Organic qualitative and quantitative analysis (CHM 404/305)

Course contents:

1. Experimental Techniques

• Purification of Organic Compounds
• Recrystallisation
• Sublimation at atmospheric pressure and under reduced pressure
• Separation or organic compounds by Steam distillation
• Distillation of organic compounds under reduced pressure
• Bulb-to-bulb distillation under reduced pressure
• Chromatography
• Thin layer chromatography (TLC) and calculation of Rf values
• Column Chromatography: separation of organic mixture.
• Preparative TLC: preparation of plates and separation of organic mixtures
• Physical Constants
• Melting Points and Boiling Points
• Optical rotation and calculation of specific rotation and molecular rotation
• Spectroscopic Methods
• Preparation of an ester and its confirmation by IR and NMR
• Structure illucidation of unknown compounds based on the given spectral data

2. Investigation and Characterization of Organic Compounds

• Detection of elements present in a given organic compound.
• Identification of functional groups in a given organic compound.
• Identification of unknown organic compounds.
• Separation of organic mixture by chemical methods, preparation of derivatives, and identification of the material

Inorganic Chemistry Laboratory - I(CHM 343/344)

Course contents:

1. Estimation of iron in minute quantities by UV-vis spectrophotometry
2. Principles of colorimetric analysis: determination of iron content of an unknown sample.
3. Preparation of hexamminenickel(II)chloride: estimation of ammonia and nickel by titrimetric and gravimetric methods
4. Determination of complex composition using simple techniques
5. Preparation of diamagnetic and paramagnetic main-group and transition-metal acetylacetonates
6. Synthesis, isolation and spectroscopic characterization of the complexes
7. Synthesis and characterization of ferrocene and acetylferrocene
8. Synthesis of the complex and their purification using chromatography
9. Acid-base and redox titration of tablets containing Vitamin-C
10. Estimation of ascorbic acid in Vitamin-C tablets
11. Paper chromatographic separation of Cu2+, Fe3+ and Ni2+
12. Utilization of paper chromatographic techniques to separate the metal salts
13. Spectrophotometric determination of phosphate: estimation of phosphate in cola drinks
14. Determination of concentration of phosphates applying Beer-Lambert law
15. Potassium tris-oxalatoferrate(III): synthesis, analysis and photochemistry
16. Synthesis of the complex and its utilization in blue-printing experiment

Suggested books:

1. Elias, A. J., A Collection of Interesting General Chemistry Experiments, Universities Press (India) Pvt. Ltd., 2002.
2. Roesky, H. W.; Möckel, K., Chemical Curiosities: spectacular experiments and inspired quotes, VCH, 1996.
3. Hand-outs prepared for the laboratory experiments: collections from various literature sources

Basic Chemistry Lab (CHM 101A)

Course contents:

1. Permanganometric Titrations
2. Acid - Base Titrations
3. Iodometric Titrations
4. Complexometric Titrations
5. Recycling Of Aluminum
6. Preparation and Analysis of a Metal Complex
7. Polynuclear Metal Complexes with Multidentate Bridging Ligands
8. Chromatography of Natural Pigments
9. Synthesis of antioxidants used as food preservative
10. Preparation of Polymer Films
11. Isolation of Caffeine from tea
12. Preparation of Fluorescein Dye
13. Preparation of 9,10-dihydroanthracene-9,10-,-succinic anhydride via Diels-Alder reaction
14. Viscosities of Solutions
15. Chemical Kinetics
16. Heterogeneous Equilibrium
17. Photochemical Oxidation - Reduction
18. The Detection of Changes in the Conformation of Bovine serum albumin by Viscosity
19. Determination of pI of Glycine
20. Conductometric titration of HCl Vs NaOH

Experiments 1-8 and 14-17 are taken from "Experiments in General Chemistry" by A.J. Elias, S.S. Manoharan and Hans Raj, IIT Kanpur (1997), private circulation. The contents of other experiments are provided by F.A. Khan and S. Verma.

Physical Chemistry Laboratory (CHM 423/423A)

Contents:

1. Calibration of volumetric apparatus. (One day).
2. Analysis of the rotational-vibrational spectra of HCl molecules. (One day)
3. Determination of partial molal volume. (One day)
4. Determination of the isotherm for a three component system. (Two days)
5. Kinetics of fast reactions by stopped-flow technique. (One day)
6. Spectrophotometric determination of the acid dissociation constant (Two days)
7. The measurement of electrical conductance for the determination of the equivalent conductance at infinite dilution (Two days)
8. Rate of the hydrolysis of sucrose using polarimeter. (Two days)
9. Determination of pKa of poly-basic acid with the pH meter. (One day)
10. Determination of critical miceller concentration. (One day)
11. Determination of transport number by moving boundary method. (One day)
12. Polarizability from refractive index measurements. (One day)
13. Formula and stability constant of a complex by spectrophotometry. (One day)
14. Fluorescence quantum yield determination of an unknown molecule. (One day)
15. Fluorescence spectrum and stern-volmer quenching constant. (One day)
16. IR and Raman spectroscopy of solvent mixtures. (Two days)
17. Computing Potential Energy Surface of molecules using Quantum Mechanics. (Two days)
18. Introduction to Scanning Probe Microscopy (Two days)

Suggested books:

1. Experimental physical chemistry, F. A. Bettelheim
2. Experimental physical chemistry, G. P. Matthews
3. Experimental physical chemistry, F. Daniels
4. Experimental physical chemistry, A. Halpern and G. McBane
5. Experimental Physical Chemistry, D. P. Shoemaker, C. W. Garland, and J. W. Nibler

Basic Chemistry Lab (CHM 101A)

Contents:

1. Invisible ink Utilization of coordination chemistry to demonstrate invisible ink in laboratory.
2. Color effects due to ligand-exchange in nickel complexes Demonstration of ligand-field strength in the spectrochemical series.
3. Color effects in aqueous systems containing divalent 3d metal ions Demonstration of crystal-field splitting parameters of 3d metal ions.
4. Acidic and basic salts Hydrolysis of salts and its consequences.
5. Preparation of nitro- and nitrito-pentamminecobalt(III) chloride Linkage isomers: synthesis and identification using various spectroscopic techniques.
6. The preparation of hexammine cobalt(III) chloride and pentammineaquo cobalt(III) chloride Synthesis, isolation and characterization of the complex.
7. The preparation of cis- and trans-potassiumdioxalatodiaquochromate(III) Geometrical isomers: synthesis and identification using various spectroscopic techniques.
8. Aquation of trans-dichloro-bis(1,2-diamminoethane) cobalt(III) chloride Investigation of acid hydrolysis of the complex.
9. The preparation and resolution of tris(ethylenediamine) cobalt(III) ion into its optical antipodes Optical isomers: synthesis, isolation and characterization.
10. Preparation of hexamminenickel(II) chloride: estimation of ammonia and nickel by titrimetric and gravimetric methods Determination of complex composition using simple techniques.
11. Synthesis and reactions of organocobaloximes Synthesis of an air-sensitive organometallic complex at low temperature under inert atmosphere.
12. Synthesis and characterization of ferrocene and acetylferrocene Synthesis, purification using chromatography and characterization.

Suggested books:

1. Roesky, H. W.; Möckel, K., Chemical curiosities: spectacular experiments and inspired quotes, VCH, 1996.
2. Hand-outs prepared for the laboratory experiments: collections from various literature sources

Organic Preparations Lab (CHM 503)

Contents:

Benzil – Benzilic Acid Rearrangement

• Prep. of benzil by oxidation of benzoin by nitric acid
• Benzil, an ® , ¯ - diketone undergoes rearrangement to benzilic acid

Fisher: Indole Synthesis: Preparation of 1.2.3.4 – tetrahydrocarbazole. This compound is prepared according to the Fisher indole synthesis starting from phenylhydrazine and cyclohexanone.

Diazotization: Forming a diazonium salt from an appropriate primary aromatic amine in the presence of HNO2.

Preparation of P - Iodonitrobenzene: By Irradiation with Sunlight OR By Reductive Coupling Prep. of Benzopinacol from benzophenone by reductive coupling

MOLECULAR REARRANGEMENT

Pinacol – Pinacolone – rearrangement

• Prep. of benzopinacol
• Prep. of benzopinacolone

REIMER – TIEMANN REACTION Prep. of β-hydroxynapthaldehyde from β-napthal
Prep. of β-hydroxynapthaldehyde from β-napthal

PERKIN REACTION
Preparation of Cinnamic acid
Bromination cinnamic acid i.e. Prep. of bromostryrene

ALDOL CONDENSATION AND EPOXIDATION

• Preparation of Chalcone
• Preparation of Chalcone epoxide