LABORATORY FOR INORGANIC CHEMISTRY
Learning outcomes of the course unit
At the end of the training activity the student should have acquired skills related to the preparation and characterization of inorganic and coordination compounds with transition metals.
In particular, the student will be able to 1) manage the glassware and laboratory equipment according to the synthesis to be performed; 2) set the synthesis of compounds (stoichiometric ratios, quantities of reagents, solvents); 3) to use spectroscopic techniques in order to characterize the obtained compounds; 4) use the reagents and products according to the current safety regulations (concerning the management, treatment and disposal of chemical products).
At the end of the course the student will be able to independently manage the preparation of simple inorganic and coordination compounds, and apply the acquired knowledge for the choice of chemical characterization techniques suitable for different compounds.
The student will also be able to draw up short scientific reports to communicate the results of the laboratory activities.
In particular, the following theoretical aspects will be addressed in the course: 1) basic concepts of coordination chemistry. 2) Design and use of ligands suitable for interaction with metal centers. 3) Description of the spectroscopic techniques commonly used for the characterization of coordination compounds: heteronuclear, IR and UV-visible NMR.
Knowledge of the basic concepts of the General and Inorganic Chemistry course.
Course contents summary
Inorganic Chemistry Laboratory: safety rules, synthesis of coordination compounds and their characterization by means of spectroscopic techniques.
Theory: coordination compounds, infrared spectroscopy, eteronuclear NMR spectroscopy, UV-vis spectroscopy, VSEPR theory and molecular geometries.
Preparation of cis-copper(II)bisglycinate monohydrate, preparation of trans-copper(II)bisglycinate. Kinetic and thermodynamic reaction control, solid state isomerization, IR spectroscopy. (4 hours)
Acetylacetone as ligand, preparation of [Al(acac)3] and [VO(acac)2]. Properties of Al3+ and VO2+, NMR and IR spectroscopies. (4 hours)
Preparation of a N,N bidentate ligand (CH2PyPz) by means of phase transfer catalysis, preparation of the [ZnCl2(CH2Pz2)] complex, Zn2+ properties, NMR spectroscopy. (4 hours)
Preparation of [Co(en)3]I3 by means of a partial asymmetric sysnthesis. Etylenediamine as ligand, chirality in coordination chemistry, polarimeter, inert and labile complexes, properties of Co2+ and Co3+, UV-vis spectroscopy. (4 +4 hours)
Spectroscopic characterization of the complexes (IR, NMR, UV-vis). (3+3+3 hours)
Theoretical lessons: safety rules, discussion of the practical experiences, UV-vis and IR spectroscopies in coordination chemistry, eteronuclear NMR (19F, 31P, 195Pt, 103Rh, etc.). VSEPR theory and molecular geometries.
1) Inorganic Chemistry (Shriver, Atkins)
2) Advanced Inorganic Chemistry (Cotton)
3) Chemistry of the Elements (Greenwood, Earnshaw)
4) Physical Methods in Advanced inorganic Chemistry (Hill, Day)
5) Infrared and Raman Spectra of Inorganic and Coordination Compounds (Nakamoto)
6) Spectrometric identification of organic compounds (Silverstein, Webster)
The course is divided in theoretical lesson and practical experiences
Theoretical lessons: 32 hours, description of the practical experiences and of the spectroscopic techniques.
Practical laboratory: 30 hours divided in 7 practical experiences.
Assessment methods and criteria
The comprehension of the subjects discussed in the course will be monitored with: 1) tests during the practical experiences (10 % weight), 2) written examination (90% weight), duration 2 h, concerning spectroscopic techniques and inorganic synthesis.
Oral examination and final evaluation is integrated with the course of Inorganic Chemistry.
Teaching material available on the web.