47)
    • ak študent vymešká viac ako jeden seminár bez dôveryhodného dokladovania dôvodu neúčasti, vyučujúci mu nemusí uznať zápočet a študent následne nebude pripustený ku skúške,
    • ak niektorý seminár alebo cvičenie odpadnú v dôsledku sviatkov alebo dekanského/rektorského voľna, body získateľné za tieto aktivity sa odpočítajú z maximálneho počtu bodov a percentuálna úspešnosť študenta sa vypočíta pomocou zníženého maximálneho počtu dosiahnuteľných bodov.

    Ostatné problémy sa budú riešiť v zmysle Študijného poriadku UK v Bratislave zverejneného na webovej stránke fakulty.