DEVI AHILYA VISHWAVIDYALAYA, DAVV INDORE Syllabus
M.Sc. (CHEMISTRY) Fourth-4th-IV Semester Curriculum/ Syllabus
MCH-407: PRACTICAL Syllabus
Inorganic Chemistry
Preparation
Preparation of selected inorganic compounds and their study by IR, electronic spectra, Mossbauer. ESR and magnetic susceptibility measurements. Handiling of air and moisture sensitive compounds involving vacuum lines. Selection can be made from the following :
1. Sodium amide. Inorg. Synth., 1946, 2, 128.
2. Synthesis and thermal analysis of group II metal oxalate hydrate. J. Chem. Ed., 1988, 65, 1024.
3. Atomic absorption analysis of Mg and Ca.
4. Trialkoxyboanes-IR and NMR spectra.
5. PhBd2 Dichlorophenylborane - Synthesis in vacuum line.
6. Preparation of Tin (IV) iodide, Tin (IV) chloride and Tin (II) iodide, Inorge, Synth., 1953, 4.119.
7. Relative stability of Tin (IV) and Pb (IV). Preparation of ammonium hexachlorostannate (NH4)2 SnCl6 ammonium hexachlorophlumbate (NH4)2PbCl6.
8. Hexa-bis (4,nitrophenoxy) cyclotriphosphazene.
9. Synthesis of trichlorodiphenylantimony (V) hydrate. Inorg. Synths., 1985, 23, 194
10. Sodium tetrathionate Na2S4O6.
11. Metal complexes of dimethyl sulfoxide (IR) : CuCl2.2DMSO, PdCl2. 2DMSO, RuCl2. 4DMSO. J.Chem. Educ., 1982, 59, 57.
12. Synthesis of metal acethylacetonate : Magnetic moment, IR, NMR, Inorg. Synths, 1957, 5, 130, 1963, 1, 183.
13. Bromination of Cr (acac)3. J. Chem. Edu., 1986, 63, 90.
14. Magnetic moment of Cu (acac)2H2O.
15. Cis and Trns [Co(en)2CI2]+.
16. Separation of optical isomer of cis-[Co(en)2CI2]CI.J. Chem. Soc., 1960. 4369.
17. Ion exchange separation of oxidation state of vanadium. J. Chem. Educ., 1980, 57, 316; 1978, 55, 55.
18. Determination of Cr (III) complexes. [Cr(H2O)6]NO3.3HO, [Cr(H2O)4Cl2]Cl.2H2O,
[Cr(en)3]Cl3, Cr(acac)3. Inorg. synths., 1972, 13, 184.
19. Preparation of N, N bis (salicycladehyde) ethylenedimine, salen H2. Co(Salen) J. Chem. Educ., 1977, 54, 443; 1973, 50, 670.
20. Preparation of Fe(II) chloride (use it as Friedel-Craft chlorination source) J. Org. Chem., 1978, 43, 2423; J. Chem. Edu., 1984, 61, 645; 1986, 63, 361.
21. Reaction of Cr(III) with a multidentate ligand; a kinetics experiment (visible spectra Cr- EDTA complex) J.A.C.S., 1953, 75, 6570.
22. Preparation and use of Ferrocene. J. Chem. Edu. 1966, 43, 73; 1976, 53, 730.
23. Preparation of copper glycine complex-cis and trans bis (glycinato Copper (II). J. Chem. soc. Dalton, 1979, 1901, J. Chem. Edu., 1982, 59, 1052.
24. Preparation of phosphine Ph3P and its transition metal complexes.
25. Any other experimetn such as conversion of p-xylene to terephtalic acid catalyzed by CoBr2 (homogeneous catalysis).
26. Preparation of [Co(phenathroline-5,6 quinone)].
Spectrophotometric Determinations
a. Manganese/Chromium/Vanadium in steel sample.
b. Nickel/molybdenum/tungston/vanadium/uranium by extractive spectrophotometric method.
c. Fluoride/nitrite/phosphate.
d. Zirconium-alizarin Red-S complex : Mole-ratio method.
e. Copper-Ethylene diamine complex : Slope-ratio method.
f. Iron-phenanthroline complex : Job's method of continuous variations.
Flame Photometric Determinations
a. Sodium and potassium when present together.
b. Lithium/calsium/barium/strontium.
c. Cadmium and magnesium in tap water.
Chromatographic Separations
a. Cadium and zinc
b. Zinc and magnesium.
c. Thin-layer chromatography-separation of nickel, manganeses, cobalt and zinc. Determination of Rf values.
d. Separation and identification of the sugars present in the given mixture of glucose, fructorse and sucrose by paper chromatography and determination of Rf values.
Organic Chemistry
Qualitative Analysis
Separation, purification and identification of the components of a mixture of three organic compounds (three solids or two liquids and one solid or two solids and one liquid), using tc for checking the purity of the separated compounds, chemical analysis, IR, PMR and mass spectral data.
Multi-step Synthesis of Organic Compounds
The exercise should illustrate the use of organic reagents and may involve purification of the products by chromatographic techniques. Photochemical reaction Benzophenone -> Benzpinacol
_> Benzpinacolone Beckmann rearrangement : Benzanilide from benzene Benzene -> Benzophenone -> Benzphenone oxime -> Benzanilide Benzilic acid rearrangement : Benzilic acid from benzoin Benzoin -> Benzil -> Benzilic acid Synthesis of heterocyclic compounds Skraup synthesis : Preparation of quinoline from aniline Fisher Indole synthesis : Preparation of
2-phenylindole from phenylhydrazine. Enzymatic synthesis Enzymatic synthesis Enzymatic reduction : reduction of ethyl acetoacetate using Baker's yeast to yield enantiomeric excess of S (+) ehtyl-3-hydroxybutanoate and determine its optical purity. Biosynthesis of ethanol from sucrose. Synthesis using microwave Alkylation of diethyl malonate with benzyl chloride. Synthesis using phase transfer catalyst. Alkylation of diethyl malonate or ethyl acetoacetate with
an alkylhalide.
Extraction of Organic Compounds from Natural Sources
1. Isolation of caffeine from tea leaves.
2. Isolation of casein from milk (the students are required to try some typical colour reactions of proteins).
3. Isolation of lactose from milk (purity of sugar should be checked by LC and PC and Rf values reported).
4. Isolation of nicotine dipicrate from tobacco.
5. Isolation of cinchonine from cinchona bark.
6. Isolation of piperine from black pepper.
7. Isolation of lycopene from tomatoes.
8. Isolation of b-carotene from carrots.
9. Isolation of oleic acid from olive oil (involving the preparation of complex with urea and separation of linoleic acid).
10. Isolation of eugenol from clove.
11. Isolation of (+) limonine from citrus rind.
Paper Chromatography
Separation of identification of the sugars present in the given mixture of glucose, fructose and surcrose by paper chromatography and determination of Rf values. Spectroscopy Identification of organic compounds by the analysis of their spectral data (UV, IR, PMR, CMR & MS) Spectrophotometric (UV/VIS) Estimations
1. Amino acids
2. Proteins
3. Carbohydrates
4. Cholesterol
5. Ascorbic acid
6. Aspirin
7. Caffeine
Physical Chemistry
Number of hours for each experiment : 3-4 hours. a list of experiments under different headings are given below. Typical experiments are to be selected from teach type. Physical chemistry Number of Hours to each experiment : 3 Hours. A list of experiments under different headings are given below. Typical experiments are to be selected from each type.
(A) Thermodynamics
i. Determination of partial molar volume of solute (e.g. KCl) and solvent in a binary mixture.
ii. Determination of the temperature dependence of the solubility of a compound in two solvents having similar intromolecular in tetractions (benzoic acid in water and in DMSO water mixture and calculate the partial molar heat of solution.
(B) Spectroscopy
iv. Determination of kPa of an indicator (e.g. methyl red) in (a) aqueous and (b) micellar media.
v. Determination of stoichiometry and stability constant of Ferricisothicoyanation complex ion in solution.
vi. Determination of rate constant of alkaline bleaching of Malachite green and effect of ionic strength on the rate of reaction.
(C) Polarography
i. Identification and estimation of metal ions such as Cd+2, Pb+2, Zn+2, and i+2 etc. polarographically.
ii. Study of a metal ligand complex polarographically (using Lingane's Method).
(D) Chemical Kinetics
i. Determination of rate constant and formation constant of an intermediate complex in the reaction of Ce(IV) and Hypophosphorous acid at ambient temperature.
ii. Determination of energy and enthalpy of activation in the reaction of KMnO4 and benzyl alcohol in acid medium.
iii. Determination of energy of activation of and entropy of activation from a single kinetic run.
iv. Kinetics of an enzyme catalyzed reaction.
(E) Electronics
This lab course will have theory as well as practicals and the lectures shall be delivered during lab hours.
Basic Electronics
Notations used in the electronic circuit, study of electronic compounds and colour codes Conversion of chemical quantities into electronic quantitles. transducer, illustration with electrodes, thermocouples and thermistors. Passive components : Resistors, capacitors and inductors with some emphasis on solid state properties of materials. Net works of resistors. Thevenin's theorem, superposition theorem, loop analysis, RC circuits, LR Circuits, LCR circuits. Illustration of the use of circuits in NQR spectroscopy, Mossbauer spectroscopy cyclic voltammetry and in power supplied as filter circuits.
Active components
Introduction to ordinary diodes and Zener diode with some emphasis on p-n junction as a solid
state property. Use of diode as rectifiers, clipping and clamping circuits. Power supplies.
Transistors : An extension of p-n-p and n-p-n transistors. Characteristics of transistors, hybrid
parameters; transistor circuits as amplifiers, high impedance (preamplifier) circuits. Darlinction
pairs, differential amplifiers.
Operational Amplifiers
Ideal characteristics; inverter, summer, integrator, differentiator, voltage follower, illustrative use of operational amplifiers. Introduction to Fourier transformation in instrumentation. List of Experiments in electronics (Do at least five experiments from this section)
1. (a) To plot the diode characteristics and find its dynamic resistance and cut in voltage.
(b) To plot the characteristics of transistor used as a diode and compare the results with
those of (a)
2. To implement a diode dipper circuit for the given transffer characteristics and verify the
3. (a) To plot the diode characteristics and find its dynamic resistance and cut in voltage.
(b) To plot the characteristics of transistor used as a diode and compare the results with those of (a)wave form.
4. To implement a diode damper circuit which damps the positive peak of the input voltage
to (a) Zero voltage adn (b) a given voltage. Verify the performance.
5. (a) To plot the characgteristics of an NPN transistor in CE configuration.
(b) To find the h-paprameter of the transistor from the characteristics.
6. (a) To plot the characteristics of an NPN transistor in CB configuration.
(b) To find the h-parameter of the transistor from the characterstics and compare it with the results of experiment No. 6.
7. (a) To plot the drain and transfer chracteristics of a JEET in CS configuration.
(b) To find out the pinch off voltage, maximum drain to source saturation current and the transconductance.
8. To obtain the frequency response of an RC coupled amplifier and estimate the bandwidth.
9. (a) To plot the characteristics of Zener diode and find its dynamic resistance under reverse biased condition.
To use zener diode for a voltage regulation.
(i) Plot the line regulation curve.
(ii) Plot the load Regulation curve.
10. (a) To vire a Half wave Rectifier circuit using diode and measure the rms voltage, de voltage and to find Riple factor
(b) To study the performance of half way and full wave doubler circuits.
11. To plot the characteristics of UJT and find the peak voltage, peak current and valley voltage and use as a relaxation oscillator.
Books Suggested
1. Inorganic Experimens, J. Derek Woolings, VCH.
2. Microscale Inorganic Chemistry, Z. Szafran, R.M, Pike and M.M. Singh, Wiley.
3. Practical Inorganic Chemistry, G. Marr and B. W. Rockett, Van Nostrad.
4. The systematic Identification of Organic Compounds, R.L. Shriner and D.Y. curlin.
