67031 - Instrumental Analytical Chemistry and Laboratory Laboratory

Learning outcomes

At the end of the course the student will know and use the main instrumental analytical techniques. He knows the operation of the main theoretical and practical analytical equipment. He is able to plan and execute a complete analysis and to report the result in a statically correct way. Knows the main analytical instrumentation and is able to perform an analitic determination on the basis of the official regulations. Will be able to identify the most appropriate methodologies and techniques to solve simple analytical problems; to report the work of a lab notebook. It will also be able to process and present experimental results using the most appropriate statistical tests.

Course contents

-Description of the phases of the analytical process. Main components of an analytical instrumentation. Outline of sampling, sampling and storage problems. The "analysis report" and the "laboratory report".

-Statistics related to instrumental analysis. Signal to noise ratio. Effect of digital sampling on the response. Calibration and regression curves. Standard addition. Confidence interval of a concentration obtained from a calibration line and through the addition method. Calibration curves in case of deviations from linearity. Limit of detection and sensitivity of the instrumental chemical analysis. Limit of quantification. The error in the analytical process.

-Electrochemical techniques. Electric conductivity of electrolytic solutions. Specific conductivity, equivalent conductivity and equivalent conductivity at infinite dilution. The conductivity meter and its use. Direct conductivity measurements. Conductometric titrations (acid-base, precipitation, complexometric). Ion selective electrodes and reference electrodes. Potentiometric methods with ion-selective electrodes and metal indicator electrodes. Gran's method for identifying the end point of a titration.

-Theoretical basis of chromatographic separations, counter-current extraction. Mechanism of the column chromatographic process. The phenomenon of the broadening of the chromatographic band and its phenomenological justifications: plate theory and kinetic theory. Instrumental chromatographic techniques: gas chromatography and high efficiency liquid chromatography (HPLC). Evaluation of the efficiency of a chromatographic column. Main chromatographic parameters. Quality of chromatographic separations. Qualitative analysis: relative retention time and retention indices. Quantitative analysis methods in chromatography. Characterization of the chromatographic phases (Rohrschneider-McReynolds indices).

-UV-Vis molecular absorption spectrometry: principles, instrumentation, operating conditions and quality control of spectrophotometric measurements. Construction of the instrumental response curve and Bouguer-Lambert-Beer law. Analysis of mixtures. Flame atomic absorption spectrometry. Principles, instrumentation, hollow cathode lamps, Boltzman's law. Methods of qualitative and quantitative analysis in flame.

The course includes numerous laboratory experiences, the design of some of which will be left to the students, under the guidance of the teachers.

Readings/Bibliography

D.C. Harris, “Chimica Analitica Quantitativa”, Zanichelli, Bologna,

F. W. Fifield, D. Kealey, “Chimica Analitica teoria e pratica”, Zanichelli, Bologna

Skoog,. West, Holler,Crouch, “Fondamenti di Chimica Analitica”, EdiSES, Napoli

Elizabeth Prichard, Victoria Barwick, "Quality Assurance in Analytical Chemistry" John Wiley

C. G. Enke, “The art and science of chemical analysis”Wiley

Teaching methods

The course of instrumental analytical chemistry and laboratory involves front lectures on the theroretical aspects of  the laboratory experiences.. Students should have a bound laboratory notebook for recording all the data at the time of the observation during laboratory classes. The recording of data on loose pieces of paper or in a preliminary note book is expressly forbidden.

Assessment methods

The exam consists of a written test lasting 3 hours. The written test aims to evaluate the acquisition of the knowledge and skills required by the course program by solving exercises and answering open questions. During the written test, the use of textbooks, the periodic table and lecture notes (or slides)is not allowed. The exam, if passed, remains valid for the sessions scheduled for the academic year in which the course was held.

The evaluation of the Instrumental Analytical Chemistry course will be integrated with that of the Laboratory of Instrumental Analytical Chemistry Course which takes place through the preparation of laboratory reports on individual experiences.

The exam will be passed if the score obtained in the written test is greater than or equal to 18/30; in this case the final score will be determined by the average, weighted on the basis of the assigned credits, of the scores obtained in the laboratory activity.

The mark obtained in the Instrumental Analytical and Laboratory Chemistry exam will be integrated (single mark) with that obtained in the Analytical Chemistry exam, weighing the two parts based on the assigned credits.

The procedures described above may be subject to changes due to the covid 19 emergency.

Teaching tools

Use of the projector and blackboard during classes.Textbook.

Office hours

See the website of Erika Scavetta

See the website of Andreas Stephan Lesch