Instrumental Analysis A 1200-1ANALINSAW4
The main stages of analytical procedure. Preparation of samples, type of analytical errors, main methods of analytical measurements. Instrumental signals used in analytical measurements. Absolute and comparative analytical methods.
Spectroscopic methods: molecular spectroscopy in UV/Vis and IR ranges, molecular luminescence methods, atomic absorption and emission spectroscopy.
Electrochemical methods: conductometry, potentiometry, and electrogravimetry, polarography and voltammetry.
Theoretical backgrounds of chromatographic methods, liquid and gas chromatography. Capillary electrophoresis.
Type of course
After finishing the course student:
- is acquainted with theoretics backgrounds and possibilities of application of selected common instrumental methods of chemical analysis,
- is able to indicate the main fields of application oif those methods,
- is able to indicate the limitations of discussed analytical methods.
The effects of learning will be verified by examination obeying the following problems:
1. General problems: Phenomena and properties of matter utilized in chemical analysis. Basic terms: analyte, analysis, determination. Instrumental signals employed in chemical analysis. Criteria of selection of analytical methods. Parameters characterizing the analytical method: accuracy, precision, sensitivity, selectivity, limit of detection. Microanalysis and trace analysis. Errors in analytical determination. Basic methods of analytical measurement: calibration curve method, standard addition, use of internal standards.
2. Spectroscopic methods of analysis: Ranges of electromagnetic radiation and its interactions with matter. Molecular spectroscopy. Changes of energy of molecules as effect of UV. visible and infrared irradiation. Chromophores. Laws of absorption of radiation. Fundamental, chemical and instrumental deviations from the law of absorption. Quantitative measurements in UV/Vis range.Absorption spectroscopy in the infrared range. Ranges of IR radiation, oscillation spectra. Application in identification of molecular structure. Detection in elemental analyzers and gaseous analytes.
Luminescence spectroscopy. Fluorescence and phosphorescence. Fluorimetric determination of trace metals.
Atomic spectroscopy. Ionization methods employed in atomic absorption spectroscopy. Thermal and optical methods of excitation. Sources of radiation. Interferences in AAS measurements. Methods of atomic emission.
3. Electroanalytical methods: Basic concepts of electrochemistry in solutions. Electrode processes. Potential of electrode. Type of currents in electrochemical cell. Conductometry: direct measurements. Conductometric tittration. Potentiometry: Indicating and reference electrodes. Nernst and Nikolsky-Eisenman equations. First and second kind electrodes. Ion-selective membrane electrodes. Measuring methods used in potentiometry. Potentiometric titrations.
Electrogravimetry: Faraday laws. Conditions of electrolysis. Applications of electrogravimetry.
Voltammetric methods: Three electrode measuring cell. Method of polarization of working electrode. Direct current voltammetry. Polarography, main advantages of dropping mercury electrode. Limiting and residual currents. Pulse polarography and voltammetry. Electrochemical stripping methods (inverse voltammetry).
4. Chromatographic methods: Chromatographic process. Retention, retention coefficient. Column and planar chromatography. Molecular interaction utilized in chromatography. Parameters describing chromatographic separation. Selectivity coefficient, resolution, efficiency of separation. Theoretical plate concept. Van Deemter equation. Gas chromatography. Partition and absorption chromatography. Type of columns. Detectors in gas chromatography. Liquid chromatography. Normal and reversed phase systems. Isocratic and gradient elution. Stationary phases in liquid chromatography. Detectors in liquid chromatography. Fundamentals of capillary electrophoresis.
Professional training outside of the University is not needed to complete this course.
W. Szczepaniak, Metody instrumentalne w analizie chemicznej, PWN, Warszawa 2002 (Wyd.IV), 2005 (Wyd.V).
Information on level of this course, year of study and semester when the course unit is delivered, types and amount of class hours - can be found in course structure diagrams of apropriate study programmes. This course is related to the following study programmes:
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