Analytical Chemistry

Theory lessons (6 ECTS - 48 hours)
DESIGN of the ANALYSIS and TREATMENT of ANALYTICAL DATA with the Quality by Design (QbD) approach.
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 2 parts and will be closely related to what was covered during the theoretical lessons.
FIRST PART (in the computer laboratory): within the Quality by Design approach, the application of experimental design will be discussed in order to optimize experimental parameters (some of which will be used in the chemical laboratory). For this purpose, exercises will be done on PC with the aid of the JMP program. The concepts of Quality Control will be applied, using the EXCEL Program or other programs suitable for the purpose. Software (e.g. CAT) will be presented and used for the use of chemometric techniques of multivariate analysis.
SECOND PART (in the chemical laboratory): laboratory experiments will be performed (some of them 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.