|
|
|
||
|
Last update: prof. RNDr. Vlastimil Vyskočil, Ph.D. (27.02.2024)
Sampling and preparation of sample 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 In the scope of the Seminar training in basic calculations used in analytical chemistry (gravimetry; precipitation, complexation, acid-base and redox equilibria) is realized. Learning Outcomes: Upon completion of the course, the student will: 1. Explain the basic concepts of chemical analysis, the process of analysis, expression of concentration. Define the following issues: analytical chemistry – science, chemical analysis – activity, qualitative and quantitative analysis. Explain the basic concepts: evidence, identification, determination, characterization, their informational value. Explain the processes of information acquisition: sensory observation, objective observation – instrumentation, acquisition of information directly and as a result of interaction. Explain types of interactions: non-selective, selective, specific (enzymatic and immunochemical reactions). Explain basic concentration units: percent, ppm, ppb (mass, volume), molarity, explain the preparation of solutions by dilution. 2. Explain chemical equilibria, requirements for chemical reactions. Explain the basic chemical equilibria – ionic product of water, solubility product, acid-base equilibria, equilibria in solutions of complexes, redox equilibria, partition equilibria. Describes real solutions – activity coefficient, effect on chemical equilibrium. Defines requirements for chemical reactions useful in analytical chemistry. 3. Explain qualitative analytical chemistry – inorganic analysis. Define the process of analysis – general outline. Describes orientation tests: description, pH-reactions, solubility, gas evolution in reaction with acid, flame tests. Explain selective (group) reactions – analytical classes of cations and anions. Describe specific reactions, examples of proof reactions and how to perform them. 4. Explain qualitative analytical chemistry – organic analysis. Defines the process of analysis – general outline. Describes the differences in methodology between inorganic and organic qualitative analysis. Explain the scheme of classical analysis of organic substances: uniformity tests, molecular analytical methods, elemental analytical methods, structural analytical methods. It will explain the instrumental methods of identification of organic substances – elemental analysis, mass spectrometry, nuclear magnetic resonance spectrometry. 5. Explain the sampling of gaseous, liquid and solid substances. Define the general principles of sampling. Describes the specifics of sampling gaseous (discrete samples – gas pipette, continuous sampling – sampling apparatus), liquid (single and serial sampling, plain and mixed samples, sample stability) and solid (heterogeneity of substances, sample crushing and splitting, soil sampling). 6. Explain non-destructive and destructive analytical methods, dissolution and decomposition of samples. Describe non-destructive analytical methods, the principle of activation analysis. Describe destructive analytical methods – dissolution (in water) and decomposition of samples (by acids, fusion, sintering, wet path mineralization, dry path – pyrolysis), mineralizers. 7. Explain elimination of interferents, separation methods and their efficiency. Describe the elimination of interferents by chemical means (masking) and physical separation (separation). Explain separation methods: separation by principle (by type of contact phase and analyte phase) and by experimental set-up (discrete separation, in-flow separation), separation efficiency (distribution ratio, distribution constant). 8. Explain the extraction. Describe extractions (liquid/liquid, liquid/gas, liquid/solid, supercritical fluid extraction). Explain ion-exchange separations (catex, anex, ion exchange, ion exchange regeneration, packed and column methods). 9. Explain weighing analysis (gravimetry). Define the basic steps of analysis: sample preparation, precipitation (quantitative precipitation conditions), precipitate maturation (precipitate properties), washing and filtration, drying and annealing, weighing of precipitate, calculation of concentration (gravimetric factor). 10. Explain volumetric analysis (volumetry) – principle, equivalence point, indications, titration curves. Describe titration: determination procedure, determination of the end point of titration (subjective and objective methods, equivalence point vs. end point of titration), titration curves (sigmoidal, linear), calculation of analyte content from titration data. Describe the preparation of volumetric solutions: from primary standards, from non-standard substances, standardisation of volumetric solutions (factor). 11. Explain precipitation and acid-base titrations. Define types of volumetric determinations. Describe precipitation titrations: argentometry, volumetric solutions, indicators, typical examples of determinations, titration curves. Describes acid-base titrations: volumetric solutions, indicators, strong and weak acid (base) titrations, titration curves, indicator selection; titrations in non-aqueous media. 12. Explain complexometric and redox titrations. Define types of titration determinations. Describe complexometric titrations: chelaton titration (effect of pH and complexity constant on the course of determination), indicators, typical examples of determinations (metal ions, water hardness). Describes redox titrations: overview of basic reagents for redox titrations, titration curves, indicators, typical examples of determinations. |
|
||
|
Last update: doc. RNDr. Karel Nesměrák, Ph.D. (28.10.2019)
• Opekar F. a kol.: Základní analytická chemie, skripta, UK, Karolinum, Praha 2002 a 2010. |
|
||
|
Last update: RNDr. Jan Fischer, Ph.D. (17.03.2022)
The course-unit credit is awarded on condition of having successfully passed a written test in a compulsory lecture seminar. Detailed information and study materials for the seminar are in Moodle: https://dlcv.cuni.cz/course/view.php?id=329 |
|
||
|
Last update: FORSTOVA/NATUR.CUNI.CZ (05.04.2013)
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).
Seminar's Syllabus: 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 |