Analytical Chemistry 1

Garant předmětu:

Vlastimil Vyskočil

Lecturer:

Tutor:

Anna Kubíčková, Vlastimil Vyskočil

Supervisor:

Department of Nuclear Chemistry

Synopsis:

Introduction, methods of analytical chemistry, scheme of analytical procedures. Sampling and preparation of Hample. Precipitation reactions, solubility product, factores influencing solubility. Gravimetry. Statistical evaluation of results. Precipitation titrations, titration curve, endpoint indication. Complex-formation reactions, stability constant, factors influencing stability of complexes. Chelatometric titrations, titration curve, endpoint indication. Qualitative analysis of cations and anions, application of precipitation and complex-formation reactions for separation and identification of ions. Acid-base reactions, acids, basis, acidity function, salts, hydrolysis of salts, buffers, acid-base indicators. Acid-base titrations, titration curves, detrmination of strong and weak acids, bases and salts. Acid-base reactions in nonaqueous solvents.

Requirements:

Knowledge of general chemistry on the level of a completed basic university course.

Syllabus of lectures:

1. Introduction. Definition of analytical chemistry. Basic terms (proof, identification, determination, characterization). Selective and specific reactions, analytical methods based on immunochemical and enzymatic reactions. Units for expression of content (concentration) of substances in analyzed samples and in reagent solutions (percentage, molar concentration). Preparation of solutions.

2. Analytical process - a basic plan.

3. Qualitative analysis. Identification of inorganic compounds (identification of cations and anions).

4. Identification of organic compound (identification of molecules), elemental analysis, mass spectrometry, nuclear magnetic resonance).

5. Sampling. Obtaining a representative sample. Basic differences in sampling of solid liquid and gaseous samples.

6. Dissolution and decomposition. Nondestructive analytical methods (activation analysis). Destructive analytical methods. Sample dissolution and decomposition (in acids, by melting, mineralization or pyrolysis).

7. Elimination of interferents (masking or separation methods). The nature of separation process (distribution ratio, distribution constant). Separation by precipitation. Extraction. Ion-exchange separations (cation-exchange resin, anion-exchange resin).

8. Measurement of analytical property - a survey of analytical methods (gravimetric methods, volumetric methods, electroanalytical methods, optical methods, separation methods) ant their general characterization. Chemical reactions, basic chemical equilibria.

9. Gravimetric analysis. Basic steps (sample preparation, precipitation -conditions for quantitative precipitation, errors in precipitations, filtration, drying and ignition of precipitates, weighing of precipitates). Gravimetric calculations. Weighing, types of (analytical) balances.

10.Volumetric analysis. Definition of some terms (standard solution, direct and indirect titration, equivalence point, end point, titration curve). Preparation of standard solutions (primary standards, secondary standards).Volumetric calculations. Measurement of volume.

11. Individual volumetric methods. Precipitation titrations (argentometry, standard solutions, indicators, examples of determination). Acid-base titrations (standard solutions, indicators, difference in titration of strong and weak acids and bases, titration curve, selection of indicator). Complex-formation titrations (titration with EDTA, indicators, effect of pH and complexity constant value). Oxidation/reduction titrations (redox potential, Nernst equation, redox titration curve, redox indicators, standard solutions for oxidation and reduction titrations, typical examples of redox determinations, e.g., water determination by K.Fischer titration).

Syllabus of tutorials:

1. Calculation of concentrations, dilution and mixing.

2. Precipitation equilibria, titrations and stochiometry.

3. Gravimetry stochiometry.

4. Complexing equilibria, titrations and stochiometry.

5. Use of precipitation reactions and their stoichiometry in practical tasks carried out in laboratory practice in analytical chemistry. Argentometry of potassium iodide and chloride. Potentiometric titration curve. Precipitation reactions used in qualitative analyses.

6. Use of complexation reactions and their stoichiometry in practical tasks carried out in laboratory practice in analytical chemistry. Chelatometry of cations in mixture using masking of cations. Colored complexes for spectrophotometric determination of analytes. Complex compounds used in qualitative analytical chemistry.

7. Use of acid-base reactions and their stoichiometry in practical tasks carried out in laboratory practice in analytical chemistry. Alkalimetry and acidimetry. Preparation of standard solutions. Cation exchanger and solid phase extraction.

8. Use of redox reactions and their stoichiometry in practical tasks carried out in laboratory practice in analytical chemistry. Iodometry with standard solutions of iodine and sodium thiosulfate. Permanganometry of iron ions. Potentiometric titration curve. Redox reactions in qualitative analytical chemistry.

9. Principle of coulometric titration. Faraday's law. Relation between the electric charge and the analyte amount. Potentiometry with ion selective electrode. Reference and indicating electrode. Ion selective electrode.

10. Principle of molecular spectrophotometry in UV/VIS region. Lambert-Beer law. Calibration curve. Principle of gas chromatography. Evaluation of chromatogram and calculation of fundamentals chromatographic quantities.

11. Statistics of experimental analytical results

Study Objective:

The course of analytical chemistry provides the students with the knowledge of the basic methods of analytical chemistry and schemes of analytical procedures.

The students will acquire competence to select independenty optimum analytical approach to the given problem.

Study materials:

Key literature:

1. Skoog D.A., West D.M., Holler F.J.: Fundamentals of Analytical Chemistry (6. edition), Saunders College Publishing, 1992 (ISBN 0-03-075397-X).

Recommended literature:

1. Christian G.D.: Analytical Chemistry (5. edition), John Wiley & Sons, New York, 1994 (ISBN 0-471-30582-0).

2. Kellner R., Mermet J.M., Otto M., Widmer H.M. (Editors): Analytical Chemistry, Willey-VCH, Weinheim 1998 (ISBN 3-527-28610-1).

Note:

Time-table for winter semester 2023/2024:

Time-table is not available yet

Time-table for summer semester 2023/2024:

Time-table is not available yet

The course is a part of the following study plans:

• BS Jaderná chemie (compulsory course of the specialization)
• Jaderná chemie (compulsory course in the program)