VOLUMETRIC ANALYSIS
Introduction to the pharmaceutical quantitative analysis
Qualitative and quantitative analysis. Introduction to the quantitative pharmaceutical analysis. General operations of the quantitative pharmaceutical analysis: the choice of the analysis method, sampling, sample processing, interference elimination, calculation and, interpretation of the results. Purpose of the quantitative analysis of a compound of pharmaceutical
interest. Role of technical and regulatory Pharmacopoeia based on the Quality
of Medicines. Italian Official Pharmacopoeia and European Pharmacopoeia
Equipment and complex operations of quantitative analytical chemistry
Measurement of the mass: analytical and technical balances. Sources of error
in weighing. Volume measurement: measuring containers. Effect of temperature on the volume measures. Safety in the chemical laboratory. Classification of reactive chemicals: risk and safety phrases.
Methods based on titration
Volumetric analysis. Volumetric titrations. Primary and secondary standards. Standard solutions: properties. Determination of the concentration of a standard solution. Equivalence and end points. Detection of the end point. Titration curves. Title of a solution. Requirements for the volumetric analysis. Definition of equivalent weight. Calculations in volumetric analysis. Ways of expressing concentration. Evaluation of the error in the analytical determination. Errors in volumetric analysis. Accuracy of the calculations in the
quantitative analysis.
Acid-base titrations in aqueous solution
Theoretical aspects of neutralization titrations. Calculation of the pH of strong acid, strong base, weak acid, weak base solutions, salt solutions, buffersolutions. Acid-base indicators. Acid-base titration curves: strong acid- strong base, weak acid-strong base, strong acid-strong base, weak base - strong acid. Influence of concentration on the titration curve. Influence of acid and base constants on titration curves. Titration curves of multifunctional acids and bases. Titration curve of mixtures of acids.
Applications of acid-base titrations.
Acidimetry: acid titrant, primary standards for acid titrants. Applications of acidimetry: Determination of sodium carbonate, alkaline dosage mixtures (Warder and Winkler methods), dosage of ammoniacal nitrogen (Kjeldahl method). Acidimetric dosages of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Alkalimetry: Basic titrants, primary standards for basic titrants. Alkalimetric dosages of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Acid-base titrations in non-aqueous solvents
General aspects. Advantages and disadvantages of the use of non-aqueous solvents. Effect of solvent on the strength of acids and bases. Classification of
solvents. Choice of solvents. Applications of titrations in non-aqueous solvents. Acidimetry. Alkalimetry. Determination of the end point. Dosages of
drugs reported in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Precipitation titrations
Theoretical aspects of the precipitation. Solubility. Titration curves of precipitation. Influence of product solubility and concentration on the titration curve. Typical methods of precipitation. Determination of the end point. Mohrmethod: applications, limitations and incompatibilities. Volhard method: applications, limitations and incompatibilities. Fajans method: applications and indicators of adsorption. Gay-Lussac Method. Titration of mixtures of halides. Applications of precipitation titrations. Dosages of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Complexation titrations
General. Complex. Complexation titrations with inorganic and organic complexing agents. Formation constant or stability of the complex. EDTA complexes with metal ions. Conditional formation constant. Effect of other complexing agents on titration with EDTA. Titration curves. Influence of concentration on the titration curve. Determination of the end point. Indicators.
Types of titrations with EDTA. Masking. Application of the complexation titration. Dosages of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Redox titrations
Introduction to electrochemistry. Redox reactions: direct and indirect transfer of electrons. Electrode potential. Nernst equation. Calculation of the potential and of the equilibrium constants. Redox titration curves. Influence of potentialand concentration on the titration curve. Redox indicators.
Applications of redox titrations.
Oxidants standards: Permanganometry. Cerimetry. Bromometry. Reducing standards: solutions of Fe (II). Iodometry. Karl Fisher titrations. Redox determinations of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
INSTRUMENTAL ANALYSIS
Potentiometry
General principles. Analytical methods based on the measurement of potential. Principle of the potentiometer. Electrodes: classification. Potentiometric titrations and determination of the end point: mathematical and graphical methods. Potentiometric assays of substances listed in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Conductimetry
Principles and applications. Electrical conductivity of the solutions. Electrical conductivity and Kholrausch Law. Methods of analysis. Conductimetric titrations. Applications of conductimetry reported in the Italian Official Pharmacopoeia and European Pharmacopoeia.
Laboratory Practice
Acidimetric determinations of substances and pharmaceutical forms.
Alkalimetric determinations of substances and pharmaceutical forms.
Complexation determinations of substances and pharmaceutical forms.
Redox determinations of substances and pharmaceutical forms.
Potentiometric determination of substances and pharmaceutical forms.
Conductivity determinations of substances and pharmaceutical forms.
Spectrophotometric determination of substances and pharmaceutical forms.
