C3100 Analytical Chemistry I

Faculty of Science
Autumn 2004
Extent and Intensity
2/0/0. 2 credit(s) (fasci plus compl plus > 4). Type of Completion: zk (examination).
Teacher(s)
prof. RNDr. Josef Havel, DrSc. (lecturer)
prof. RNDr. Přemysl Lubal, Ph.D. (lecturer)
Guaranteed by
prof. RNDr. Josef Havel, DrSc.
Chemistry Section – Faculty of Science
Timetable
Wed 12:00–13:50 02004
Prerequisites (in Czech)
Předpokladem je absolvování základních přednášek z Obecné chemie (C1020), Anorganické chemie I (C1061), Anorganické chemie II (C2062), Organické chemie I (C2021), Organické chemie II (C3022) a příslušných laboratorních cvičení z těchto předmětů.
Course Enrolment Limitations
The course is also offered to the students of the fields other than those the course is directly associated with.
fields of study / plans the course is directly associated with
Course objectives
A systematic treatment of the basic principles of analytical chemistry for students of chemistry - part I. The course includes qualitative analysis, gravimetric analysis, and titrimetry.
Syllabus
  • I. Introduction into subject Analytical chemistry. Definition of basic terms. Definition of analytical chemistry a its position in chemistry and society. Terms: sample, analyt, matrix, method sensitivity. Standards and reference materials. Sampling, analytical methods and procedures. Foundations of Good Laboratory Practice (GLP) and analysis evaluation. Standard deviation of analysis and their determination.
  • 1. Protolytic reactions in aqueous solutions : acids, bases, water as solvent, autoprotolysis of solvent, constants, calculations of proton concentration in solutions of acids, bases and salts, graphical description of acid-base equilibria.
  • 2. Complex formation equilibria : stepwise formation of complexes in solutions, graphical and numerical description of complex formation equilibria, equilibrium constants and stability constants, examples of complex formation equilibria (complexes of ammonia, cyanide, thiocyanate, iodide), cation and anion hydrolysis, chelates of metals and non-metals, organic analytical reagents. Side equilibria in solutions, conditional stability constants and their analytical importance.
  • 3. Precipitation reactions : solubility and solubility product, conditional solubility product - influence of side reactions in solutions, substitution precipitation, converse of precipitates, examples of low soluble hydroxides, sulphides, sulphates, halides, chromates, oxalates, 8-hydroxychinolinates, etc.
  • 4. Redox equilibria : description of redox reactions and the types, standard and conditional potential, influence of formation of precipitates and complexes in solution, influence of pH, redox disproportionation, examples of oxidising and reducing agents in aqueous solutions.
  • 5. Principles of quantitative inorganic chemical analysis. Group and selective reactions. Examples of group precipitating agents, group reduction and oxidation, group characterisation of anions. Selective agents, origin of analytical selectivity. Importance of masking of element ions, masking agents.
  • 6. Gravimetry. Processes during precipitation and their influence on gravimetric analysis, contamination of precipitates, processes on precipitates, analytical balance and weighing, some basic operations in gravimetry : filtration and filter washing, drying, ignition, termogravimetry, examples of gravimetric procedures : methods based on AgCl, BaSO4, and hydroxide formation, SiO2 determination, organic agents in gravimetry, precipitation from homogenous solutions, gravimetric calculations, errors in gravimetric determination.
  • 7. Titration methods (volumetric analysis). Kinds of titrations, explanation of titration curves of all titration types, relation between inflection point (end of titration) and equivalence point, slope of curve and buffer range, titration calculations, primary standards in volumetry, evaluation of characteristic points on curves. Basic operations and aids in volumetry.
  • 8. Precipitation titrations. Explanation of titration curves, estimate of equivalence point, problems joined with indication of equivalence point, titration solutions and primary standards, origin of titration errors. Argentometric titrations : titration curves and their interpretation, interpretation of logarithmic diagrams during precipitation of AgCl, AgBr, AgI, Ag2CrO4, titration curves of mixtures Cl-, Br-, I-; titration errors for each equivalence point, determination Ag+ by NaCl solution without indicator, titration in presence of chromate as indicator, titration in presence of adsorption indicator, titration Ag+ by SCN- solution a indirect Br-, I-, SCN- determination, argentometric titration in presence of redox indicator; iodide titration by Ag+ solution in presence of (I2 + starch). Titration of sulphate by Ba(ClO4)2 solution using sulfonazo III indicator.
  • 9. Acid-base titration. Explanation of titration curve, characteristic regions, pH calculation of equivalence point. Titration curves of strong and weak acids and bases; acid-base buffer solutions, capacity (buffer index) and limits of buffer system, suitable buffer solutions for different pH regions, one-colour and two-colour indicators, mixed and fluorescence indicators. Examples of alkalimetric titrations: determination of strong, weak, concentrated acids, HF, B(OH)3, NH4+, alfa-aminoacids; titration of polyprotic acids; buffer capacity of hydrogensalts; determination of oxalic and phosphoric acids; pH estimate of equivalence titration point, calculation of titration error.
  • 10. Complexometric titrations. Requirements for complex formation reaction used in titration. Argentometric titration of cyanide : explanation of titration curve, problems joined with equivalence point evaluation (Liebig, Denigés). Mercurimetric determination of halides, thiocyanates, cyanides : explanation of titration curve, indication of equivalence titration point using nitroprusside a diphenylcarbohydrazone. Determination of Hg2+ using SCN- solution. Chelatometric titration : survey of currently used chelating agents, EDTA - titration; explanation of titration curves and determination of characteristic regions of titration curves; influence of conditional stability constants on curve shape; titration curve span and slope of titration curves, criteria for the choice of suitable pH for titration, equivalence point indicators, metallochromic indicators and their functional transitions, mechanism of equivalence point indication using currently used indicators (eriochrom black T, murexide, fluorexon); examples of EDTA titrations, determination of Mg(II) a Ca(II), determination of water hardness, EDTA titration using xylenole orange indicator, possibilities of simultaneous determination of two metal ions, titration solutions, standardization, errors of chelatometric titrations.
  • 11. Redox titrations. Explanation of titration curve, characteristic ranges, calculation of potential of equivalence point, conditions for quantitative course of reaction, choice of suitable redox systems taken from redox potentials and equilibrium constants, coupled redox systems, primary titration standards, reversible and irreversible redox indicators, explanation of reaction mechanism of redox indicators, errors of redox titrations. Oxidimetry with KMnO4 solution in acidic medium : stepwise reduction of permanganate, kinetics of reduction, Mn(II) autocatalysis and influence of medium, determination of oxalic acid, oxalates, Ca(II), Fe(II), hydrogen peroxide. Oxidimetry with KMnO4 solution in slightly acidic and alkaline medium, Mn(II) determination.
  • 12. Oxidimetry with iodine solution: mechanism of equivalence point indication, determination of sulphites, SO2, H2S, As(III), formaldehyde. Iodide oxidation to iodine and their titration by thiosulphate solution : hydrogen peroxide determination, oxygen in water, Cu(II), Mn(II), chromate, halogens, active chlorine. Analytical use of the system iodate + iodide. Amplification reactions. Oxidimetry with Ce(IV) solution: equivalence point indication; determination of Fe(II), hydrogen peroxide, iodide, oxalic acid, As(III). Oxidimetry with K2Cr2O7 solution : equivalence point indication, determination of Fe(II), ethanol in blood. Oxidimetry with KBrO3 solution: equivalence point indication; determination of As(III), Sb(III), organic compounds; indirect aluminium determination in 8-hydroxychinoline chelates.
Literature
  • Sommer L., Základy analytické chemie I, VUTium Brno 1998.
  • SOMMER, Lumír. Teoretické základy analytické chemie. I. Brno: Vysoké učení technické, 1995. info
  • ŠENKÝŘ, Jaroslav. Kvalitativní analýza : vybrané postupy k důkazu iontů. 2. vyd. Brno: Vydavatelství Masarykovy univerzity, 1995, 76 s. ISBN 8021011726. info
  • Analytická příručka. Díl I [Zýka, 1988]. Edited by Jaroslav Zýka. 4. upr. vyd. Praha: SNTL - Nakladatelství technické literatury, 1988, 678 s. info
  • ŠENKÝŘ, Jaroslav. Kvantitativní analýza : pracovní návody pro základní cvičení. 1. vyd. Brno: Vydavatelství Masarykovy univerzity, 1995, 44 s. ISBN 8021012145. info
  • SKOOG, Douglas A. Analytical chemistry :an introduction. 7th ed. Fort Worth: Saunders College Publishing, 1999, xxiv, 773. ISBN 0-03-020293-0. info
  • HARRIS, Daniel C. Quantitative chemical analysis. 4th ed. New York: W.H. Freeman, 1995, xix, 837 s. ISBN 0-7167-2508-8. info
  • Kellner R., Mermet J.-M., Otto M., Widmer H. M., Analytical Chemistry, Wiley 1998.
Assessment methods (in Czech)
2 hodinová přednáška
kombinovaná zkouška (písemná a ústní část)
Language of instruction
Czech
Follow-Up Courses
Further Comments
The course can also be completed outside the examination period.
The course is taught annually.
Listed among pre-requisites of other courses
The course is also listed under the following terms Autumn 2007 - for the purpose of the accreditation, Autumn 1999, Autumn 2010 - only for the accreditation, Autumn 2000, Autumn 2001, Autumn 2002, Autumn 2003, Autumn 2005, Autumn 2006, Autumn 2007, Autumn 2008, Autumn 2009, Autumn 2010, Autumn 2011, Autumn 2011 - acreditation, Autumn 2012, Autumn 2013, Autumn 2014, Autumn 2015, Autumn 2016, autumn 2017, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2022, Autumn 2023, Autumn 2024.
  • Enrolment Statistics (Autumn 2004, recent)
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