SYNTHESIS TECHNIQUES IN INORGANIC CHEMISTRY
- Overview
- Assessment methods
- Learning objectives
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- Full programme
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The student must have a good knowledge of basic general and organic chemistry.
The examination includes a final written test of typically 3 h duration. The written test will be organized in the formulation of two questions concerning general topics discussed in the course. The final grade will take into account the accuracy and quality of the responses, the synthetic capacity of the candidate in presenting the required topics
The course aims to illustrate the techniques most commonly used in inorganic chemistry to the synthesis and spectroscopic characterization of molecular compounds containing transition metals. Theory, methods of measurement and interpretation of experimental data and some practical considerations are adequately described.
Lesson 1: group theory, with particular reference to the molecular symmetry, the reducible and irreducible representations and character tables.
Lesson 2: Application of group theory to the IR and Raman spectroscopy and interpretation of infrared spectra.
Lesson 3: Basic principles of nuclear magnetic resonance spectroscopy.
Definition of chemically and magnetically equivalent nuclei (spin system) and notes on the chemical shifts and coupling constants. Particular attention will also be devoted to the interpretation of NMR spectra of simple molecular compounds containing transition metals.
Lesson 4: UV-Vis, electronic structure and spectra of ions of transition metals.
Lesson 5: Explanation of experience that will be carried out in the laboratory.
Laboratory
The laboratory exercises will focus on the synthesis, characterization and reactivity of inorganic compounds.
1. Triphenylphosphine borane adduct
2. Bis (triphenylphosphine) copper (I) borohydride
3. Manganese (III) acetylacetonate
4. Bis(triphenylphosphine)nickel(II) chloride
5. Bis (N, N'-diethyldithiocarbamate) nitrosyl iron(II)
6. Bis (N,N-Diethylethylenediamine) copper (II) perchlorate
7. Thiocyanato bis(pyridine) triphenylphosphine copper(I)
8. Tetrakis(acetonitrile)copper(I) perchlorate
9. trans-{Fe(h2-H2)(H)[1,2-bis(diphenylphosphino)ethane]2}[BF4]
10. Copper(I) and Silver(I) Pyrazolate
Each inorganic compound synthesized will be characterized using the most common techniques for spectroscopic investigation. IR spectra (in solution and in the solid state), UV-Vis spectra and multinuclear NMR spectra (mainly 1H and 31P) will be recorded and interpreted. Where possible, for a further characterization of the derivative isolated, will be employed also techniques such as thermogravimetric analysis coupled with differential scanning calorimetry (TGA / DSC) and X-ray fluorescence
Lesson 1: group theory, with particular reference to the molecular symmetry, the reducible and irreducible representations and character tables.
Lesson 2: Application of group theory to the IR and Raman spectroscopy and interpretation of infrared spectra.
Lesson 3: Basic principles of nuclear magnetic resonance spectroscopy.
Definition of chemically and magnetically equivalent nuclei (spin system) and notes on the chemical shifts and coupling constants. Particular attention will also be devoted to the interpretation of NMR spectra of simple molecular compounds containing transition metals.
Lesson 4: UV-Vis, electronic structure and spectra of ions of transition metals.
Lesson 5: Explanation of experience that will be carried out in the laboratory.
Laboratory
The laboratory exercises will focus on the synthesis, characterization and reactivity of inorganic compounds.
1. Triphenylphosphine borane adduct
2. Bis (triphenylphosphine) copper (I) borohydride
3. Manganese (III) acetylacetonate
4. Bis(triphenylphosphine)nickel(II) chloride
5. Bis (N, N'-diethyldithiocarbamate) nitrosyl iron(II)
6. Bis (N,N-Diethylethylenediamine) copper (II) perchlorate
7. Thiocyanato bis(pyridine) triphenylphosphine copper(I)
8. Tetrakis(acetonitrile)copper(I) perchlorate
9. trans-{Fe(h2-H2)(H)[1,2-bis(diphenylphosphino)ethane]2}[BF4]
10. Copper(I) and Silver(I) Pyrazolate
Each inorganic compound synthesized will be characterized using the most common techniques for spectroscopic investigation. IR spectra (in solution and in the solid state), UV-Vis spectra and multinuclear NMR spectra (mainly 1H and 31P) will be recorded and interpreted. Where possible, for a further characterization of the derivative isolated, will be employed also techniques such as thermogravimetric analysis coupled with differential scanning calorimetry (TGA / DSC) and X-ray fluorescence
All the necessary educational materials, slides and handouts laboratory will have been previously given to students by the teacher.
The course uses lectures duration of 16 hours and will involve the use of a video projector with slides which will be projected and discussed regarding the different topics learned during the course. The laboratory will last for 48 hours and will consist of 10 experiences that will take place at the didactic laboratories of chemistry.
Every day at the teacher's office, by appointment made by e-mail at least on the day before that of the desired reception.