Course program
The course starts with the discussion of general problems related to the complete execution of a chemical analysis: sampling; the principles that guide the choice of the most suitable method of analysis and, from this, the equipment, the characteristics of the material and the type of reagents needed (highlighting any possible hazardous characteristics both in terms of their use and disposal); the evaluation and processing of the results obtained; the expression of the final result of the analysis.
The principles of volumetric analysis are then illustrated: solution equilibria are evaluated for their application in quantitative analysis, taking into consideration the physical-chemical parameters that influence them (temperature, ionic strength, matrix effect and collateral reactions in general, etc.). In particular, titrations based on neutralization reactions (acidimetry and alkalimetry), on the formation of sparingly soluble salts (argentometry), on complexation (complexometry and chelometry), on oxidation-reduction (permanganometry, dichromatometry, cerimetry, iodimetry and iodometry, bromometry) are treated. For each system, theoretical titration curves are constructed and the choice of suitable indicators in order to minimize the error in the analysis is discussed.
In a similar way, the principles of gravimetric analysis both by volatilization and precipitation techniques are then illustrated. In particular, the theoretical aspects of precipitation reactions are discussed in order to identify the most suitable experimental conditions for their application to quantitative analysis: purity and quantitative recovery of the precipitate, the need of having a defined and known chemical formula for the weighed species, etc. The theoretical treatment is completed with several examples of gravimetric determination of cations and anions that make it possible to point out specific analytical problems.
The last part of the course is dedicated to issues related to the of analysis of multiple chemical species simultaneously present in the same sample. The general criteria for the evaluation of the system are discussed in order to perform the analysis under experimental conditions that make the method sufficiently specific and selective or, in the absence of these requirements, the modalities for operating a separation of the analyte from the interfering species. The illustration of the main (non-instrumental) separation techniques for inorganic ions (precipitation, volatilization, ion exchange, solvent extraction) is completed with examples chosen in order to have a broad picture of the multiple parameters to be controlled in the analytical procedure to obtain accurate results.
Each topic is accompanied by numerical exercises and by one or more experimental analyses in the laboratory (single place) on unknown samples, in order to allow the student to evaluate the "difficulties" of the application of the theoretical principles discussed in the experimental analysis and, above all, to personally realize the importance of correctly performing all the individual analytical operations to obtain accurate and precise results. After a first experimental approach with some essential operations of quantitative analysis (taking a solid sample or a solution, weighing using top loading and analytical balances, preparing a solution with an approximate or exactly known title, etc.), the student is guided through the execution of analyses that, for the diversification of the operative modalities and their increasing complexity, allow to integrate and improve the experimental preparation of the students. Each analysis is concluded with the drafting of a brief report that commits the student to rethink the experimental operations carried out, to examine in depth its meaning and purpose, and to deliver the final result of the analysis only after a careful evaluation of the partial ones.
Prerequisites
There are no particular prerequisites for attending the course.
Books
E.Bottari, M.R.Festa, “Chimica Analitica Quantitativa”, La Sapienza Editrice, Roma.
E.Bottari, M.R.Festa, “Problemi di Chimica Analitica”, La Sapienza Editrice, Roma.
I.M. Kolthoff, E.B. Sandell, E.J. Meehan, S. Bruckenstein, "Analisi Chimica Quantitativa Vol. 1 e 2", Piccin Editore, Padova
Further texts:
D.S. Hage, J.D. Carr, Chimica analitica e analisi quantitativa, Piccin Editore, Padova
G. Giorgio Bombi, Paolo Pastore e Valerio Di Marco, Chimica analitica. Trattazione algebrica e grafica degli equilibri chimici in soluzione acquosa, Edises, Napoli
Teaching mode
The course consists of classroom lectures where the topics will be dealt with from a theoretical point of view and with numerical exercises and a relevant laboratory (single places - individual activity) part where the student can acquire good laboratory practice and develop that "analytical sensitivity" which is fundamental for the preparation and experimental execution of any chemical analysis.
Frequency
While for the lectures the frequency can be considered optional, since the evaluation of the laboratory tests is an integral part of the final evaluation the frequency of laboratory experiences is mandatory
Exam mode
The students will be assessed based partly on the evaluation of the laboratory practicals performed during the course and, in part, on the outcome of an oral examination to check the knowledge of the topics under consideration.
Lesson mode
The course consists of classroom lectures where the topics will be dealt with from a theoretical point of view and with numerical exercises and a relevant laboratory (single places - individual activity) part where the student can acquire good laboratory practice and develop that "analytical sensitivity" which is fundamental for the preparation and experimental execution of any chemical analysis.