ADVANCED ANALYTICAL CHEMISTRY AND LABORATORY OF ADVANCED ANALYTICAL CHEMISTRY
Academic year and teacher
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- Versione italiana
- Academic year
- 2015/2016
- Teacher
- MAURIZIO REMELLI
- Credits
- 9
- Didactic period
- Primo Semestre
- SSD
- CHIM/01
Training objectives
- The aim of the course is to give detailed information on the operation and working principles of complex instrumentation of general use in all laboratories of chemical analysis. The following techniques will be considered: gas-chromatography, high-performance liquid-chromatography, ion chromatography, polarography, mass spectrometry, surface analysis, electronic microscopy, thermogravimetric analysis and differential scanning calorimetry. The following knowledge will be specifically addressed: i) chemical and physical principles on which the instrumentation is based; ii) main instrumental components; iii) main parameters characterizing analytical performance.The students will also learn the principles of good laboratory practice and quality management, as well as the main guidelines regarding the validation of analytical methods.
The students will learn how to manage, as regards the essential features, the most common chromatographic instrumentation of various complexity. They will gain experience in the development of analytical methodologies for different applications such as the study of materials, environmental protection and cultural heritage, life sciences. The students will also learn how to discuss the analytical results and how to write a concise and complete report, including the statistical analysis of experimental data.
The students will have to get used to: working in groups, sharing tasks and responsibilities; following the safety rules in the lab; solving the problems arising from the experimental work; comparing different methods in order to choose the most suitable to the sample under analysis; respecting the protocols and timetables established for the laboratory sessions. Prerequisites
- Basic knowledge of Analytical Chemistry: solution equilibria, titrations, atomic and molecular spectrophotometry, potentiometry and the general theory of chromatography. Basic knowledge of General and Inorganic Chemistry, Organic Chemistry, Physical Chemistry, Physics, Mathematics and Statistics.
Theoretical and practical knowledge of the basic instrumentation and the elementary operations of chemical laboratory.
Knowledge of safety regulations for a chemical laboratory.
The curriculum of the course of study does not provide other more specific prerequisites or barriers. Course programme
- Sampling and sample preparation (3 hours): sampling of solids, liquids and gases; procedures for preparation of a laboratory sample.
Concepts and methods for the development of an analytical methodology with quality assurance (4 hours). Method validation and accreditation of laboratories. This argument is completed by inviting an ARPAE specialist in the area of quality to give a seminar.
Chromatographic techniques (15 hours): general principles, parameters and basic equations. In depth description of the instrumentation and the principles of operation of: gas chromatography (GC), high performance liquid chromatography (HPLC), ion chromatography (IC). Applications and methods of analysis.
Molecular mass spectrometry (MS) (8 hours): ionisation methods (electronic impact, chemical ionization, desorption sources); mass analyzers (magnetic sector, quadrupole, time of flight, ion trap, cyclotron resonance with Fourier transform). Coupled chromatographic methods: GC-MS and HPLC-MS.
Thermal analysis (2 hours): thermogravimetry, differential thermal analysis, differential scanning calorimetry; examples of applications.
Surface Analysis (4 hours): methods using probes consisting of photons, electrons, ions or fields.
Voltammetric methods (2 hours): direct current polarography, quick and linear scanning voltammetry, cyclic voltammetry, normal pulse voltammetry, differential pulse voltammetry, square wave voltammetry, anodic and cathodic dissolution voltammetry.
Explanation of the laboratory experiences (2 hours).
The course includes a series of practical laboratory experiences (described below), which keep busy 12-16 afternoons for a total of 48 hours.
Practical experiences on a gaschromatograph equipped with capillary column and flame ionization detector: separation of linear hydrocarbons under isothermal and programmed temperature; analysis of a gasoline. Analysis of a gasoline in GC-MS. Practical experiences on a gaschromatograph equipped with packed column and thermal conductivity detector: control of the methanol content in wines and distilled spirits. Experiences of HPLC on a reversed phase column: control and performance comparison of two columns; mobile phase optimization for the resolution of toluene, naphthalene and benzophenone; determination of vanilla aroma in confectionery products; quantitative determination of anions and / or cations in drinking water by ion chromatography. Analysis of trace metals by voltammetric methods. Demonstration sessions of mass spectrometry with electro-spray injection and electron microscopy. Didactic methods
- Theoretical lessons with the help of the blackboard and slide show on all the subjects of the program (5 ECTS = 40 hours). 12 laboratory practice (4 ECTS = 48 hours) with the use of spreadsheets for data processing. Additional lab sessions are planned where students will discuss the results of the experiences and write reports, with the assistance of the teacher and teaching support staff.
The frequency of the laboratory will be allowed only to students who have achieved certification on security. The attendance of the laboratory sessions is mandatory for at least 8 experiences among those scheduled. Learning assessment procedures
- Scope of the exam is to verify both the knowledge of the students on the course topics and their ability to use this knowledge to solve complex analytical problems. The final exam, in an oral test, will consist of 3-4 questions covering all the topics treated in the course, including the laboratory experiments. In order to take the exam, the student must have handed the teacher the reports, prepared individually or in groups, of the laboratory experiences, which will be corrected and evaluated in thirtieth. The final score will be the average of the marks of laboratory reports and oral exam.
Reference texts
- The main textbook is the following: R. Kellner, J.-M. Mermet, M. Otto, H.M. Widmer, "Chimica Analitica", EdiSES, 2003.
For consultation, the following texts are also recommended:
1. R. Cozzi, P. Protti, T. Ruaro, "Analisi Chimica Strumentale", 2a edizione, Zanichelli, 1997.
2. D.C. Harris, "Chimica Analitica Quantitativa", 2° edizione, Zanichelli, 2005.
3. D.A. Skoog, F.J. Holler, S.R. Crouch "Chimica Analitica Strumentale", 2° edizione, EdiSES, 2009.
The teacher will also provide students with the slides shown in class, in the form of handouts.
