27542 - Analytical Chemistry 1

Learning outcomes

At the end of the course the student  knows the principles of an analytical sequence: the main sampling techniques and sample treatments for solids, liquids, and gases; as well as the main analytical methods, i.e. gravimetry, acid-base titrations, spectrophotometry, and chromatography.

Course contents

Prerequisite:
No previous knowledge is required, except math and fundamentals of chemistry. Foreign students should master Italian (writing, speaking and listening) at a C1 level.
Program:
a) Lectures (24 hours).
Definition of analytical chemistry. Outline of an analytical process. Fundamentals of statistics: average, standard deviation, correlation coefficient, significant figures. Methods for quantitative analysis: calibration line, internal standard, standard additions, internal normalization. Classical analytical methods. Sampling: water, air, soil. Sample preservation . In-situ analysis probes . On-site/on-line analysis of air and water. Sample preparation: milling, drying, filtering, concentrating . Use of an analytical scale. Weighing and related errors . Sample digestion (wet, microwaves, Kjeldahl). Solid-liquid extraction. Vapour current extraction. Soxhlet extraction . Accelerated solvent extraction. Ultrasound assisted extraction . E xtraction with supercritical fluids. Percolation. Liquid-liquid extraction (theory, pH effect, use of chelating ligands, continuous extractors using solvents more/less dense than water, Lickens-Nickerson extractor). Chromatographic techniques (adsorption, partition, ion-exchange, affinity, size-exclusion). Thin-layer chromatography (TLC). On column chromatography (fundamentals, separation of two bands, numerical example for partition coefficients K=1 and K=3). Chromatogram (selectivity, efficiency, resolution). Gas chromatography (GC) (Van Deemter equation; gas chromatographic detectors: flame ionization detector (FID), thermal conductivity detector (TCD), mass spectrometer (MS, fundamentals). High-performance liquid chromatography (HPLC) (normal and reverse phase, eluotropic series of solvents, six-port valve injector, detectors: UV-visible adsorption with fixed and variable wavelength, diode array, refraction index, electrochemical/ammeter, mass spectrometer). Spectroscopy techniques. UV-visible spectroscopy: theory, transmittance, absorbance, Lambert-Beer equation. Lambert-Beer equation limits. Spectrophotometer scheme.

b) Classroom exercises (12 hours).
Students apply basic concepts (mole, equivalent, concentration, and dilution) to solve problems of analytical chemistry. Students are also requested to do some homework with subsequent correction during the class.

c) Laboratory experiments (32 hours).
Students apply to experimental work som of the lecture subjects and stoichiometric exercises. At the end of each experiment, students write a report.

Readings/Bibliography

Daniel C. Harris, CHIMICA ANALITICA QUANTITATIVA, Zanichelli, Bologna, 1997

R. Cozzi, P. Protti, T. Ruaro, ANALISI CHIMICA: MODERNI METODI STRUMENTALI, Zanichelli, Bologna, 1994

Richard Anderson, SAMPLE PRETREATMENT AND SEPARATION, John Wiley & sons, 1987

Brian W. Woodget and Derek Cooper, SAMPLES AND STANDARDS, John Wiley & sons, 1987

J. N. Butler, Equilibri Ionici, Ed. Universo, Roma

Teaching methods

The course comprises lectures (24 hours), classroom exercises (12 hours), and laboratory experiments (32 hours). During the lectures, the principles of an analytical sequence will be explained. The exercises consist of stoichiometric calculations. In the laboratory classes, the students will apply some of the analytical techniques and stoichiometric calculations which have learned during the lectures.

Assessment methods

The final exam is an oral discussion about the lecture subjects and the laboratory experiences. Both the discussion and the written reports on the laboratory experiences contribute to the student's final evaluation and, consequently, to the exam score.

Rule 1. Admission to the final exam is allowed to the students who:
a. have attended at least 5/6 of the laboratory experiences; and
b. have handed over all the experience reports.

Rule 2. At the end of each laboratory experience, students should write a report and hand it to the teacher or assistant within 7 days after the end of experience.

Rule 3. Admission to the final exam is subjected to the compliance with the present rules.

Teaching tools

Blackboard; transparencies; power-point and other similar softwares; instruments which can be studied and/or used in laboratory.

Teaching materials published on AMS Campus web site.

Office hours

See the website of Guido Galletti