Analytical Chemistry

A.Y. 2024/2025
9
Max ECTS
96
Overall hours
SSD
CHIM/01
Language
Italian
Learning objectives
This course allows the student to acquire specific knowledge regarding the use of complex instruments for general use in all chemical analysis laboratories, learning to manage analytical instruments of different complexity. The student will acquire the principles of good laboratory practice and quality management and control, as well as the main rules regarding the validation of analytical methodologies and protocols.
Experience will also be gained in planning (through experimental design) and in the subsequent development of analytical methodologies for different applications such as the study of materials, environmental and cultural heritage protection, life sciences. The student will also be able to discuss the analytical results also on the basis of the statistical analysis of the results, through chemometric techniques. Finally, the student will develop teamwork skills, dividing tasks and responsibilities; will operate in the laboratory according to safety standards; will solve the problems inherent in experimental studies; will be able to compare different methods in order to choose the most appropriate one in relation to the sample to be analysed; will respect the protocols and schedules established for the laboratory activity.
Expected learning outcomes
- Solving problems inherent to the sampling and pre-treatment of the matrices to be analysed.
- Acquiring detailed specific knowledge regarding the characteristics and functioning of complex analytical instruments used in chemical analysis laboratories, for the characterization of different matrices and for the identification of pollutants present even at the trace level.
- Using statistical and IT methods for Quality Control, Experimental Design, Chemometric techniques.
- Comparing different methods in order to choose the most appropriate one in relation to the sample to be analysed.
· Formulating analyses' protocols.
Single course

This course can be attended as a single course.

Course syllabus and organization

Single session

Responsible
Lesson period
First semester
Course syllabus
Theory lessons (6 ECTS - 48 hours)
DESIGN of the ANALYSIS and TREATMENT of ANALYTICAL DATA
Principles of design of experiment. Statistical thinking for analytical problem solving. Experimental design and OFAT method. Full and fractional factorial method. Screening Design. Response Surface Experiments (Central Composite). Sequential Experimentation. Use of the JMP Program.
Quality control principles. Quality control of chemical products and processes. The seven classic tools for quality control: Flow Charts, Control Charts, Scatter Plots, Cause-Effect Diagrams (Ishikawa), Pareto Diagrams, Histograms, Check Sheets. Notes on the ISO 9001 Standard for Quality Control.
Principles of chemometrics and multivariate analysis. Acquisition and processing of analytical data. From data to information for knowledge and awareness. Principles of multivariate analysis. Principal component analysis (PCA). Independent component analysis (ICA). Cluster analysis. Classification. Regression methods: ordinary (calibration plot, analyte addition, standard addition); non-ordinary (PCR, PLS). Artificial Neural Networks (ANN). Using of the R Program.
TREATMENT of the ANALYTICAL SAMPLE
Methods of sampling and treatment of the sample with particular reference to the elimination of interferences and concentration of the analytes; applications in various fields including the environmental and food sectors. Active and passive sampling techniques and emissions.
ADVANCED ANALYTICAL TECHNIQUES
Advanced applications of elemental analysis techniques including ICP-MS and LA-ICP-MS for the quantification of trace metals with applications in the environmental and cultural heritage fields.
Advanced chromatographic methods (UHPLC, triple quadrupole LC-MS) with insights and applications (analysis of plant protection products, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, dioxins, analysis of substances of abuse); introduction to protein profiling.
Sensors and biosensors: definitions, enzymatic sensors, affinity sensors, nucleic acid based sensors, nanomaterials and sensors, thermochemical sensors, potentiometric sensors, semiconductor based sensors, chemoresistors, amperometric sensors, impedance sensors, optical sensors, acoustic sensors.
Multivariate analysis for sensors.
Applications of evolved gas analysis (EGA) methods such as thermo-optical methods and infrared spectroscopy coupled with thermogravimetric analysis and gas chromatography (TGA-FTIR-GC-MS).
Applications of advanced SEM-EDX techniques which require the acquisition of maps, profiles and 3D reconstruction of the sample.
Advanced molecular spectroscopy methods (spectral imaging techniques and multi-spectral and hyper-spectral analysis); applications to the study of the surface distribution of chemical species; non-destructive on-site analysis with applications.
For the different analytical techniques proposed, applications for the quantification of both inorganic and organic substances will be illustrated in the field of the study of environmental matrices (analysis of atmospheric pollutants both solid and in the gas phase, water and soil pollutants) and food (with particular reference to the quantification of toxic substances) as well as in the characterization of materials, including applications for the analysis of cultural heritage.
Laboratory (3 ECTS - 48 hours)
The laboratory will be structured in three phases and will be closely related to what was covered during the theoretical lessons.
FIRST PHASE (in the computer laboratory): the application of the experimental design will be treated in order to optimize the parameters that will be set in the subsequent analysis phase. For this purpose, exercises will be carried out on a PC with the help of the JMP program.
SECOND PHASE (in the chemical laboratory): laboratory experiments will be performed (previously optimized with the experimental design). These experiments will generally focus on the quantification of trace analytes in environmental and/or food matrices and on the characterization of artefacts of historical and artistic interest. The techniques used will mainly be methodologies of elemental analysis, spectroscopic techniques, use of sensors and biosensors and advanced chromatographic techniques. The problem of sample preparation will also be addressed in detail.
THIRD PHASE (in the computer laboratory): the results acquired in the second phase will be processed through the use of chemometric techniques of multivariate analysis, after learning how to use dedicated softwares.
Prerequisites for admission
Fundamentals of general and inorganic chemistry, stoichiometry, mathematics (knowledge deriving from a L27 type three-year Bachelor degree).
Knowledge of analytical chemistry with particular reference to instrumental analytical chemistry. This knowledge is generally acquired in the Analytical Chemistry I and Analytical Chemistry II courses of the Bachelor's Degree in Chemistry.
Knowledge that could be very useful is that acquired in the course of Environmental Chemistry and Advanced Electroanalytical Chemistry.
Teaching methods
Frontal lessons integrated with WOOCLAP, Exercises on MyARIEL/MOODLE platform, numerical exercises on PC (with the aid of specific programs for Quality Control, Experimental Design, Chemometrics), laboratory experiences.
In addition, some seminars are held by experts who may come from companies operating in the instrumental analytical chemistry sector or from qualified research institutes; during the seminars, practical demonstrations with portable analytical instruments will also be carried out, if possible.
Teaching Resources
Power Point presentations of lessons, model spreadsheets, solved exercises, experimental laboratory methods. All this material can be downloaded from the teachers' MyARIEL website.
Recommended reference texts:
· Kaoru Ishikawa, Guide to Quality Control, Asian Productivity Organization.
· R. Todeschini, Introduzione alla chemiometria, (https://michem.unimib.it/wp-content/uploads/sites/43/2019/04/introduzione_alla_chemiometria.pdf).
· P. Patnaik, Handbook of environmental analysis, chemical pollutants air, water, soil and solid wastes, CRC Press.
· F. W. Fifield, Environmental analytical chemistry, Balckwell Science
· F.B. Bănică, Chemical Sensors and Biosensors: Fundamentals and Applications, Wiley-VCH.
· B.R. Eggins, Chemical Sensors and Biosensors, Wiley-VCH.
Assessment methods and Criteria
Written exam (2 hours) based on 6 open-ended questions. Grade is given in thirtieths (each question is worth 5 points).
CHIM/01 - ANALYTICAL CHEMISTRY - University credits: 9
Single bench laboratory practical: 48 hours
Lessons: 48 hours
Shifts:
Turno
Professors: Falciola Luigi, Fermo Paola
Professor(s)
Reception:
Every Day from Monday to Friday, 9-18, by appointment
by Professor's Office in via Golgi 19, Building 5A, West Wing (Electrochemistry), III floor, room 3114-O