Pharmaceutical Analysis I MU BPH_C_304_T




Pharmaceutical Analysis I

No. Details Hours
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
them.
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 Non-aqueous titrations 2
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
indicator used).
•   Applications: Assay of Sodium benzoate and Acetazolamide.

 

4 Complexometric titrations 3
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
titrations.
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 Precipitation Titration 3
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
potassium chloride.
7 Gravimetry 3
7.1 Theory: Mass as measurement signal and precipitation equilibria, Unit operations in 2
gravimetric  analysis,  Organic  and  inorganic  precipitants,  precipitation  from
homogeneous solution.
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
8 Miscellaneous methods 2


8.1

  • 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
9.1 Polarography- 2
  • 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
trihydrate.
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 Liquid-Liquid Extraction 2
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
Continuous extraction.
•   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.
Total 36







Books:

  1. Practical Pharmaceutical Chemistry by Beckett, A H & Stenlake, J B, 2005, 4thedition, Part I and II, CBS Publishers and Distributors, India.

 

  1. A Textbook of Pharmaceutical Analysis by Kenneth A Connors, 2002, 3rd edition, John Wiley and Sons, Canada.
  2. Principles of Instrumental Analysis by Douglas A. Skoog, F. James Holler, 1992, 5thedition, Saunders College Publishing, USA.
  3. Fundamentals of Analytical Chemistry by Douglas A. Skoog, Donald M. West, F. James Holler, 1991, 7th edition, Saunders College Publishing, USA.

 

  1. Analytical Chemistry by Gary D. Christian, 6th edition, John Wiley & Sons, Singapore.
  2. Vogel’s Textbook of Quantitative Chemical Analysis by Mendham J, R.C. Denney, J.D. Barnes, M. Thomas, 2002, 6th edition, Pearson Education Ltd.
  1. Pharmaceutical Drug Analysis by Ashutosh Kar, 2005, 2nd edition, New Age International (P) Ltd Publishers, India.
  2. Instrumental Methods of Analysis by S. S. Mahajan, 2010, 1st edition, Popular Prakashan Pvt Ltd, India.
  3. 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.
  4. Indian Pharmacopoeia, 2014 or latest edition.
  5. Instrumental Method of Analysis by Willard H.H., L. L. Merritt& John A. Dean, 1986, 6th edition, CBS Publishers & Distributors, New Delhi.
  6. Instrumental Method of Chemical Analysis by Ewing Galen W, 1969, 3rd edition, McGraw Hill Book Company, New York.
  7. Undergraduate Instrumental Analysis by J.W. Robinson, E.M. Skelly Frame and G.M. Frame II, Pub. Marcel Deckker, 2009
  8. Analytical Chemistry, 2nd edition, R. Kellnar, M. Mermet, M. Otto, M. Valcarcel, H. M. Widner.
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