COURSE GOALS: Training the students to acquire the more complex methods in synthesis of inorganic compounds by guiding them to prepare and isolate more complex compounds as well as to overwhelm particular instrumental methods of compounds characterization.To teach the students the fundamentals of instrumental methods which are used in qualitative and quantitative analyses and help them acquire experimental skilfulness.
LEARNING OUTCOMES AT THE LEVEL OF THE PROGRAMME:
1. KNOWLEDGE AND UNDERSTANDING
1.2. demonstrate a thorough knowledge and understanding of the fundamental concepts in chemistry
1.4. demonstrate a thorough knowledge and understanding of the most important chemistry laws and theories
1.5. demonstrate knowledge and understanding of basic experimental methods, instruments and methods of experimental data processing in physics and chemistry
2. APPLYING KNOWLEDGE AND UNDERSTANDING
2.2. describe important aspects of chemical change
2.4. recognize and follow the logic of arguments, evaluate the adequacy of arguments and construct well supported arguments
2.7. apply basic laboratory safety and security measures
4. COMMUNICATION SKILLS
4.2. present complex ideas clearly and concisely
4.4. use the written and oral English language communication skills that are essential for pursuing a career in physics, chemistry and education
5. LEARNING SKILLS
5.1. search for and use professional literature as well as any other sources of relevant information
LEARNING OUTCOMES SPECIFIC FOR THE COURSE:
Students will be able:
1. to perform more complex methods for synthesis of particular inorganic compound,
2. to plan the synthesis depending of the reaction conditions or desired compound property (apparatus selection and mind all safety precautions that ought to be done),
3. to find the optimal conditions for performing the reaction and efficient isolation of the product, its purification and identification,
4. to handle with most of available instruments for characterizing of the compound regarding its physical and chemical properties and critically discuss obtained results,
5. to introduce new ideas clearly and concise,
6. to obtain high?quality data of analysis,
7. use English language in communication, in literature scanning and writing the professional and scientific papers,
8. on the basis of achieved fundamental knowledge student will be able to suggest the mini-projects for teaching chemistry by discovering as backbone of their future work with pupils in the schools.
COURSE DESCRIPTION:
1. Chromium(V) and chromium(III) complexes
1.1. Preparation of K3CrO8 and determination of potassium as K[B(C6H5)4]
1.2. Preparation of cis-K[Cr(C2O4)2(H2O)2].2H2O and determination of oxalate and chromium content in the complex
2. Iron(I) Complexes
2.1. Preparation of [Fe(NO)(S2CNEt)2]
3. Cobalt(III) Complexes
3.1. Preparation of [Co(NH2CH2CH2NH2)3].1/2NaCl.3H2O
3.2. Preparation of [CoCl(C4H7N2O2(C5H5N)]
3.3. Preparation of [Co(NH3)5(NO3)](NO3)2
3.4. Preparation of [Co(NH3)5(H2O)]I3
4. Double salts of manganese(II)
4.1. Preparation of (NH4)2Mn(SO4)2.6H2O
5. Copper(II) Complexes
5.1. Preparation of [Cu(HOCH2CH(NH2)CO2(C12H8N2)]2SO4
5.2. Preparation of [Cu(C3H2O4)(H2O)(C12H8N2)].H2O
5.3. Preparation of [Cu(C5H5N)4]S2O8.
6. Nickel(II) Complexes
6.1. Preparation of [NiCl2(PPh3)2] (PPh3 = P (C6H5)3)
6.2. Preparation of [Ni(NH3)4(NO2)2]
7. Recording and interpretation of the IR spectra (of two samples
8. Investigation the thermal stability of complex (TG/DTG/DSC analysis of two samples)
9. Determination metal to ligand ratio in complex with Job?s method (continual variation method) and by molar ratio method.
10. Determination of amount of iron and aluminium in same solution by derivative spectrophotometric method.
11. Determination of aluminium in water by spectrofluorimetric method. Standard addition method.
12. Determination of amount of iron in complex by quenching of fluorescence and HPLC method. Statistical analytical data treatment and evaluation
13. Extraction of vanadium with 1?phenyl-2-methyl-3-hydroxy-4-pyridone dissolved in chloroform
14. Analysis of C-vitamin drug with HPLC method. Recording and interpretation of the IR and Raman spectra of naringenin.
15. The seminar: the student should elaborate of one selected scientific manuscript.
REQUIREMENTS FOR STUDENTS:
Regular attendance at the laboratory, taking the partial exams prior the performing the exercises and submission of written reports after the laboratory work.
GRADING AND ASSESSING THE WORK OF STUDENTS:
Attending the course, high quality preparation for planned experiment, successful performing of all required exercises, writing the reports of all performed exercises. Final exam. During the course by attending the preliminary exams one can acquit the final exam.
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- Z. Popović, B.-M. Kukovec, Viši praktikum iz kemije, Upute za internu upotrebu, PMF, 2009., Zagreb
2. D. A. Skoog, D. M. West, F. J. Holler, Uvod u kromatografske metode, Osnove analitičke kemije, 1. izd., Školska knjiga, Zagreb 1999.
3. G. S. Girolami, T. B. Rauchfuss, R. J. Angelici, Synthesis and Techniques in Inorganic Chemistry, 3rd Ed., University Science Books Sausalito, 1999.
4. W. L. Jolly, The Synthesis and Characterization of Inorganic Compounds, Waveland Press, 1991.
5. D. L. Pavia, G. M. Lampman, G. S. Kriz, Introduction to Spectroscopy, 3rd Ed., Harcourt, Inc. Orlando, USA, 2001.
6. Infrared and Raman Spectroscopy, Methods and Applications, Ed. B. Schrader, VCH Publishers, New York, 1995.
7. E. de Hoffmann, V. Stroobant, Mass Spectrometry, 2nd Ed., John Wiley& Sons, Chichester, UK, 2002.
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