Analytical Chemistry

Students will get acquainted with the current state of quantitative observation; generation of analytical signal; analytical processes, principles, procedures and techniques and their classification; solving identification problems; and characterization and quantification of chemical substances in science and technology. Students will also get acquainted with the possibility of detecting and finding solutions to materials research, production and social practice using chemical analysis as a tool of analytical chemistry. Students will also get acquainted with instrumental experimental work in the laboratory.

Syllabus

• Definition, subject of interest and resources of analytical chemistry.
• Relationship between analytical chemistry and chemical analysis. Analytical method (classification). Analytical principle. Sampling.
• Measurement (qualitative and quantitative analysis). Analytical signal and its properties. Calibration. Statistical evaluation of data (measurement errors).
• Simple sample preparation procedures. Decomposition of inorganic and organic samples, extraction.
• Chemical methods of analysis (qualitative, quantitative). Evidence of chemical reactions and tests, gravimetric analysis, volumetric analysis. Titration curves. Principles of neutralization, precipitation, redox and complexometric titrations.
• Chemical equilibria (acid-base, complex-forming, precipitating, redox).
• Electroanalytical methods. Basic scheme of electrochemical cell. Classification of electroanalytical methods. Equilibrium potentiometry (reference and indicator electrodes, direct potentiometry and potentiometric titrations, ion-selective electrodes as a selectivity coefficient). Principle and use of linear and cyclic voltammetry, coulometry and conductometry.
• Optical analytical methods. Properties of electromagnetic radiation. History and classification of optical methods. Basic instrumentation of optical analytical methods. Atomic spectrometry. Atomic spectrometry techniques.
• Molecular spectrometry. Molecular spectrometry techniques – absorption UV-VIS spectrophotometry, spectrofluorometry, infrared and Raman spectrometry. Non-spectral optical methods. Reflectometry, interferometry, polarimetry, turbidimetry and nephelometry.
• Mass spectrometry. Basic principles. Basic scheme of equipment. Measurement conditions. Instrumentation in mass spectrometry. Basic types of ionization techniques and ion sources.
• Separation techniques, their function and importance in analytical procedures. Classification of separation principles and methods. Precipitation and filtration. Separation of volatile substances by distillation. Isolation and separation of substances by extraction. Ion-exchange. Chromatographic separation. Classification of chromatographic methods. Gas chromatography – principles and instrumentation. High-performance liquid chromatography – principle and instrumentation. Electroseparation methods. Capillary electrophoresis vs planar techniques. Instrumentation. Basic principles of electrophoretic methods: zone electrophoresis, isotachophoresis, isoelectric focusing.
• Automation in analytical laboratories. The application of combined analytical methods to solve selected analytical problems.

   

  Practicals

• Volumetric analysis. Determination of calcium and magnesium in water
• Potentiometric analysis. Determination of acetic acid in fermented spirit vinegar.
• Optical analytical methods. Determination of calcium and sodium in mineral water by emission flame photometry. Spectrophotometric determination of copper in the water. Identification and quantification of synthetic dyes by molecular absorption spectrometry.
• Chromatographic separation methods. Determination of methanol in alcoholic beverages by GC. RP-HPLC separation of aromatic hydroxycompounds and gallic acid. Separation of water-soluble dyes by paper chromatography.
• Electroseparation methods. Isotachophoretic separation of synthetic dyes using column-coupling technique. Isotachophoretic determination of glutamate in food.

Course evaluation

• Biological Chemistry:
  Lecture – a maximum of 50 points, for the final test.
  Practicals – a maximum of 50 points, for theoretical preparation for practicals and active participation in practicals (5 points), lab reports from practicals (35 points) and final test from practicals (10 points). In case of late submission of lab reports, the maximum number of points for the lab report will be reduced by 25% (late submission by 8-14 days), by 50% (late submission by 15-21 days), by 75% (late submission by more than 21 days).
  The final grade will consist of evaluation of the final test from lecture and practicals.
• Environmental Studies:
  Lecture – a maximum of 40 points, for the final test.
  Seminar – a maximum of 20 points, for elaboration and presentation of a seminar paper.
  Practicals – a maximum of 40 points, for theoretical preparation for practicals and active participation in practicals (4 points), lab reports from practicals (28 points) and final test from practicals (8 points). In case of late submission of lab reports, the maximum number of points for the lab report will be reduced by 25% (late submission by 8-14 days), by 50% (late submission by 15-21 days), by 75% (late submission by more than 21 days).
  The final grade will consist of evaluation of the final test from lecture, seminar, and practicals.

Overall Course Evaluation

Laboratory practicals

• Titration Methods
  B1T1 Determination of calcium and magnesium in water
  B1T2 Determination of acetic acid in fermented spirit vinegar
• Optical Methods
  B2T1 Determination of calcium and sodium in mineral waters by emission flame photometry
  B2T2 Molecular spectrophotometry. The spectrophotometric determination of copper in the water
• Chromatography Methods
  B3T1 Determination of methanol in alcolohic beverages by gas chromatography
  B3T3 Separation of water-soluble dyes by paper chromatography
• Electroseparation Methods
  B4T1 Isotachophoretic separation of synthetic dyes using column-coupling technique
  B4T2 Isotachophoretic determination of glutamate in food

Suggested readings

• D.A. Skoog, F.J. West, F.J. Holler, S.R. Crouch: Analytical Chemistry. An Introduction, Saunders Coll. Publ., 2000.
• G. Schwedt: The Essential Guide to Analytical Chemistry, Wiley, New York, 1997.
• R. Kellner, J.M. Mermet, M. Otto, Analytical Chemistry, John Wiley & Sons Australia, 2013.
• Notes from Analytical Chemistry lectures.