Unit METHODS FOR THE CHARACTERIZATION OF INORGANIC COMPOUNDS
- Course
- Chemical sciences
- Study-unit Code
- A001116
- Curriculum
- Chimica inorganica per l'energia e la catalisi
- Teacher
- Cristiano Zuccaccia
- Teachers
-
- Cristiano Zuccaccia
- Hours
- 52 ore - Cristiano Zuccaccia
- CFU
- 6
- Course Regulation
- Coorte 2022
- Offered
- 2022/23
- Learning activities
- Caratterizzante
- Area
- Discipline chimiche inorganiche e chimico-fisiche
- Academic discipline
- CHIM/03
- Type of study-unit
- Obbligatorio (Required)
- Type of learning activities
- Attività formativa monodisciplinare
- Language of instruction
- Italian
- Contents
- Basic principles of nuclear magnetic resonance (NMR) spectroscopy. Single and double resonance one-dimensional techniques. Multidimensional techniques: connection through bonds (COSY, HSQC, HMQC and HMBC); connection through space: NOESY, HOESY, ROESY; connection through chemical exchange (EXSY). Advanced techniques for investigating supramolecular systems: PGSE and DOSY. Basic principles and applications of electronic paramagnetic resonance spectroscopy (EPR): EPR spectra of organic radicals, inorganic radicals and transition metal complexes; brief notes on advanced techniques, multi-pulse techniques and double-resonance techniques.
- Reference texts
- Notes provided by the teacher
- Educational objectives
- The main target of the course is to provide the student with basic and advanced concepts concerning the most common methods for structural analysis at the molecular level with specific reference to inorganic and organometallic systems. To this end, mainly nuclear magnetic resonance (NMR) and electron paramagnetic resonance (EPR) spectroscopic techniques will be discussed. After a brief introduction to recall the basic principles, the student will be guided towards the deepening of more advanced methodologies based on both single- and two-dimensional experiments (NMR). The acquired knowledge will allow the student to critically analyze of the results of both simple and more complex spectroscopic experiments, and acquire the necessary skills to design further experiments to face problems concerning the molecular and supramolecular structure of inorganic systems, also in reference to their reactivity. Furthermore, brief notes to other techniques such as vibrational spectroscopy, electron spectroscopy and mass spectrometry will be given, with particular emphasis on their inorganic applications. The theoretical lessons will be flanked by laboratory sessions (especially NMR) in which the student will be able to better understand the potentialities and the experimental limitations of the techniques covered during the course, using inorganic or organometallic systems also synthesized by the student himself.
- Prerequisites
- Basic knowledge of the interaction phenomena between electromagnetic radiation and matter
- Teaching methods
- The course includes both theoretical lessons in the classroom and experimental sessions.
- Other information
- In each of the exam periods planned according to the calendar of teaching activities, at least a couple of dates are scheduled for the exam. Students are required to register for the exam following the University procedure. In case of problems and difficulties students are invited to contact the teachers. The student can participate in all the required exam tests.
- Learning verification modality
- The final evaluation consists in an oral interview, with the purpose of verifying the acquired knowledge and the ability of the student to re-elaborate the contents proposed during the course in a correct form.
For information on support services for students with disabilities and / or DSA visit http://www.unipg.it/disabilita-e-dsa - Extended program
- - Basic principles of nuclear magnetic resonance (NMR): energy levels, resonance condition, theory of chemical shift, the vector model, the Fourier transform and data processing.
- Monodimensional techniques: the basic sequence 90 ° -FID, longitudinal relaxation (T1) and inversion recovery, transverse relaxation (T2) and spin-echo, sensitivity optimization.
- Scalar coupling theory, decoupling, double resonance techniques, multiple pulse sequences (SPT, SPI, INEPT, DEPT ...)
- Introduction to multidimensional techniques: general scheme of a 2D experiment preparation, evolution, mixing and acquisition periods.
- Connection through chemical bonds: correlation through single bonds (COSY spectra, HSQC and HMQC spectra), correlation through multiple bonds (HMBC spectra).
- Connection through space: principles of dipolar coupling and nuclear Overhauser effect, steady state and kinetic NOE experiments, estimation of internuclear distances, two-dimensional experiments (NOESY and ROESY).
- Investigations of dynamic motions and reactivity in inorganic and organometallic systems with NMR techniques.
- Basic principles of electron paramagnetic resonance (EPR): electron magnetic moment and electronic levels; coupling with nuclear spin and hyperfine structure; relaxation; the EPR spectra of organic, inorganic radicals and transition metal complexes; brief notes on advanced techniques, multi-pulse techniques and double-resonance techniques.
- Laboratory sessions: structural characterization of transition metal complexes using advanced NMR techniques. The part dedicated to the laboratory will be mainly used to illustrate the components of a Fourier transform NMR spectrometer and to train the student about the acquisition, processing and interpretation of the main 1D and 2D NMR experiments in homogeneous liquid phase. Furthermore, the student (or groups of students) will have the opportunity to perform NMR experiments on samples prepared by the student himself in the laboratory and to deepen its structural characterization also in reference to the in situ monitoring of their reactivity.