Pharmaceutical Analysis I
|1||Introduction to Pharmaceutical Analysis||4|
|1.1||•||Scope of Pharmaceutical Analysis, Classification of Quantitative Analytical techniques||2|
|(Instrumental and Non-Instrumental).|
|•||Introduction to pharmacopoeial monograph –Significance of a pharmacopoeial|
|monograph. (Only relevance of all the tests and principle of the assay procedures in the|
|monographs mentioned below to be discussed).|
|Active Pharmaceutical Ingredient (API): Aspirin, Calcium gluconate and Dried|
|aluminium hydroxide gel.|
|Formulations: Soluble Aspirin tablets.|
|1.2||•||Types of Errors: Determinate and Indeterminate, Causes of errors and ways to minimize||2|
|•||Concept and numericals of: Mean, Median, Standard deviation, relative standard|
|deviation, Absolute and relative errors, precision, accuracy, significant figures.|
|2||Aqueous acid-base titrations.||6|
|2.1||•||Theoretical terms: Titrimetric analysis, Titrant, Titrand, Theoretical end point or||2|
|equivalence point, end point of titration, Titration error, conditions for titrimetric|
|analysis, classification of reactions for titrimetric analysis, Expression of concentration of|
|Standard solutions-Molarity- (Analytical and equilibrium molarity), Molality, percent|
|concentration, ppm, ppb, Normality, Primary and Secondary standards.|
|•||Law of Mass Action, Equilibrium Constant, Application of Law of Mass Action to|
|solutions of weak electrolytes, pH, pKa, pKb, hydrolysis of salts (weak base-strong acid,|
|weak acid-strong base, weak acid-weak base), Buffer solutions, Buffer Capacity.|
|2.2||•||Neutralization curves-(strong acid versus strong base, weak acid versus strong base,||2|
|weak base versus strong acidand weak acid versus weak base).|
|•||Neutralization indicators-different theories (Ostwald’s theory, Resonance theory),|
|Mixed indicators, concept of range of indicators, Choice of indicators.|
|2.3||•||Methods of titration: Direct titration, back titration and need, blank determination use,||2|
|significance (one example for each type) and concepts of factor calculation for assay.|
|•||Problems related to calculation of– pH and its numericals with respect to neutralization|
|curve, Strength of Electrolytes (molarity, normality, and milliequivalence), and assay.|
|•||Applications: Assay of benzoic acid, aspirin, sodium hydroxide.|
|3.0||• Theoretical considerations-Need, Types of non-aqueous solvents (aprotic, protophilic,||2|
|protogenic, amphiprotic), characteristics of solvents for non-aqueous titrations (acid-|
|base character, dielectric constant, leveling and differentiating effect), Indicators for|
|non-aqueous titrations, Determination of Bases and Acids (solvent, titrants and|
|• Applications: Assay of Sodium benzoate and Acetazolamide.|
|•||Terms-Complex, complexing agents (Complexones), chelate, ligand, co-ordination|
|number, chelating agent, sequestering agent, metal-ligand complex.|
|•||Aspects in complex formation with respect to Disodium edetate- Dissociation|
|constant, pH, Stability, colouration, titrability of polyvalent metal ions, pM indicators,|
|presence of auxiliary complexing agent, and general structure of complexes formed|
|with di-, tri- and tetravalent metal ions.|
|•||Complexometric titrations: Direct method, back titration, replacement titration,|
|titration of mixture of metal ions, masking agent (auxiliary ligand) and demasking|
|agents and titration curve with respect to disodium edetate.|
|•||Applications: Determination of individual cations (aluminium by back titration, nickel|
|by direct titration), determination of mixture of lead, zinc and magnesium in a sample,|
|and assay of calcium gluconate injection.|
|5||Oxidation – Reduction Titrations||6|
|5.1||•||Terms: Oxidation, Reduction, oxidising and reducing agents, standard reduction||1|
|potential, Nernst equation, redox titration curve and equivalence point.|
|5.2||•||Theory, indicators, and titrants for :||2|
|Permanganometry and Cerimetry,|
|• Applications- Assay of hydrogen peroxide solution (Permanganometry), Assay of|
|Ascorbic acid tablets, Dried Ferrous sulphate, Paracetamol (Cerimetry).|
|5.3||•||Theory, indicators, and titrants for :||2|
|Iodometry, iodimetry, potassium dichromate, potassium iodate and potassium bromate|
|•||Applications- Assay of Ascorbic acid API (Iodimetry), Assay of potassium|
|permanganate (Iodometry), Assay of Potassium iodide (Iodate titration)|
|5.4||•||Balancing of redox equation-half cell reaction and net reaction.||1|
|6.1||•||Theoretical considerations-Common Ion Effect, Solubilty Product, Factors affecting||1|
|solubility of precipitates, Fractional precipitation.|
|6.2||•||Types of Precipitation Titration: Argentometric Titration methods -Mohr’s method,||2|
|Volhard’s Method and Adsorption Indicator Method.|
|•||Applications: Standardization of silver nitrate, Assay of||sodium chloride and|
|7.1||•||Theory: Mass as measurement signal and precipitation equilibria, Unit operations in||2|
|gravimetric analysis, Organic and inorganic precipitants, precipitation from|
|•||Problems associated with gravimetric analysis and methods to overcome (co-|
|precipitation and reprecipitation, Ostwald’s ripening, degree of supersaturation or Von|
|Weimarn ratio, solubility of precipitate, peptisation).|
|7.2||•||Applications-Assay of Nickel by dimethylglyoxime, Assay of||aluminium by oxine||1|
|reagent, Assay of Ba+2 as Barium sulphate..|
|•||Numericals related to gravimetric factor|
- Oxygen flask combustion method-technique, apparatus, principle and determination of organically bound halogens, sulphur and phosphorus, Application– Diloxanide furoate.
- Nitrite titrations- Concept of external indicator and application- Assay of Sulphacetamide sodium
- Determination of nitrogen (Kjeldahl method)-Technique (direct and indirect method), reagents & apparatus used, reaction & factor calculation and numerical for estimation of nitrogen.
Application-Assay of Urea (API)
|9||Electro Analytical Techniques:||5|
- Apparatus-Construction and working of Dropping mercury electrode (DME), advantages and disadvantages of DME.
- Theory-Current-Voltage curve (Polarogram), supporting electrolyte, Oxygen wave, polarographic maxima, Ilkovic equation, factors affecting limiting current, half wave potential.
- Applications-In brief.
- Pulse polarography-Normal pulse polarography, Differential pulse polarography and square wave polarography).
|9.2||• Amperometry-DME cell, four types of end points in amperometric titrations,||1|
|advantages, general applications and Biamperometric titrations.|
|• Aquametry by Karl Fischer titration: Principle, composition and stability of KFR,|
|standardization of KFR as per I.P, determination of water in a sample-e.g. Amoxycillin|
|9.3||• Coulometry and High Frequency Titration-Faraday’s first law of electrolysis,||1|
|Current vs Time plot, Cells for coulometric titration and generation of titrant, Types of|
|coulometric methods (potentiostatic and amperostatic), primary and secondary|
|coulometric titrations, advantages of coulometric titrations, and applications in brief.|
|9.4||• Electrogravimetry- Theory of electrolysis – constant current electrolysis and constant||1|
|potential electrolysis, theory of electrogravimetry- Ohm’s Law, Faraday’s second law|
|of electrolysis, Terminology: polarization, overvoltage, current density, current|
|efficiency, decomposition potential, polarized electrode, types of polarization-|
|concentration and kinetic, apparatus for electrogravimetric determinations,|
|characteristics of the deposit, factors affecting physical properties of the deposit,|
|applications in brief.|
|10.1||• Terms: Nernst Distribution law and partition coefficient, Distribution coefficient,||2|
|Distribution Ratio, Percent extraction or extraction efficiency, Separability factor.|
|• Types-Single extraction (Batch), multiple extraction, Countercurrent Distribution and|
|• Factors influencing solvent extraction, Emulsion formation problem in extraction and|
|ways to minimize.|
|• Examples –Assay of soluble Aspirin tablets.|
|10.2||• Problems based on distribution coefficient.|
- Practical Pharmaceutical Chemistry by Beckett, A H & Stenlake, J B, 2005, 4thedition, Part I and II, CBS Publishers and Distributors, India.
- A Textbook of Pharmaceutical Analysis by Kenneth A Connors, 2002, 3rd edition, John Wiley and Sons, Canada.
- Principles of Instrumental Analysis by Douglas A. Skoog, F. James Holler, 1992, 5thedition, Saunders College Publishing, USA.
- Fundamentals of Analytical Chemistry by Douglas A. Skoog, Donald M. West, F. James Holler, 1991, 7th edition, Saunders College Publishing, USA.
- Analytical Chemistry by Gary D. Christian, 6th edition, John Wiley & Sons, Singapore.
- Vogel’s Textbook of Quantitative Chemical Analysis by Mendham J, R.C. Denney, J.D. Barnes, M. Thomas, 2002, 6th edition, Pearson Education Ltd.
- Pharmaceutical Drug Analysis by Ashutosh Kar, 2005, 2nd edition, New Age International (P) Ltd Publishers, India.
- Instrumental Methods of Analysis by S. S. Mahajan, 2010, 1st edition, Popular Prakashan Pvt Ltd, India.
- Instrumental Methods of Chemical Analysis (Analytical Chemistry) by Gurudeep R. Chatwal and Sham. K. Anand, 2008, 5th revised and enlarged edition, Himalaya Publishing House Pvt Ltd.
- Indian Pharmacopoeia, 2014 or latest edition.
- Instrumental Method of Analysis by Willard H.H., L. L. Merritt& John A. Dean, 1986, 6th edition, CBS Publishers & Distributors, New Delhi.
- Instrumental Method of Chemical Analysis by Ewing Galen W, 1969, 3rd edition, McGraw Hill Book Company, New York.
- Undergraduate Instrumental Analysis by J.W. Robinson, E.M. Skelly Frame and G.M. Frame II, Pub. Marcel Deckker, 2009
- Analytical Chemistry, 2nd edition, R. Kellnar, M. Mermet, M. Otto, M. Valcarcel, H. M. Widner.
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