87822 - CHIMICA ANALITICA INDUSTRIALE CON LABORATORIO M

Learning outcomes

The course is aimed to acquire the capability to use the suitable instrumentation, on the bases of the characteristics of the analyte, matrix and amount of sample. To project a scheme of an analytical procedure, starting from appropriate sampling plans, even with technical regulation. The students will be able to evaluate the quality of an analytical or industrial process with statistical tests and controls charts.

Course contents

Learning Objectives

Knowledge and Comprehension

At the end of the course, students will know:

• statistical methods to evaluate results given by sundry operators
• how to do the quality control of processes and reference regulation
• easy procedure to design experiments
• principle and instrumental assets of chromatographic, spectroscopic and electrochemical techniques, also hyphenated
• principle and instrumental assets of surface analysis
• ·operating principle of sensors and bio-sensors

At the end of the course, students will have understood:

• the role of statistical procedure in the management and control of analytical and industrial processes
• the role of physical-chemical parameters in the optimization and prediction of chromatographic separations (GC and HPLC)
• issues related to analyte detection in trace and ultra-trace analysis
• relationships between energy levels of an analyte and the desiderated result
• relationships between mass transfer and the electrochemical signal of an analyte

Ability and Competence

At the end of the course the student will be able to:

• evaluation of the analytical result coming from two or more operators
• build and use control curves for quality evaluation of analytical process
• find possible strategies to optimize a chromatographic separations
• use small and medium instrumentation (HPLC, GC, atomic absorption, electrochemical stations)
• detect correct procedures to control interferences and limit of detection
• design an appropriate analytical procedure for two or more analytes determinations, using also the regulations

Topic of the course

Sampling theory, control charts, analysis of variance (ANOVA). Accreditation and test labs. ISO 9000 certification and registration. Basics of experimental design. Sampling in industrial field.

Optimization of chromatographic separations (GC and HPLC). Electrophoresis and TLC. Extraction and purification systems in solid phase.

Automated analytical methods. Elemental analysis.

Spectroscopy and spectrometry. Atomic spectrometry in absorption and emission mode. Graphitic furnace, plasma.

Reflection and Refraction of light. Total internal reflection. Optical fibers. Attenuated total reflection (ATR). Near infrared spectroscopy: principles and industrial applications. Raman spectroscopy.

Analysis of surfaces by X-Ray methods. X-ray - matter interaction. Basic of x-ray absorption and emission spectroscopy. Photoelectron spectroscopy. Industrial application of X-ray analysis.

Hyphenated techniques. Detection in Mass Spectrometry. Basics of ICP-MS, GC-MS, SIMS.

Electroanalytical Chemistry and Sensors. Electron transfer. Mass transport (diffusion, convection, migration). Controlled potential techniques (cronoamperometry, cronocolumbometry, polarography, cyclic voltammetry)

Techniques for the trace and ultratrace analysis (anodic, cathodic and potentiometric stripping)

Modified electrodes for sensors applications

Amperometric sensors and biosensors

Practical

The course is completed by some laboratory work (practical).

PRE-REQUIREMENTS OF KNOWLEDGE AND ABILITY TO FOLLOW THE COURSE

In general, the knowledge and skills acquired in the following courses are required: Mathematics, Physics, Analytical Instrumental Chemistry

In particular, students must:

• be able to perform graphs and calibration curves
• be able to prepare solutions at a given concentration (also low concentration) with the appropriate precision
• Possess basic element of optics and algebra
• be able to use simple analytical instruments

Readings/Bibliography

1. H.H. Willard, R.R. Merritt, J.A. Dean, F.A. Settle. Instrumental Methods of Analysis 7th edition. Wadsworth Publishing Company, 1988
2. J.C. Miller and J.N. Miller, Statistics and Chemometrics for Analytical Chemistry, 6^th ed., Prentice Hall (UK), 2010
3. M.Castino, E. Roletto, Statistica applicata. Trattamento dei dati per studenti universitari, ricercatori e tecnici. Piccin, 1999 (ISBN: 9788829909353)
4. D.A. Skoog, D.M. West, F.J. Holler, S.R. Crouch, F Chimica Analitica Strumentale, III Ed., Edises, 2009 (ISBN:9788879593427).
5. K. A. Rubinson, J. F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002
6. P.M.S. Monk "Fundamentals of Electroanalytical Chemistry" J. Wiley & Sons, New York, 2002.

Teaching methods

The course involves front lectures and laboratory work.

Assessment methods

The assessment of the learning consists in final written exam on some selected research topics learned during the course.

The written exam is made up of a maximum of 10 items between: a) multiple-choice questions; B) open answer questions; C) execution of problems and exercises related to the acquired knowledge and skills acquired on the theoretical, practical and applied contents of the course. The test may also include questions related to previous knowledge not explicitly covered by the course but resulting essential for the understanding of the course.

The duration of the written test is 3 hours.

The use of textbooks, the periodic table, and lessons (or slides) is expressly forbidden. It is compulsory to have a calculator (not allowed on tablet or cellular devices) and the need to draw millimeter charts (pencils, rulers, team, rubber, pencil sharpeners) if required.

Examination, if passed, keeps its validity for the sessions scheduled for the full academic year. The positive outcomes will be erased the moment a second test will be submitted to correction. It’s possible to reject maximum two positive grades.

Teaching tools

Lecture slides and other material useful for exam preparation is made available to the student electronically via the Internet. . To get the teaching material the student must be connected to the specific web site (Moodle).

Office hours

See the website of Marco Giorgetti

See the website of Domenica Tonelli

See the website of Sergio Zappoli

See the website of Andreas Stephan Lesch