ANALYTICAL CHEMISTRY I AND LABORATORY A - L

Learning Objectives

• MODULO 1

  To enable students to become conversant with issues concerning equilibria in solution (acid-base, precipitation, complexation, redox).

  Concepts acquired from this Module will then be used in the Laboratory Module.

• MODULO 2

  To enable students to use autonomously the concepts acquired during the theoretical course (Module 1).

Course Structure

• MODULO 1

  Lectures associated to the analysis of numerical problems. Problems are presented and illustrated by the teacher and sometimes by the students themselves upon request.

• MODULO 2

  Lectures associated to the analysis of numerical problems. Problems are presented and illustrated by the teacher and sometimes by the students themselves upon request.

Detailed Course Content

• MODULO 1

  Aim of the Course. Classification of the methods of analysis. Concentration units. Numerical examples.

  Solution Equilibria. General principles. Gibbs energy and equilibrium constants. Factors influencing equilibrium constants; temperature, solvent, ionic strength. Activity and activity coefficients. Debye-Huckel's Law. Numerical examples. Acid-base equilibria. Strength of an acid. Mass, charge and proton balance equations. pH. Rigorous definition. Calculation of the pH of strong acids: rigorous equation and approximations. Approximation criterion. Numerical examples. Weak acids/bases. Calculation of the pH of weak bases: rigorous equation and approximations. Numerical examples. Mono- and two-color indicators: rigorous equations. Numerical examples.

  Polyprotic acids: rigorous and approximate equations. Acid mixtures. Ampholytes. Distribution diagrams. Titration curves. Strong base with a strong acid, weak acid with a strong base, polyprotic acids. Numerical examples. Buffer solutions. Buffering capacity: rigorous equation. Numerical examples.

  Precipitation equilibria. Solubility and solubility product. Factors influencing electrolyte solubility: temperature, solvent and ionic strength. Effect of a common ion, pH and formation of complexes. Titrations based on the formation of a precipitate. Error at the end point: rigorous equation. Numerical examples.

  Complexation equilibria. Degree of formation. pH effect on complexation equilibria. Conditional constant. Metallochromic indicators. Choice of operational conditions. Complexometric titrations. Numerical examples.

  Data treatment: outline. Experimental errors. Bias and random errors. Precision and accuracy. Sampling. Sample description. Position and dispersion parameters. Binomial distribution, Poisson distribution, normal distribution. Reduced normal. Main tests (Student test, F-test, χ2, Dixon’s test). Significant figure. Error propagation. Numerical examples.

  This Module requires approximately 48 hrs, while the second Module requires 72 hrs; the total working time goes up since Students often ask for extra time for exercises outside the scheduled hours.

  Please note: All the above arguments are deemed indispensable.

• MODULO 2

  Laboratory. Choice of the analytical method. Instrumentation, precision, sensitivity. Result report.

  Gravimetric analysis. Analysis through precipitation. Precipitate formation. Nickel determination by DMG.

  Titrations: general principles. Preparation of standard solutions. Primary standards. Standardization procedure.

  Acid-Base titrations. Na₂B₄O₇.10H₂O in acidimetric titrations. Determination of the titre of acids/bases commonly employed in a laboratory.

  Precipitation titrations. Argentometry. Chloride determination according to Mohr and Fajans. Chloride/Carbonate separation

  Complexometric titrations. EDTA titrations. Determination of Cu²⁺.

  Redox titrations. Permanganometry. Determination of Fe²⁺ and H₂O₂. Iodometry. Determination of Cu²⁺.

  This Module is expected to last for 72hrs. This does not include exercises upon student request, provided only if a facility is available.

Textbook Information

• MODULO 1

  1. Kolthoff, Sandell, Meehan e Bruckenstein - Analisi Chimica Quantitativa. Vol. 1 e Vol. 2, Piccin Editore.

  2. E. De Simoni - Chimica Analitica, CUL (Bologna).

  3. Skoog & West - Chimica Analitica. S.E.S.

  4. D. H. Harris - Chimica Analitica quantitativa, Zanichelli.

  5. Freiser e Fernando - Gli equilibri ionici della Chimica Analitica. Piccin Editore.

  6. J. N. Butler - Ionic Equilibrium: Solubility and pH Calculations, Wiley

• MODULO 2

  Kolthoff, Sandell, Meehan e Bruckenstein - Analisi Chimica Quantitativa. Vol. 1 e Vol. 2, Piccin Editore.

  Vogel - Analisi Chimica Quantitativa. Vol. 1 e Vol. 2, J. H. Jeffery, J. Bassett, J. Mendham, R. C. Denney Editori, CEA

  Freiser e Fernando - Gli equilibri ionici della Chimica Analitica. Piccin Editore.

  Slides provided by the lecturer