Ateneo - UPO

The course is divided into three modules, the contents of which are listed below:
1) Mass spectrometry: General principles and basic instrumental aspects of mass spectrometry: Ionization techniques and detector. Basic rules for the interpretation of spectra
2) Optical spectroscopies: theory on vibrational (IR and Raman) and electronic spectroscopies both in absorption and emission (fluorescence, phosphorescence). A hint to adsorption of probe molecules to study the surface sites.
3) Magnetic Resonance Techniques: physical principles of Nuclear Magnetic Resonance, spectral analysis and structural determination of simple metal complexes and inorganic compounds will be developed. Particular attention will also be paid to the study of electron paramagnetic resonance spectroscopy (EPR) in inorganic chemistry.

• Slides
• Daniel C. Harris, Chimica Analitica quantitativa Zanichelli Editore (ISBN 9788808821058, ed. cartacea)
• G.D. Christian, P. K. Dasgupta, KA Schug, Analytical Chemistry seventh edition, Wiley, (ISBN 978-0-470-88757-8)
Online course on the site: http://www.cis.rit.edu/htbooks/nmr/inside.html (J.P. Hornak);
H. Friebolin, "Basic One- and Two-Dimensional NMR Spectroscopy", VCH.
M. Brustolon, E. Giamello, Electron Paramagnetic Resonance – A Practitioner's Toolkit, Ed. John Wiley & Sons, Inc., Hoboken, New Jersey, 2009.
M. Weller, T. Overton, J. Rourke, F. Armstrong, “The Inorganic Chemistry of Atkins”, Zanichelli.
N.B. Colthup, L.H. Daly, S.E. Wiberley, Introduction to Infrared and Raman Spectroscopy, Academic Press;

1) The course aims to provide knowledge on analytical mass spectrometry and to develop the ability to choose the right spectrometer according to the specific problem and the critical sense of students towards a problem of analytical chemistry.
Communication skills: acquire and know how to use an appropriate chemical vocabulary in relation to the topics covered in the course. Develop the ability to autonomously learn new notions on analytical mass spectrometry applications and to draw conclusions on the most appropriate choice in relation to the specific problem.
2) Acquisition of knowledge on the Identification of organic molecules and inorganic systems. Adsorption of probe molecules on surface sites and interpretation of the gas/solid interaction Interpretation of electronic spectra of transition metals and identification of the different type of electronic transitions.
3) Solid foundation of the principles of Nuclear Magnetic Resonance Spectroscopy and a preliminary knowledge of the basics of the EPR technique. Particular attention will be paid to the development of the ability to interpret one-dimensional and multinuclear spectra of simple inorganic compounds in the light of theoretical concepts.

Knowledge of the topics of General and Inorganic Chemistry, Physical Chemistry I and Analytical Chemistry.

Lectures integrated with some classroom exercises and related discussion and practice lessons in instrumental laboratories.

The concepts covered by the course will be discussed collegially in the classroom and applied directly during classroom exercises for the interpretation of spectra, obtained with the various spectroscopic techniques. The final examination will be the only learning control.

The evaluation is articulate on the three parts of the course:
1) Mass spectrometry: evaluation is based on an oral examination (the number of questions varies according to the preparation of the candidates)
2) Optical spectroscopies: oral exam; questions concerning the program. The capacities of the students in the spectra interpretation of organic or inorganic systems both materials will be also evaluated.
3) Magnetic Resonance Techniques: written exam of 2h consisting of 8 questions (which include both theoretical open questions and small exercises in the interpretation of spectra of inorganic compounds). The highest grade is achieved with solid knowledge and the ability to apply knowledge on all topics covered. The results of the exam highlight the degree of understanding of theoretical concepts and the degree of acquisition of an adequate technical-scientific language through the answers to the open questions. The autonomy of judgment is also assessed through the request to express judgments and make comparative choices, and the ability to learn independently.

1) Mass spectrometry: General principles and basic instrumental aspects of mass spectrometry. Ionization techniques. Low- and high-resolution mass spectrometers. Basic rules for the interpretation of spectra ESI-Ion Trap. Spectra Acquisition and interpretation.
2) Optical spectroscopies: Optical spectroscopies will be addressed from a theoretical and practical point of view. The vibrational spectroscopy (IR and Raman), with particular reference to the origin of group frequencies, of the overtones, of the combination bands and Fermi resonance will be explored. The bases will be provided for the understanding the vibrational spectra of polyatomic molecules, also with a certain structural complexity. The adsorption of probe molecules of a different nature for the spectroscopic study of surface sites and the characterization of the acidic properties, basic or redox will be treated. The principles of electron spectroscopic techniques of absorption (UV-Vis NIR) and emission (fluorescence and phosphorescence) will also be explained in the course. Special attention will be given to diffuse reflectance techniques.
3) Magnetic Resonance Techniques: Spectroscopic methods based on Magnetic Resonance for the study of the molecular structure and dynamic processes will be studied. Basic principles of the technique; nuclei in a magnetic field; resonance; population of nuclear spin levels; continuous wave experiment. Pulse NMR method: generalities, pulse angle, rotating coordinate system, Bloch equations, relaxation, Fourier transform. NMR parameters: chemical shift (diamagnetic, paramagnetic and local contributions) and coupling constants (geminal, vicinal, long-range, homo- and heteronuclear). Chemical and magnetic equivalence of nuclei. Order of an NMR spectrum. Examples of NMR spectra of multinuclear inorganic compounds. Brief outline of the basic principles of electronic paramagnetic resonance spectroscopy (EPR) and its application in the characterization of simple paramagnetic compounds.

Knowledge and understanding: knowledge of the theoretical bases of the different spectroscopic and spectrometry techniques and their applications; Ability to apply knowledge and understanding: ability to apply theoretical knowledge to the interpretation of spectra obtained from various spectroscopic and resonance techniques. Ability in identifying the most suitable spectrometer for a specific analytical problem. Autonomy of judgment: Ability to critically analyse the notions learned. Communication skills: ability to use appropriate scientific language in answering questions, in analysing spectral data; acquisition of an appropriate scientific language to communicate in a precise, concise and clear way. Learning skills: ability to use the teaching material for a critical and reasoned study that allows the subsequent autonomous acquisition of further knowledge in the field of spectroscopies.