INSTRUMENTAL ANALYTICAL CHEMISTRY
Academic year and teacher
If you can't find the course description that you're looking for in the above list,
please see the following instructions >>
- Versione italiana
- Academic year
- 2022/2023
- Teacher
- FLAVIO ANTONIO FRANCHINA
- Credits
- 6
- Didactic period
- Primo Semestre
- SSD
- CHIM/01
Training objectives
- The class aims to provide students with (i) the basic theoretical background and technical skills to solve quali- and quantitative analytical problems in complex matrices of different natures; (ii) the chemical-analytical skills adequate to handle complex instrumentation for chemical, such as the various chromatographic instruments and a mass spectrometer. This knowledge will specifically cover not only the chemical-physical principles on which the instrumentation is based, but also the components of the instrumentation and the main parameters that characterize analytical performance. Thus, by the end of the course, each student will acquire the necessary knowledge to be able to compare different analytical methods and instrumentation, in order to choose the most appropriate in relation to the sample to be analyzed and the research question.
The course also aims to provide students with knowledge about the principles of good laboratory practice, quality management and teamwork, as well as the main standards operating procedures regarding the validation of analytical methods to be able to write a technical report of analysis, including the statistical analysis of results. Prerequisites
- Basic knowledge of Analytical Chemistry: the basics of measurement, error, molecular spectrophotometry, potentiometry, and the general theory of chromatography. Basic knowledge of General and Inorganic Chemistry, Organic Chemistry, Chemistry-Physics, Physics, Mathematics and Statistics. Theoretical and practical knowledge of the basic instrumentation and operations of a chemical laboratory. Knowledge of safety regulations related to a chemical laboratory. The curriculum of the course of study does not provide other more specific prerequisites or barriers.
Course programme
- Introduction to instrumental chemical analysis and the various steps in the analytical process.
Sample preparation and pretreatment techniques: liquid, solid and gas-phase extraction methods (headspace, purge & trap); physical-assisted extraction methods (microwave, ultrasound); derivatization techniques of analytes of interest.
Separative techniques and main instrumental aspects.
Gas chromatography (GC): sample introduction techniques (split/splitless, direct, PTV, thermal desorption), characteristics of carrier gases and high-efficiency columns (geometry, stationary phases, etc.), constant-temperature or programmed separations, fast and ultra-fast GC systems, detectors (flame ionization, electron-capture, thermoconductivity, vacuum ultraviolet).
High (or ultra-high) performance liquid chromatography (HPLC/UHPLC): main separation mechanisms, column geometry and composition, stationary phase preparation methods, isocratic or gradient separations, detectors (UV-Vis diode array, fluorescence, refractive index, evaporative light scattering, circular dichroism).
Preparative liquid chromatography: concepts of linear/nonlinear chromatography, adsorption isotherms, instrumentation, continuous multi-column preparative chromatographic techniques.
Supercritical fluid chromatography (SFC): properties of supercritical fluids, instrumentation and operating variables, characteristics of columns and detectors.
Multidimensional chromatographic techniques: "heart-cut" and "comprehensive" approaches, instrumental configurations (LC-LC, LC×LC, GC-GC, GC×GC, LC-GC), modulators, interpretation of chromatograms.
Capillary electrophoresis (CE): sample introduction techniques, characteristics of instrumentation and detectors.
Mass spectrometry (MS): general characteristics of a mass spectrometer; ion sources (electron impact, chemical ionization, electrospray ionization, atmospheric pressure chemical ionization, etc.); analyzers (magnetic sector, quadrupole, time-of-flight, Fourier transform cyclotron resonance, Orbitrap, etc.); tandem mass spectrometry (MS/MS).
Hyphenated techniques: coupling of major chromatographic techniques with mass spectrometry (instrumental configurations, operating conditions, interfaces, etc.) or other spectroscopic/spectrometric techniques (e.g., LC coupled to inductively coupled plasma mass spectrometry, LC-ICP-MS).
The course also includes a series of hands-on laboratory experiences (described below), consisting of various experiments and demonstrations in the department's research laboratories, for a total of 24 hours.
Laboratory experiments:
-Extraction and determination of phthalic acid esters by GC-ECD with capillary column.
-Derivatization and determination of fatty acids by GC-FID with capillary column.
-Determination of methanolic content in alcoholic distillates by GC-TCD with packed column.
-Determination of vanilla aroma in confectionery products by HPLC-DAD with RP-C18 column.
-Determination of anions (chlorides, nitrites, nitrates, phosphates, sulfates) in surface water by ion chromatography.
-Demonstration analyses in GC-MS, GC×GC-MS, preparative LC and HPLC-ESI-MS. Didactic methods
- Theoretical lessons with the help of the blackboard and slide show on all the subjects of the program (4 ECTS = 24 hours). Laboratory practice (2 ECTS = 24 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 2/3 of the scheduled experiences. Learning assessment procedures
- The purpose of the exam is to test the level of knowledge of the topics covered and to assess the ability to use the acquired knowledge to solve even complex analytical problems. For the theoretical part, there will be a test in the form of an oral interview or written test that will consist of three/four questions that may cover all the topics of the program. The laboratory part will consider the preparation of scientific reports on the practical experiments. The final grade depends on the outcomes of the 2 in the following way: the theoretical part will account for 80 percent of the final grade, while the laboratory part will account for the remaining 20 percent. The grade takes into consideration also the behavior of the student during the laboratory.
Reference texts
- The main textbook is the following: D.A. Skoog, F.J. Holler, S.R. Crouch "Chimica Analitica Strumentale", 2° edizione, EdiSES, 2009.
For more in-depth descriptions, the following texts are also recommended:
1) Moret, Purcaro, Conte, “Il campione per l’analisi chimica”, Springer, 2014
2) Gross, “Spettrometria di massa”, edizione italiana, EdiSES, 2016
3) D.C. Harris, "Chimica Analitica Quantitativa", 3° edizione italiana, Zanichelli, 2017.
4) Grotti, Ardini, “Il laboratorio di chimica analitica”, EdiSES, 2022.
