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Classical Analytical Methods

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Course Unit Code617-2006/02
Number of ECTS Credits Allocated4 ECTS credits
Type of Course Unit *Compulsory
Level of Course Unit *First Cycle
Year of Study *First Year
Semester when the Course Unit is deliveredSummer Semester
Mode of DeliveryFace-to-face
Language of InstructionCzech
Prerequisites and Co-Requisites Course succeeds to compulsory courses of previous semester
Name of Lecturer(s)Personal IDName
BAR57doc. Mgr. Lucie Bartoňová, Ph.D.
Summary
Lectures of Classical Analytical Methods are focused to description of fundamental theory, principles, calculations, sample preparation and utilization of gravimetric and titrimetric analytical methods. Calculation of typical exercises is trained during calculation seminars; practical skills needed for analytical measurements are obtained during laboratory classes.
Learning Outcomes of the Course Unit
Subject objectives:
- to provide survey of classical analytical methods,
- to describe principles of individual analytical methods,
- to describe technique of sample preparation prior to analysis itself,
- to use fundamental procedures of analytical calculations,
- to perform analytical measurements in laboratory,
- to assess practical possibilities of utilization of individual analytical methods (advantages and drawbacks).

Acquired knowledge:
- to characterize fundamental terms, variables and units used in analytical chemistry,
- to define fundamental methods in analytical chemistry,
- to characterize basic procedures of samples preparation prior to analysis itself,
- to characterize principles, advantages and drawbacks of individual methods of classical analytical chemistry.

Acquired skills:
- capability to perform fundamental analytical calculations for classical analytical methods,
- capability to perform practical analytical measurements in laboratory (using gravimetric and titration methods),
- capability to chose suitable analytical method for derermination of given analyte.
Course Contents
Lectures
1. Introduction, fundamental terms, survey of analytical–chemistry methods, variables and units, fundamental analytical calculations, analytical method and procedure, normalization in analytical chemistry, reference materials

2. Reaction kinetics, reaction rate, rate constant, Arrhenius equation, catalysis and autocatalysis, reactions of first, pseude-first and second order, Gibb´s free energy, enthalpy and entropy, chemical equilibria, equilibrium constant, activity, activity coefficient, ionic strenth of solution

3. Neutralization equilibria: acid - base theory, weak and strong acids and bases, buffers, salt hydrolysis, fundamental calculations

4. Complex – formation equilibria: complex types, utilization of complexes in analytical chemistry, stability constant, conditional stability constant, fundamental calculations

5. Precipitation equilibria: solubility product, solubility, solubility examples of some compounds and utilization in analytical chemistry, fundamental calculations

6. Redox equilibria: Electrochemical potential and its calculation, Peters equation, Nernst equation, examples of some important redox systems and its utilization in analytical chemistry, fundamental calculations

7. Evaluation of analytical results – normal distribution, tests for outlying results, precision and acuracy of results and corresponding tests, reference materials, confidence interval, characteristics of analytical methods

8. Sample collection (gaseous, liquid and solid samples), sample preparation prior to analysis and their preconcentration (extraction liquid / liquid phase, liquid/solid phase etc.), sample decomposition, conservation, applications

9. Volumetric analysis – titration curve, equivalence point and its detection, standardization of volumetric solutions, titration types. Neutralization titration: titration of strong acids with strong bases, titration of weak acids and weak bases, calculation of titration curves, indicators and its selection for given reaction, alcalimetry and acidimetry, practical examples

10. Complex-fromation titrations (mercurimetry, chelatometry), titration agents, indicators, effect of pH, titration curve calculations, direct and back titrations, practical examples of utilization

11. Precipitation titrations: argentometry, indication of equivalence point, utilization in analytical praxis. Gravimetry: gravimetric factor, precipitate formation, effect of pH, postprecipitation, filtration and rinsing of precipitates, drying and calcination, organic agents, practical examples

12. Separation methods in classical analytical chemistry: distillation, rectification, sublimation, extraction liquid / liquid phases, ionic exchange, adsorption on various adsorbents, preparational chromatography (column and thin-layer), applications

13. Fundamentals of qualitative analytical chemistry – separation of inorganic anions and cations, groups of cations and anions, verification reactions, elemental analysis (O, C, N and H)

14. Practical examples of analyses of silicates, steel and iron, slags, effluents, fuels etc. Sample collection, decomposition, titration and gravimentic analyses and evaluation of analysis results

Theoretic/calculation classes
1. Fundamental variables, units, mutual relations
2. Analyte content in solution / solid / gaseous sample
3. Mixing of solutions
4. Gravimetry
5. Volumetric analysis (titrations)
6. Volumetric analysis (titrations)
7. Test
8. pH – strong acids and bases
9. pH – weak acids and bases
10. Solubility product
11. Redox potential – fundamental variables and equations
12. Redox potential – effect of oH, equivalence point
13. Quantification and evaluation of analytical results
14. Test

Laboratory classes
1. Safety precautions, organization of laboratory classes, fundamental instructions of analytical glassware, procedures and equipment
2. Fundamental analytical precedures – callibration of pipette / byurette
3. Gravimetric determination of nickel
4. Gravimetric determination of iron
5. Gravimetric determination of calcium
6. Alkalimetric determination of H3PO4,
Cerimetric determination of K4[Fe(CN)6] content
7. Determination of Mn in steel by means of VIS - spectrometry,
Determination of Mn in steel by means of redox titration
8. Alkalimetirc determination of calcium carbonate content in limestone, Alkalimetric determination of boric acid content
9. Chelatometric determination of calcium and magnesium,
Chelatometric determination of aluminium using back titration
10. Determination of neutralizing capacity of water,
Determination of chemical oxygen demand using KMnO4
11. Chelatomeric determination of Bi and Pb,
Mercurimetric determination of choride ions
12. Argentometric determination of chloride ions,
Iodometric determination of iodate ions
13. Determination of iron in iron ore using potassium permanganate titration,
Gravimetric determination of loss on ignition of limestone
14. Finishing operations, missing measurements, test reparation
Recommended or Required Reading
Required Reading:
CHRISTIAN, Gary D. Analytical chemistry. 5th Ed., New York: John Wiley and Sons, 1994. ISBN 0471597619.
BENÁTSKÁ, Ludmila. Výpočty v analytické chemii. Ostrava: VŠB - Technická univerzita Ostrava, 1999. ISBN 80-7078-676-0.
KLIKA, Zdeněk a Petr PRAUS. Analytická chemie I. Ostrava: VŠB - Technická univerzita Ostrava, 2002. ISBN 80-248-0164-7.
CHRISTIAN, Gary D. Analytical chemistry. 5th Ed., New York: John Wiley and Sons, 1994. ISBN 0471597619.
Recommended Reading:
DE LEVIE, Robert. Aqueous acid-base equilibria ans titrations. Oxford: Oxford University Press, 1999. ISBN: 9780198506171.
VOHLÍDAL, Jiří, Alois JULÁK a Karel ŠTULÍK. Chemické a analytické tabulky. Praha: GRADA Publishing, 1999. ISBN: 978-80-7169-855-5
Studijní opora: http://katedry.fmmi.vsb.cz/Opory_FMMI/617/617-Bartonova-Vypocty-rovnovaznych-stavu.pdf
DE LEVIE, Robert. Aqueous acid-base equilibria ans titrations. Oxford: Oxford University Press, 1999. ISBN: 9780198506171.
Planned learning activities and teaching methods
Lectures, Tutorials, Experimental work in labs
Assesment methods and criteria
Task TitleTask TypeMaximum Number of Points
(Act. for Subtasks)
Minimum Number of Points for Task Passing
Credit and ExaminationCredit and Examination100 (100)51
        CreditCredit45 20
        ExaminationExamination55 10