Carmine GAETA | ADVANCED METHODS FOR STRUCTURAL CHARACTERIZATION
Carmine GAETA ADVANCED METHODS FOR STRUCTURAL CHARACTERIZATION
cod. 0522300039
ADVANCED METHODS FOR STRUCTURAL CHARACTERIZATION
| 0522300039 | |
| DEPARTMENT OF CHEMISTRY AND BIOLOGY "ADOLFO ZAMBELLI" | |
| EQF7 | |
| CHEMISTRY | |
| 2018/2019 |
| OBBLIGATORIO | |
| YEAR OF COURSE 1 | |
| YEAR OF DIDACTIC SYSTEM 2016 | |
| SECONDO SEMESTRE |
| SSD | CFU | HOURS | ACTIVITY | |
|---|---|---|---|---|
| CHIM/06 | 5 | 40 | LESSONS | |
| CHIM/06 | 1 | 12 | EXERCISES |
| Objectives | |
|---|---|
| THIS COURSE FOCUSES ON ADVANCED SPECTROSCOPIC METHODS, SUCH AS BIDIMENSIONAL NMR, CIRCULAR DICROISM, AND HIGH-RESOLUTION MASS SPECTROMETRY. AT THE END OF THE COURSE, THE STUDENT WILL KNOW THE ADVANCED SPECTROSCOPIC METHODS TO ABLE TO CARRY OUT THE STRUCTURAL DETERMINATION OF ORGANIC MOLECULES WITH CONFIDENCE. |
| Prerequisites | |
|---|---|
| ORGANIC CHEMISTRY AND FUNDAMENTALS OF NMR SPECTROSCOPY AND MASS SPECTROMETRY |
| Contents | |
|---|---|
| UV-VIS SPECTROSCOPY (6 HOURS). INTERACTION BETWEEN LIGHT AND MATTER : THE LAW OF LIGHT ABSORPTION- UV-VIS SPECTROSCOPY- THE NATURE OF ELECTRONIC EXCITATIONS – SELECTION RULES. THE EFFECT OF CONJUGATION – THE EFFECT OF CONJUGATION ONALKENES, POLYENES - THE WOODWARD-FIESER RULES FOR DIENES –CARBONYL COMPOUNDS, ENONES. THE WOODWARD-FIESER RULES FOR AROMATIC COMPOUNDS: AND SUBSTITUTED AROMATIC COMPOUNDS. AROMATIC POLYCICLIC COMPOUNDS. TRAINING EXERCISES. CHIROOPTICAL METHODS (4 HOURS). OPTICAL ROTATORY DISPERSION THEORY AND APPLICATIONS. CIRCULAR DICROISM THEORY. THE OCTANT RULE. EXCITON CHIRALITY METHOD: PRINCIPLES AND APPLICATIONS. CIRCULAR DICHROISM OF PEPTIDES AND PROTEINS. INTRODUCTION TO FLUORESCENCE SPECTROSCOPY (4 HOURS), JABLONSKI DIAGRAM, KASHA'S RULE, STOKES' SHIFT, MIRROR IMAGE RULE, NON-RADIATIVE DECAY PROCESSES, VIBRATIONAL RELAXATION, INTERNAL CONVERSION AND INTERSYSTEM CONVERSION, FLUORESCENCE QUENCHING, QUANTUM YIELD AND LIFE TIME, EXCIMER AND EXCIPLEXES. FRET AND APPLICATIONS OF FRET. IR SPECTROSCOPY (4 HOURS). IR SPECTROSCOPY AND MOLECULAR MODE VIBRATIONS. INFRARED ABSORPTION PROCESS. HOOKE'S LAW CHARACTERISTIC INFRARED BANDS OF HYDROCARBONS: ALKANES, ALKENES, ALKYNES AND AROMATIC COMPOUNDS. CHARACTERISTIC INFRARED BANDS OF DIFFERENT ORGANIC FUNCTIONAL GROUPS: ALCOHOLS AND PHENOLS, ETHERS, AMINES, ALKYL AND ARYL HALIDES. CARBONYL COMPOUNDS, FACTORS INFLUENCE THE CABONYL GROUP, ALDELYDES, KETONES, CARBOXYLIC ACIDS, ESTERS, AMIDES,ACID CHLORIDES, ANHYDRIDES. NITRILES,.NITRO COMPOUNDS. TRAINING EXERCISES. NMR (14 HOURS) FUNDAMENTALS OF NMR THEORY. NUCLEAR SPIN STATES, NUCLEAR MAGNETIC MOMENTS, ABSORPATION OF ENERGY, THE MECHANISM OF ABSORPATION (RESONANCE), THE CHEMICAL SHIFT AND SHIELDING, CHEMICAL AND MAGNETIC EQUIVALENCE AND NON-EQUIVALENCE. QUANTITATIVE 1H NMR. NMR OF DYNAMIC PROCESSES, NMR TIME SCALE, COALESCENCE TEMPERATURE, EYRING EQUATION AND KURALN-RUBIN-WISE EQUATION. TWO-DIMENSIONAL NMR SPECTROSCOPY: COSY, HSQC, HMBC, INADEQUATE, NOESY, ROESY, EXSY. EXAMPLES OF STRUCTURE ELUCIDATION BY NMR SPECTROSCOPY. DIFFUSION NMR:PGSE AND DOSY. HIGH RESOLUTION MASS SPECTROMETRY (8 HOURS). IONIZATION PROCES AND IONIZATION ENERGY. ISOTOPIC COMPOSITION, MASS ACCURACY, ACCURATE MASS, ISOTOPIC DISTRIBUTION, ISOTOPIC PATTERN. SEPARATING IONS BY M/Z, BASIC PRINCIPLES. TYPES OF MASS ANALYZERS AND THEIR MODES OF OPERATION. ELECTRON IONIZATION ION SOURCES. BASICS OF CHEMICAL IONIZATION (CI). ATMOSPHERIC PRESSURE CHEMICAL IONIZATION (APCI). ATMOSPHERIC PRESSURE PHOTOIONZATION (APPI). ION SOURCES AND ION FROMATION IN FAB. MALDI. ESI. ANALYZER FOR HR MASS SPECTROMETRY: FT ICR AND ORBITRAP. LABORATORY EXPERIENCES OF NMR (2H) AND MASS SPECTROMETRY (2H). TRAING EXERCISES IN CLASSROOM (8H) OF INTERPRETATION OF MR SPECTRAL DATA AND CALCULATION OF MAX USING WOODWARD-FIESER RULES IN THE UV SPECTRA OF ORGANIC COMPOUND. |
| Teaching Methods | |
|---|---|
| TEACHING METHODS. CLASSROOM LECTURES FOR A TOTAL OF 40 H. LABORATORY EXPERIENCES OF NMR (2H) AND MASS SPECTROMETRY (2H). TRAING EXERCISES IN CLASSROOM (8H) OF INTERPRETATION OF MR SPECTRAL DATA AND CALCULATION OF MAX USING WOODWARD-FIESER RULES IN THE UV SPECTRA OF ORGANIC COMPOUND. |
| Verification of learning | |
|---|---|
| THE AIM OF THE FINAL EXAM IS TO CHECK THAT THE LEARNING OUTCOMES HAVE BEEN ACHIEVED. MINIMUM THRESHOLD OF 18 UP TO A MAXIMUM VALUE OF 30. EXAMINATION METHODS: WRITE AND ORAL. THE EXAM CONSISTS OF A WRITTEN TEST FOLLOWED BY AN ORAL DISCUSSION. THE WRITTEN EXAMINATION CONSISTS IN TWO PARTS A AND B. PART A: AN EXERCISE FOR APPLICATION OF THE WOODWARD-FRIESMAN'S RULE. PART B: ASSIGNMENT OF 1D AND 2D NMR SPECTRA OF A KNOWN COMPOUND. A MINIMUM THRESHOLD OF 18/30 FOR THE WRITTEN TEST MUST BE REACHED IN ORDER TO BE ALLOWED TO ATTEND THE ORAL DISCUSSION. ORAL PART: CONCERNS QUESTIONS ABOUT THE THEORETICAL CONTENTS OF THE COURSE. |
| Texts | |
|---|---|
| 1) METODI SPETTROSCOPICI IN CHIMICA ORGANICA (SECONDA EDIZIONE). MANFRED HESSE, HERBERT MEIER AND BERND ZEEH. 2) T.D.W. CLARIDGE, HIGH-RESOLUTION TECHNIQUES NMR IN ORGANIC CHEMISTRY, PERGAMON, 1999. 3) A.E. DEROME, MODERN NMR TECHNIQUES FOR CHEMISTRY RESEARCH, PERGAMON PRESS, 1987. 4)H. FRIEBOLIN, BASIC ONE- AND TWO-DIMENSIONAL NMR SPECTROSCOPY, VCH PUBLISHERS, 1991. 5) J.K.M. SANDERS, B.K. HUNTER, MODERN NMR SPECTROSCOPY - A GUIDE FOR CHEMISTS, 2ND EDITION, OXFORD UNIVERSITY PRESS, 1993. 6) E. BREITMAIER, W. VOELTER, CARBON-13 NMR SPECTROSCOPY, 3RD EDITION, VCH PUBLISHERS, 1989. 7) APPUNTI DALLE LEZIONI. |
| More Information | |
|---|---|
| PROF. CARMINE GAETA, CGAETA@UNISA.IT, 089969556 |
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