67136 - Health Products' Analysis I (GR_A)

Learning outcomes

The student acquires theoretical and practical knowledge for analytical laboratory work, in particular for the identification and quantitative determination of inorganic drug-related compounds by means of chemical reactions and volumetric titrations.

Course contents

Introduction. Aim of the course. Introduction to qualitative and quantitative analysis . The Italian Official Pharmacopoeia (F.U.) and the European Pharmacopoeia. Safety in the laboratory environment.

Introduction to drug analysis. Solubility. Solution properties. Solubility product. Formation and dissolution of precipitates, co- and postprecipitation. Crystals, colloidal precipitates and their characteristics. Periodic table.

Qualitative analysis

Cations. Properties, compounds interesting from a pharmaceutical point of view, biological roles, toxicological aspects and reactions used to identify the following cations: Silver, Lead, Mercury, Arsenic, Antimony, Bismuth and Copper. How to calculate the pH of precipitation of sulphides. How to calculate the pH of precipitation of hydroxydes Common properties of transition metals. Properties, biological roles, compounds interesting from a pharmaceutical point of view, reactions of Aluminum, Iron, Zinc, Manganese, Nickel and Cobalt. Common properties of alkaline earths. Calcium, Barium and Magnesium: properties, biological roles, compounds interesting from a pharmaceutical point of view, reactions. Common properties of alkali metals. Sodium, Lithium and Potassium: properties, biological roles, compounds interesting from a pharmaceutical point of view, reactions. Ammonium ion. Systematic analysis of cations. Principles of color theory. Flame tests.

Anions. Halides: common properties. Chlorides, bromides and iodides: properties, biological roles, compounds interesting from a pharmaceutical point of view, reactions. Properties, biological roles, compounds interesting from a pharmaceutical point of view, reactions of Acetates, Borates, Sulphates, Phosphates, Carbonates and Bicarbonates, Sulphides and Thiosulphates, Nitrates, Oxalates. Iodine. Hydrogen peroxide. Introduction to complex ions. Limit tests.

Introduction to volumetric analysis. Glassware and its use. Electronic balances. Concentration units. Normality, equivalents, calculus in volumetric analysis. Standard solutions. Primary standards, their properties and use.

Quantitative analysis

Acid-base titrations . Titration curves of acid and bases. Indicator theory. Common acid-base indicators and their use. How to choose a suitable indicator. Mixed indicators. Acid and base standard solutions used in volumetric analysis. Primary standards used in preparing and standardising acid and base solutions. Examples of acid-base titrations according to F.U.

Precipitation titrations . Precipitation titration curves. Common precipitation indicators and their use. Standard solutions used in precipitation titrations. Determination of halides by Mohr's, Volhard's and Fajans' methods. Practical aspects, limitations and applicability of the methods. Examples of precipitation titrations according to F.U.

Redox titrations. Introduction and theoretical aspects. Redox titration curves. Redox indicators and specific indicators. Permanganometry. Properties, reactions and use of permanganate solutions. Identification of the final point. Standardisation of permanganate solutions. Examples of permanganometric titrations according to F.U. Iodimetry. Preparation and use of iodine solutions. Examples of iodimetric titrations according to F.U. Iodometry. Principles, applications, properties. Use of starch water as an indicator. Examples of iodometric titrations according to F.U. Cerimetry. Properties and preparation of Ce4+ solutions. Examples of cerimetric titrations according to F.U.

Complex-formation titrations . Complex-formation and instability constants. Complexometric titration curves. Titrations employing EDTA. Conditional formation constant, a and their relationship to pH. Indicators for EDTA titrations. Direct titrations, back-titrations, displacement titrations, titrations based on indicators for an added metal ion, indirect titrations. Masking agents, masking and demasking. Analysis of complex cations mixtures. Water hardness. Examples of complexometric titrations according to F.U.

LABORATORY

Qualitative analysis

Reactions used to identify the cations: Silver, Lead, Mercury, Arsenic, Antimony, Bismuth, Copper, Aluminum, Iron, Zinc, Manganese, Calcium, Barium and Magnesium, Sodium, Lithium, Potassium, Ammonium ion. Flame tests.

Reactions used to identify the anions: Chlorides, Bromides, Iodides, Acetates, Borates, Sulphates, Phosphates, Carbonates and Bicarbonates,  Nitrates, Oxalates. Limit tests.

 

Quantitative analysis

Standardization of HCl and of NaOH. Purity of acid compounds according to F.U.

Standardization of AgNO3. Purity of NaCl.

Standardization of Na2S2O3 and of KMnO4. Purity of redox compounds according to F.U.

Standardization of EDTA. Purity of ZnO.

During the lab course,  unknown solutions will be analyzed.

Readings/Bibliography

Qualitative analysis:

P. Barbetti, M.G. Quaglia

L'Analisi qualitativa in chimica farmaceutica e tossicologica inorganica

1991, Galeno Editrice

 

Quantitative analysis

G.C. Porretta

Analisi di preparazioni farmaceutiche.

Analisi quantitativa

2000, CISU ed

Teaching methods

The course takes place during the second semester and is subdivided in 2 modules (attendance is mandatory):

Qualitative analysis module (Prof. Roberto Mandrioli), 16 theory hours and 36 lab hours: identification reactions of inorganic active principles according to F.U. are explained and applied in practice.

Quantitative analysis module (Prof. Robeto Mandrioli), 16 theory hours and 36 lab hours: volumetric analysis is explained and applied during laboratory practical for the purpose of drug purity controls and inorganic active principle determinations.

Laboratory practical is carried out individually, with a final test.

Assessment methods

Verification of learning is carried out by means of an oral examination, which can only be sustained after laboratory practical attendance. The laboratory practical includes intermediate tests whose outcome becomes part of the final judgement.

Teaching tools

The theoretical lessons will be held by  using slides or trasparents.The practical activity will be carried out in laboratories equipped with chemical reagents and analytical instrumentation

Office hours

See the website of Vincenzo Tumiatti

See the website of Andrea Milelli

See the website of Andrea Milelli