BPH-202: PHARMACEUTICAL CHEMISTRY – IV
(PHARMACEUTICAL ANALYSIS – I)
THEORY
Max. Marks: 80 Total Hours: 75 (3hrs/week)
Note: Examiner to set eight questions and the candidates are required to attempt any five.
1. Introduction: Importance of quality control, computation of analytical results, significant figure, concept of error, precision, accuracy, standard deviation, normal distribution curve, calibration of analytical equipments, fundamental of volumetric analysis, methods of expressing concentrations, primary and secondary standards.(3)
2. Neutralization titrations: Acid base concept, Acid base dissociation constant, Role of the solvent, Relative strength of acids, bases, Distribution of acid base species with pH, Buffer solution (Effect of dilution, added acids & bases upon buffer) Henderson Hasselbalch equation, neutralization curves, Acid base indicators, Mixed indicators, Acid base titrations (strong acid vs. strong base,weak acids-weak bases and mixtures of strong & weak acids) Polyprotic systems, phosphoric acid system, polyamine and amino acid systems. Titration of sodium carbonate. (7)
3. Non-aqueous titrations: Theoretical basis, types of solvents, indicators, scope, limitations, preparation and standardization of titrant solutions.. Titrations of weak acids and weak bases. Standardization of perchloric acid, lithium and sodium methoxide, tetrabutyl ammonium hydroxide. Pharmaceutical applications. (4)
4. Precipitation titrations: Principles of precipitation titrations, solubility product, effect of acids, temperature and solvent on the solubility of precipitate. Argentimetric titration, mercurimetric and titration involving ammonium or potassium thiocyanate, barium sulphate, adsorption indicators, Mohr’s method, Volhard’s method and Fajan’s method. (5)
5. Complexometirc titrations: Concept of complexation and chelation, Warner’s coordination number and electronic structure of complex ions, stability constants, titration curves, masking and demasking agents, types of complexometric titration, metal ion indicators, factors influencing the stability of complexes, EDTA-metal ion complexes, Determination of hardness of water. (5)
6. Oxidation – reduction titrations: Concepts of oxidation–reduction, standard oxidation potential, Nernst equation, theory of redox titrations, redox indicators, titrations involving cerric ammonium sulphate, potassium permanganate, titanous chloride, sodium–2,6–dichlorophenol–indophenol, iodimetry, iodometry, preparation, standardization and titration. (6)
7. Gravimetric analysis: Colloidal state, Supersaturation, Co-precipitation, Post-precipitation, Digestion, Washing of the precipitate, Filtration, Filter papers and crucibles, Ignition, thermogravimeteric curves Specific examples like barium as barium sulphate aluminium as aluminium oxide: Calcium as calcium oxalate and Magnesium as Magnesium pyrophosphate: Organic precipitants. (4)
8. Miscellaneous methods: 1. Diazotisation, 2. Kjeldhal method of nitrogen estimation, 3. Oxygen Flask combustion 4. Karl fischer titration 5. Analysis of oils, fats and waxes. (7)
9. Chromatography with Pharmaceutical applications of each category: (20)
i. Column chromatography: Adsorption and Partition theory, preparation, procedure and methods of detection.
ii. Thin layer chromatography: Theoretical consideration, preparation, procedure and detection of compounds.
iii. Paper chromatography: Theory of partition, different techniques employed and different grades of papers used, quantitative and qualitative detection.
iv. Gas Chromatography: Introduction, fundamentals of column operation and detection.
v. Ion Exchangers: Types of exchangers, mechanism of ion exchange and column operation.
vi. Size Exclusion Chromatography.10. Potentiometric titrations: Introduction, Electrochemical cells, half-cells, electrodes, measurement of potential and application in pharmaceutical analysis. (4)
11. Conductometric titrations: Basic concepts, different types of conductometric titrations, apparatus used and applications in Pharmaceutical Analysis. (4)
12. Polarography: Basic concept, theoretical considerations, Basic instrumentation, apparatus, principles, general polarography analysis and applications in pharmaceutical analysis. (3)
13. Amperometry: Amperometric titrations with one polarized electrode, general procedure, titration curves and applications. (3)
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