Learning objectives
• Learning the fundamental concepts of analytical chemistry related to the analytical process, measurement quality, and calibration.
• Knowledge of the principles of operation of spectrophotometric techniques based on UV-visible and infrared radiation absorption, and on fluorescence emission, including qualitative and quantitative analysis.
• Knowledge of the fundamental concepts and principles of operation of electroanalytical techniques based on potential (potentiometry) and current (voltammetry) measurements.
• Evaluation and interpretation of the experimental data and the results of an analysis.
• Evaluation and correct usage of analytical information in the context of materials science.
The student:
• Will acquire the main concepts of analytical chemistry and learn to correctly present, process, and interpret the results of an analytical procedure.
• Will acquire the physicochemical principles underlying the instrumental spectrophotometric and electroanalytical techniques presented in the course.
• Will learn the principle of operation and the instrumental configuration of such techniques, learning the type of information that is possible to obtain from their application, especially in the context of materials science.
• Will acquire notions in chemometrics necessary to interpret the analytical data and correctly evaluate the results of an analysis.
• Will develop critical thinking and be able to assess the potential and the limitations of the presented techniques, developing the ability to tackle analytical problems in the context of materials science.
• Will be able to properly apply the acquired knowledge to the development of qualitative and quantitative methods in the context of materials science.
• Will develop adequate communication skills and use the correct terminology
• will grow independent thinking and will be able to re-elaborate notions from the textbooks and the lecture notes.
Prerequisites
General and Inorganic Chemistry
Mathematics I
Course unit content
1) Analytical process: terminology and procedures.
2) Analytical measurements: concentrations, dilutions, parameters of measurement quality.
3) Overview of chemometrics: distributions and statistical tests for the interpretation of the results.
4) Calibration: general concepts and methods.
5) Spectrophotometric techniques: UV-vis, IR and fluorescence spectrophotometry.
6) Electroanalytical measurements: fundamentals of electrochemistry, potentiometry, voltammetry.
7) Zeta potential measurements.
Laboratory: exercises on data processing and calibration curves, UV-vis and IR spectrophotometric analysis in the context of materials science problems, characterization of the surface functionalization of nanomaterials through zeta potential measurements.
Full programme
Analytical process: sampling, sample treatment, analysis, interpretation of results, qualitative and quantitative analysis.
Analytical measurements: expression and calculation of concentrations, units of measurement, conversions, dilutions, preparation of working solutions, significant figures, random and systematic error, precision, accuracy, specificity, limit of detection and quantification.
Chemometrics: population and sample, Gaussian distribution, confidence interval, comparison of sample means (t-test), paired t-test, analysis of variance, F test.
Calibration: calibration curves and least squares method, linearity and dynamic ranges, external standard method, standard additions method.
UV-vis spectrophotometry: interaction between electromagnetic radiation and molecules, electronic transitions, absorption bands, transmittance and absorbance, Lambert-Beer law, limitations and deviations, instrumentation, qualitative and quantitative measurements.
Fluorescence spectrophotometry: origin of fluorescence and phosphorescence phenomena, Jablonsky diagram, Stokes shift, Kasha rule, mirror image rule, lifetime and quantum yield, quenching mechanisms, Stern-Volmer equation, instrumentation, quantitative fluorescence measurements.
IR spectrophotometry: molecular vibrations, classical and quantized harmonic oscillator model, selection rules, anharmonic oscillator, normal modes of vibration, active modes, interpretation of IR spectra and qualitative analysis, instrumentation, Michelson interferometer, measurements in total attenuated reflectance modality.
Electroanalytical measurements: charge, current, voltage and free energy, galvanic cells, standard reduction potentials, Nernst equation, potentiometry, reference electrodes, ion-selective electrodes, glass electrode, membrane electrodes, selectivity coefficient, voltammetry, three-electrode setup, current e reaction kinetics, mass transportation and limiting current, quantitative measurements, polarography, faradic and non-faradic currents, square wave voltammetry, differential pulse voltammetry, stripping analysis, cyclic voltammetry.
Zeta potential measurements: Stern layer and slipping layer, definition of zeta potential, electrophoretic light scattering measurements, Henry’s equation, characterization of the surface functionalization of nanomaterials.
Laboratory: exercises on data processing and calibration curves, UV-vis and IR spectrophotometric analysis in the context of materials science problems, characterization of the surface functionalization of nanomaterials through zeta potential measurements.
Bibliography
Quantitative Chemical Analysis - Daniel C. Harris.
Principle of Instrumental Analysis - Skoog, Holler, Crouch (Skoog, Leary).
Lecture material.
Teaching methods
In-person lectures, including classroom exercises and laboratory experiences.
