M.Sc. PREVIOUS, ANALYTICAL CHEMISTRY PAPER-IV 1. MAX: MARKS: 100 BASIC CONCEPTS OF ANALYSIS Introduction to analytical Chemistry, analytical process: Defining the problem, sampling, handling the sample, performing necessary chemical separations, performing the measurement, calculation and interpretation of the measurement 2. ERRORS AND DATA HANDLING Determinate and indeterminate errors, significant figures, rounding off, accuracy and precision, arithmetic means, medians, average deviation, standard deviation, confidence limit, testing for significance, Q-test, T-test, correlation coefficient 3. GRAVIMETRIC ANALYSIS General principle, steps of gravimetric analysis: Solution preparation, precipitation, digestion, washing, filtration, drying and ignition of precipitates, calculation, applications of gravimetric analysis. 4. PHYSICOCHEMICAL BASIS OF REACTIONS IN AQUEOUS SOLUTION Introduction, types of chemical reactions, chemical equilibrium, equilibrium constants, factors effecting equilibrium constants, Law of mass action, LeChatelier principle and its applications. a) ACID-BASE EQUILIBRIA Ionization, ionization constants, activity coefficient, pH measurements and calculations, pH of an acid and base, , strong and weak acid base titration’s common ion effect, indicators, titration curves, buffer solution and buffer capacity. b) REDOX-EQUILIBRIA Theory of oxidation and reduction, redox titration’s, indicators, titration curves. c) COMPLEXATION EQUILIBRIA 1 Theory, complex-forming reagents, complex formation constants, cheletes, EDTA equilibria, EDTA titration curves, indicators. d) PRECIPITATION EQUILIBRIA: Solubility, factors effecting solubility, solubility product constant, precipitation titration’s, Indicators. 5. 6. SEPARATION TECHNIQUES a) Solvent extraction: General principle and terminology of solvent extraction, experimental techniques, important experimental variables, and metal extraction system. b) Chromatography: Principles of chromatography, classification, techniques of chromatography (column, ion exchange, size exclusion, and thin layer chromatography. BASIC CONCEPTS OF ELECTRO-ANALYTICAL TECHNIQUES Principle, instrumentation and applications of potentiometry and polarography. I 7. INTRODUCTION TO SPECTROSCOPIC METHODS OF ANALYSIS Introduction: The nature of electromagnetic radiation as waves (general nature, diffraction, dispersion, refraction, reflection, scattering, polarization). Quantum mechanical properties (photoelectric effect, absorption and emission of radiation by atoms and molecules). Electromagnetic spectrum, Beer’s and Lambert laws, deviations from Beer’s law, instrumentation and applications of uv-vis spectroscopy. Reference Books For M.Sc. Previous Analytical Chemistry 1. Analytical Chemistry An introduction 7”’ edition), By Skoog Holler. Edition 2000. 2. Analytical Chemistry R. M. Verma CBS publications India. 3. Analytical Cbemistry,5 edition, By G.D. Christian, John Wiley & Sons, lnc., 1994. 4. Analytical Spectroscopy by Bensal K. 5. Instrumental method of Analysis: by H. Bauer, 6. Principles of analytical Chemistry (A textbook) by Valcarcel. 2 7. Principles of Instrumental Analysis,6tt edit By Skoog /HolIerl Nieman & Sounders College Publishing Company. 8. Problem solving in Analytical Chemistry by Crawford. K. 9. Quantitative Analysis by Day & Underwood. 10. Textbook of quantitative Inorganic Chemistry by A.l Vogel. M.Sc. PREVIOUS, ANALYTICAL CHEMISTRY PRACTICAL-IV MAX: MARKS: 50 1 Calibration of common apparatus / glass wares and basic techniques. 2 Determination of Sulphate in the given sample gravimetrically. 3 Determination of calcium as calcium oxalate gravimetrically. 4 Preparation and standardization of sodium hydroxide solution and titration of hydrochloric acid. 5 Preparation and standardization of sodium thiosulphate solution with a primary standard reagent. 6. Analysis of commercial Hypochlorite solution lodometrically. 7. Analysis of hydrogen peroxide Iodometrically. 8. Determination of calcium and magnesium in the given sample with EDTA volumetrically. 9. Preparation of standard potassium permanganate solution and titrimetric determination of iron. 10 Determination of potassium permanganate in the given sample by spectrophotometry. 11. Determination of nitrate-nitrogen in water sample by spectrophotometry. 12. Determination of lead spectrophotometrically using solvent extraction. 13 Separation of metal ions (Nickel, copper, Zinc and Cobalt and determination of Rf values by Thin Layer Chromatography. 3 14 Separation of metal ions and amino acids by paper chromatography. 15 Separation of dyes by column chromatography. 16 Conductometric titration of strong acid-base. 17 Determination of chloride in water volumetrically. 4