ADVANCED TECHNICAL AND ANALYTICAL LABORATORY - MOD.1

The course of Advanced Analytical Techniques and Laboratory is part of the training activities characterizing the Master's Degree Course in Chemistry and Sustainable Technologies, aimed at providing students with the appropriate preparation to study complex aspects in the chemical field in its various aspects and to propose original approaches for their resolution.

The course is divided into two modules (defined Module 1 and Module 2), each of them divided into theory classes (held in the classroom) and laboratory lessons. Both modules have common training objectives as listed below:

1. To provide knowledge on a wide spectrum of advanced electrochemical and coupled analytical techniques, the latter based, in particular, on inorganic and organic mass spectrometry.
2. To provide in-depth knowledge on the theoretical aspects that underlie the different analytical techniques taken into consideration, strengthening, if necessary, the basic contents already acquired in the previous study cycle.
3. Provide advanced and rigorous knowledge on how to deal with an analytical datum.
4. Provide knowledge on the instrumental apparatus and develop practical skills in order to perform an experimental measurement with the appropriate accuracy and precision.
5. Develop the ability to propose new approaches in the chemical-analytical field to solve complex problems related to the qualitative and quantitative determination of components in real matrices.
6. Develop skills to extract analytical information from instrumental signals obtained under limiting conditions.
7. Develop skills for associating IT skills with the instrumental apparatus to extract chemical-analytical information, even with automated and / or "on line" procedures.

The expected results are defined according to the different contents of the two modules in which the course of Advanced Analytical Techniques and laboratory is divided.

1. Knowledge and understanding
A) Knowledge and understanding of the fundamental laws on which the principles of the most modern static and dynamic electroanalytical techniques are based , reinforcing the theoretical principles already acquired in the Bachelor's Degree. In particular, the course provides advanced knowledge for the study of electrode processes with associated chemical reactions both in the homogeneous phase and in the interphase.
B) Knowledge and understanding of the instrumental elements to perform experimental measurements of electroanalytical type with awareness.

2. Ability to apply knowledge and understanding
A) Ability to use the laws and knowledge learned to establish, from a theoretical point of view, the performance and expected results from the use of dynamic electroanalytical techniques.
B) Knowing how to choose the most appropriate technique and analytical strategy for the electroanalytical study of simple and complex systems.

3. Ability to judge
A) Ability to evaluate the reliability of an analytical response even in the presence of interferences related to the complexity of the studied chemical matrices
B) Being able to verify the congruence between the experimental responses obtained in experiments conducted in the laboratory and the expected theoretical ones.

4. Communication skills
A) Knowing how to describe, both in written and oral form, the results obtained from the application of an analytical method and communicate them, with appropriate language, to specialists and non- specialists interlocutors.
B) Being able to argue, with appropriate scientific consistency, the validity of the conclusions extrapolated from a chemical-analytical study on various substances.

5. Learning skills
A) To develop the ability to integrate the innovations that emerge from the real world with the knowledge and skills acquired in the course of the course.

Elements of electrochemistry and general analytical chemistry.

Electrochemical systems and types of conductors. Inter-phase electrode-solution: double layer and its models. Electrodic potential: absolute. Potential of electrified surfaces: Galvani, Volta and superficial potentials. Electrochemical potential and its properties. Electrochemical cells. Thermodynamics of batteries. Experimental measurements of the electromotive force. Junction potential and calculation methods. Potential and its dependence in dynamic conditions. Overvoltage and Ohmic drop. Electrochemical cells with two and three electrodes. Faradic and capacitive current. Electrode reactions Classification. Charge transfer process and Butler-Volmer equation. Reversible, irreversible and quasi reversible electrode processes. Mass transport. Fick’s laws and equations. Concentration profiles at an infinite planar, spherical and hemispherical electrodes, and at disks having a finite size. Chronoamperometry (CA) with conventional electrodes and microelectrodes. Double pulse (DP). Sweep voltammetry: linear (LSV) and cyclic voltammetry (CV). Diagnostic criteria to classify electrode processes using CA, DP, LSV and CV. Equations of voltammograms for macro- and micro-electrodes. Electron transfer with associated chemical reactions and diagnostic criteria and parameters. Adsorption phenomena. Electrocatalysis. Elettrocristallizzation. Microelectrodes. Scanning Electrochemical Microscopy. Coulometry.
Laboratory.
Determination of experimental parameters contributing to the formation of liquid junction potentials: application of the Kohlrausch equation for the determination of equivalente conductivity at infinite dilution of strong electrolytes.
Construction of electrochemical cells providing with liquid junctions of I, II and III types. Use of potentiostats and determination of open circuit potentials and capacitive currents in various electrolytic solutions.
Use of the chronoamperometry for the determination of the exchange current through the use of macro- and micro-electrodes.
Use of the double pulse to determine whether or not an electrode process is under diffusion control: use of macro- and micro-electrodes.
Use of linear and cyclic scanning voltammetry to study the reversibility of electrode processes and to determine the heterogeneous charge transfer constant: use of macro- and micro-electrodes.
Preparation of an electrochemical sensor for the determination of electroactive species in synthetic and real samples.
Measurements using a scanning electrochemical microscope to characterize an electrode / solution inter-phase.

As support to the study, various texts of analytical instrumental Chemistry can be used at university level and in particular, the following texts are suggested:
-Instrumental Methods inElectrochemistry:" Southampton Electrochemical Group, Ellis Horwood seriesin Physical Electrochemistry .
-J. Wang, Analytical Electrochemistry, Wiley.
-M.A.Brett, O. Brett, Electrochemistry: principles, methods, and applications, Oxford University Press
-Lecture notes
-Free download of powerpoint presentation (Italian)

The assessment of the teaching activities related to the course of Advanced Analytical Techniques, module 1, is done through an oral test on the topics covered during the lectures (theoretical part) and the evaluation of written reports related to the experiences performed in the laboratory.
In particular, the oral exam consists of a series of open questions in which the theoretical aspects of the techniques, the different instrumental parts that characterize the techniques and the electroanalytical methods studied are discussed. The student will have to expose the various topics in a formally and scientifically correct language, demonstrating at the same time that he understood the link between the different theoretical aspects treated, and their correlation with the experiences carried out in the laboratory. Depending on the ability to discuss the required topics, the exam lasts between 45 to 60 minutes.
The final mark of the teaching activities of Advanced Analytical Techniques is composed of the arithmetic average of the marks obtained in the two different modules.

Teaching will take place through class and laboratory lessons.
In the class-room lectures (28 hours) the theoretical principles concerning static and dynamic electroanalytical techniques will be presented. Examples of types of questions will be given on which the exam will be performed; time to time texts / notes / handouts where better to study / deepen the topics covered will also be suggested.
The laboratory part (32 hours) includes a series of experimental measurements with the electroanalytical instrumentation available both in the teaching laboratories and in the research laboratory. Students will work in groups (3-4 people for each group). For each series of measurements, the various tools will be presented to the various groups of students beforehand. Information will be provided on the potential critical nature of the execution of some practical operations, on the appropriate use of materials, also in relation to the safety and toxicity of the chemical reagents used. Information on how to transfer data obtained from the instrumentations to spreadsheets for the subsequent processing of experimental data will be also provided.

Italian

Attendance to the laboratory course is mandatory and only one day of absence is admitted, however to be agreed with the teacher.

Accommodation and support services for students with disabilities and students with specific learning impairments:
Ca’ Foscari abides by Italian Law (Law 17/1999; Law 170/2010) regarding support services and accommodation available to students with disabilities. This includes students with mobility, visual, hearing and other disabilities (Law 17/1999), and specific learning impairments (Law 170/2010). In the case of disability or impairment that requires accommodations (i.e., alternate testing, readers, note takers or interpreters) please contact the Disability and Accessibility Offices in Student Services: disabilita@unive.it.

oral