Analytical Chemistry I with Lab

Part 1 Propedaeutic concepts Analytical Chemistry: definition, history, significance. Analytical methods. Sequence of steps in a typical quantitative analysis. Sampling (hints). Elements of theory of errors applied to analytical chemistry; criteria for data treatment and statistical tests. Concentration scales, ionic strength, activities, activity coefficients. Equilibrium constants, standard states. Nernst law, galvanic cells, ion-reversible electrodes, electrode potential scale.

Part 2 Equilibria in solution and volumetric analysis. Titration methods: definitions, classification, standards. Acid/base, precipitation, complessation and redox titrations: mathematical description of the corresponding equilibria and elaboration and interpretation of titration diagrams for model systems. Speciation diagrams and Pourbaix diagrams.

Part 3 Electroanalysis. Conductimetry, potentiometry (ion-selective electrodes, pH-metry, p-Ionometry, redox potential, water hardness), voltammetry (cyclic voltammetry, polarography, pulsed techniques, stripping techniques for trace analysis), amperometry (trace water by Karl Fischer method, dissolved oxygen by Clark method), biosensors and electronic tongues/noses (hints). Fundamentals, instrumentation, protocols (standardization, direct measurements, instrumental titrations). Model cases in the analytical laboratory and in fundamental and applied research.

Lessons [16 hours] Concentration and concentration scales. Dilutions. Laboratory materials and reagents. Instrumentation for mass and volume measurements. Analytical methods characteristics, prediction and analysis methodologies. Safety regulations. Good laboratory practice. General principles of acid-base, precipitation, complexometric and redox titrations. General principles of conductimetry, potentiometry and pH-metry, amperometry. Survey of experimental procedures.
Numerical exercises [8 hours] Calculations concerning solution preparation and titrations. Excel electronic spreadsheet use for experimental data treatment.
Laboratory experiments [48 hours]
1) Volumetric analysis with colorimetric indicators: preparation of standard solutions, acid/base titrations (KHPh, TRIS, vinegar, bicarbonates), complexation titrations (water hardness with EDTA), precipi¬tation titrations (chlorides with Mohr and Fajans methods), redox titrations (iodine, ascorbic acid) [24 hours].
2) Electroanalysis: Conductimetry: conductimeter calibration, direct measurement of specific con¬ducti¬vi¬ty, conductimetric titrations [4 hours]. Potentiometry: ion-selective electrode assembling, calibra¬tion and use for direct p-Ion determination; pH-meter standardization and direct pH measurements; potentiometric acid/base (HCl, HCl+CH3COOH, unknown aminoacid detection), precipitation (chlorides in egg pasta), complexation (water hardness) and redox (iron determination) titrations [16 hours]. Amperometry: dead stop end point amperometric detection of Vitamin C in real samples (tablets and fruit juices) [4 hours].