Course unit code:
N418I0_4B
Course unit title:
Instrumental Methods in Analysis
Mode of delivery, planned learning activities and teaching methods:
lecture – 2 hours weekly (on-site method)
seminar – 2 hours weekly (on-site method)
Credits allocated:
4
Recommended semester:
Biotechnológia – bachelor (full-time, attendance method), 5. semester
Chemical Engineering – bachelor (full-time, attendance method), 5. semester
Potraviny, výživa, kozmetika – bachelor (full-time, attendance method), 5. semester
Automation, Information Engineering and Management in Chemistry and Food Industry – bachelor (full-time, attendance method), 5. semester
Level of study:
1.
Prerequisites for registration:
none
Assesment methods:
Students will write 3 tests during the semester, together they can earn 24 points as bonus point to the exam. The exam comprises 2 different tests, together with 98 points. For succesful passing the exam 50 % from each test is neccessary.
Learning outcomes of the course unit:
The students know the principles of analytical experimental methods and the basics of complex instrumentation, that are used to obtain the information on real objects chemical composition, including its time variation and its spatial distribution. They can handle basic electroanalytical, chromatographic and spectrometric methods and measurement techniques, including the mesaurement processing and deriving the final results, with characteristics of qualitative and quantitative analysis. They know the applications of analytical methods for the analysis of biological systems, the foods samples, environmental samples, technology samples, and for the process control.
Course contents:
1. Basic concepts and terms of analytical chemistry, the basics of evolution of analytical signal, priciples and use of instrumental methods of analysis. Electroanalytical, spectral and chromatographic methods of analysis, the overview of other methods. (allowance 2/2)
 
a. General aspects of analytical chemistry. The subject of analytical chemistryl. Analytical process as a concept of obtaining the analytical information. The classification and selection of analyticla methods. Qualitative requirements on chemical analysis. The basic rules of sampling, the ucertainty of sampling. The sample preparation. Analytical chemical measurements, the principles of analytical measurement. Signals in analytical chemistry. The characteristics of detectors. The signal and noise.
b. The tracing of measurements, adjusting, calibration and verification, regression and calibration with corresponding uncertainties, reference materials, standard sample, addition methods. The result of measurement (the accuracy, precision, errors and uncertainties of measuremen results). The evaluation of analytical information, information of quantitative analysis. The quality assurance in analytical chemistry, accreditation. Good laboratory praxis. Validation of methods. Statistical quality control. Analytical chemistry in technology and praxis.
c. Physical and physicochemical procedures for obtaining the analytical information. Electrochemical interactions as a basis of analytical signal. Electrochemical analytical methods, basic terms. Measurement of electrical quantities in chemical laboratory. Conductometry, Potentiometry - direct measurement of pH, pX. Potentiometric titrations. Addition methods. Potentiometric detectors.
d. Electrolysis and electrochemical reactions. Polarisation I-E curves. Electrogravimetry, coulometry with controlled potential, coulometric titrations. Voltammetry with constant surface area electrodes. Electrolysis under voltammetric conditions. Polarography, methods. Cyclic voltammetry. Sensitivity enhancement in voltammetry. Electrochemical stripping analysis. Voltammetric titrations. Amperometric and biamperometric titrations. Potentiometric titrations with polarised electrodes.
e. Chromatographic analysis - general aspects. The principles of separation of compounds, basic terms, the classification of chromatographic methods. Chemical interactions as a basis of chromatographic separation. The partitioning, adsorption, ionic, gel and affinity chromatography. Chromatogram, retention characteristics, retencion indexes. The peak pattern, the theory of chromatographic process, equations, resolution, separation efficiency.
f. The column chromatography. Experimental, qualitative and quantitative analysis. Liquid chromatography. Mobile and stationary phases. Sample introduction systems, detectors.
g. Gas chromatography, mobile and stationary phases, samplers. Temperature programs. Analytical use.
h. Thin layer and paper chromatography, stationary and mobile phases, the chromatogram deriving and evaluation, analytical use. Electromigration methods, electrophoresis, isotachophoresis, analytical use. The combined separation methods.
i. Interaction of electromagnetic radiation with analyte and the types of analytical signals. Emision of electromagnetic radiation as analytical information. Atomic emision spectrometry. Flame fotometry. ICP. Multielement spectral analysis. Luminescent analysis. Atomic fluorescence. Spectrometry of X-rays, Auger electron spectrometry, fotoelectron spectrometry, atomic mass spectrometry.
j. Analytical methods based on absorption of electromagnetic radiation. Atomic absorption spectrometry. Molecular absorption spectrometry (UV/VIS). Infrared spectrometry, Raman spectrometry. Absorption of electromagnetic radiation under concurent effect of magnetic field, NMR and EPR spectrometry. Mass spectrometry of organic compounds. The combination of methods of molecular spectrometry.
k. Analytical methods based on light scattering. Turbidimetry and nefelometry. Chiroptical methods - polarimetry and spectropolarimetry. Refractometry and interferometry. Radioanalytical methods, activation analysis.
l. Bioanalytical methods. Flow analysis, combined methods. Obtaining the analytical information for technology, process analysis. The specific application of analytical chemistry in praxis - clinical analysis, environmental analysis (water, sludge, sediment, soil analysis, atmospheric pollution analysis), foods analysis, analysis for metal processing and inorganic amd organic technology.

Recommended or required reading:
Basic:
  • GARAJ, J. – HLADKÝ, Z. – LABUDA, J. Analytická chémia I. Bratislava : STU v Bratislave, 1996. 188 p. ISBN 80-227-0838-0.
  • BUSTIN, D. Analytická chémia II. Bratislava: STU v Bratislave, 1996. 213 p. ISBN 80-227-0885-2.
  • TARAPČÍK, P. Zbierka príkladov z analytickej chémie. Bratislava : STU v Bratislave, 1995. 253 p. ISBN 80-227-0777-5.
  • TARAPČÍK, P A K. Analytická chémia: Seminárne cvičenia - riešené príklady. Bratislava : STU v Bratislave, 2001. 145 p. ISBN 80-227-1469-0.
  • PURDEŠOVÁ, A. Praktikum z analytickej chémie. Bratislava: STU, 2011. 242 p. ISBN 978-80-227-3555-1.
Recommended:
  • Labuda, J. a kol, Analytická chémia, Bratislava, STU v Bratislave, 2014
Language of instruction:
Slovak, English
Assessed students in total:
206

A 28.6 %

B 19.4 %

C 18.4 %

D 16.5 %

E 14.1 %

FX 3 %

Course supervisor:
doc. Ing. Eva Benická, CSc.
Last modification:
16. 1. 2018

Department:
Department of Analytical Chemistry

AIS: 2018/2019   2017/2018  

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