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 XII Ed and European Pharmacopoeia IX Ed.
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, buffer solutions. 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 XII Ed and European Pharmacopoeia IX Ed. Alkalimetry. Basic titrants, primary standards for basic titrants. Alkalimetric dosages of substances listed in the Italian Official Pharmacopoeia XII Ed and European Pharmacopoeia IX Ed.
Amino acids: classification, titration curves of simple amino acids, acid and basic aminoacids. Dosages of amino acids reported in the Italian Official Pharmacopoeia XII Ed and European Pharmacopoeia IX Ed.
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 XII Ed and European Pharmacopoeia IX Ed.
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. Mohr method: 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 XII Ed and European Pharmacopoeia IX Ed.
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 XII Ed and European Pharmacopoeia IX Ed.
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 potential and 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’s titrations.
Redox determinations of substances listed in the Italian Official Pharmacopoeia XII Ed and European Pharmacopoeia IX Ed.
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 XII Ed. and European Pharmacopoeia IX Ed.
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 XII Ed and European Pharmacopoeia IX Ed.
Spectrophotometry.
General. Qualitative and quantitative analysis. Spectrophotometric titrations. Spectrophotometric assays of substances listed in the Italian Official Pharmacopoeia XII Ed and European Pharmacopoeia IX Ed.
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.
