UNIVERSITY OF MADRAS
B.Sc. DEGREE COURSE IN CHEMISTRY
SEMESTER SYSTEM WITH CREDITS
(Effective from the Academic Year 2003-2004)

Semester V - Paper VIII - Analytical Chemistry-I

Duration: 3 hrs
Maximum Marks: 100
Credits: 4

(60 hrs)

Unit - I

(20 hrs)

1.1 Data analysis - Theory of errors - idea of significant figures and its importance with examples - precision - accuracy -- methods of expressing accuracy - error analysis - minimising errors method of expressing prison - average deviation - standard deviation and confidence limit.

1.2 Principles of gravimetric analysis - characteristics of precipitating agents - choice of precipitants and conditions of precipitation - specific and conditions of precipitation - specific and selective precipitants - DMG, cupferron, salicylaldehyde, ethylendediamine - use of seuestering agents - co - precipitation - post precipitation - peptisation - differences reduction of error - precipitation from homogeneous solutions - calculations in gravimetric methods - use of gravirnetric factor.

1.3 Thermal analytical methods - Principle involved in thermogravimetric analysis and differential gravimetric analysis - discussion of various components with block diagram - characteristics of TGA and DTA - factors affecting TGA and DTA curves - thermometric titrations.

Unit - II

(15 hrs)

2.1 Separation and purification techniques: - Principles involved in the separation of precipitates - solvent extraction and electrophoresis.

2.2 Purification of solid organic compounds - extraction - use of immiscible solvents - soxhiet extraction - crystallisation - use of miscible solvents - fractional crystallization - sublimation. Purification of liquids - experimental techniques of distillation - fractional distillation - vacuum distillation - steam distillation - tests for purity.

2.3 Chromatography techniques - Principles adsorption, thin layer, partition and paper. chromatography column chromatography - adsorbents - preparation of column - adsorption - elution, recovery of substance and applications. TLC - choice of adsorbent and solvent - preparation of chromatogram and applications - Rf value. Paper chromatography - Solvents used and principles - factors affecting Rf value - separation of aminoacid mixtures. Radial paper chromatography - Ion exchange chromatography - principle - resins - action of resins - experimental techniques - applications - separation of Zn-Mg, Co-Ni, Cd-Zn, Chloride - bromide. Gas chromatography and high pressure liquid chromatogrphy - principles - experimental techniques - instrumentation and applications.

Unit - III

(25 hrs)

3.1 UV- Visible spectroscopy - Absorbtion laws - calculations involving Beer - lambert's law - instrumentation - photocolonmeter and spectrophotometer - block diagrams with description of components - theory - types of electronic transitions - chromophore and auxochromes - absorbtion bands and intensity - factors governing absorbtion maximum and intensity.

3.2 Infrared spectroscopy - principle - types of stretching and bending vibrations - vibrational frequencies - instrumentation - block diagram - source - monochromator - cell sampling techniques - detector and recorders - identification of organic molecules from characteristic absorption bands.

3.3 Raman spectroscopy - Raleigh and Raman scattering - stoke's and anti stokes lines - instrumentation block diagram - differences between IR and Raman spectroscopy - mutual exclusion principle - applications - structural diagnosis.

Reference Books:

Analytical Chemistry:

1. Analytical Chemistry S.M Khopkar - New Age International
2. Analytical chemistry - R.Gopalan - Suhan Chand
3. Fundamentals of analytical chemistry- A.Skog and M.West
4. Vogel's hand book of quantitative inorganic analysis - Longman
5. Instrumental methods of' analysis - Skog
6. Instrumental methods of analysis - Willard et al - CXBS
7. Physico-chernical techniques of analysas-P.B.Janarthanam. Vol-I and Il-Asian publishing
8. Instrumental methods of chemical analysis - B.K. Sharma - God Publications
9. Analytical Chemistry S .Usharani, Macmillan