00090 - Analytical Chemistry

Learning outcomes

The course on Analytical Chemistry provides students with the fundamental notions of analytical chemistry useful in carrying out and evaluating controls on medicines and in understanding drug validation studies. In particular it provides the means for critical evaluation (also statistically and chemometrically) of the experimental results obtained and those reported in drug application studies and in the quality control of medicines and health products. The course contents also make it possible to acquire the cultural knowledge necessary to follow the next courses, in particular the course on analysis laboratories.

Course contents

BOLOGNA

- Foreword: Basic knowledge of the following subjects is presumed: General chemistry: Chemical reactions, stochiometric coefficients. Classification of chemical reactions, Oxidation-reduction reactions, Oxidation numbers, Oxidation and reduction, Balancing of oxidation-reduction reactions, Solutions, Water as a solvent, Electrolytes and non-electrolytes, Solubility, Solubilization process, Activity and concentration, Percentage concentration, Molarity or molar concentration, Definitions of equivalent weight, Definitions of acids and bases, Acid-base systems in water, Expression of chemical equilibrium, Equilibrium constants, Autoprotolysis of water, Acid and base dissociation constants, pH of aqueous solution. The SI system. Mathematics: Logarithms: significance, use and calculations, Calculation with exponential numbers, Quadratic equations.

- To pass the exam it is necessary to know how to use a calculator in the subjects covered in the course (e.g. standard deviation, least squares, etc.) together bibliographic research in Analytical Chemistry. This test is preparatory to the continuation of the oral exam.

Programme of the Module “Analytical Chemistry”. Teacher: Prof. Stefano Girotti.

- Introduction:

Aims of Analytical Chemistry

Bibliographic research in Analytical Chemistry, with practical tests

Analytical Chemistry procedure and basic instrumentation

Glossary of Analytical Chemistry terms

- Statistical processing of analytical data:

Chemometric elements: Calculation and significant figures in relation to uncertainty (instrumental). Main expressions of concentration. Parts per million (ppm) parts per billion (ppb). Titre

Determinate and indeterminate errors (systematic, random and rough errors)

Mean values of a series of data, mode, median and weighted mean

Absolute error and relative error

Standard deviation, relative standard deviation and coefficient of variation, variance

Absolute and relative uncertainty

Probability distribution: Gauss

Accuracy and precision (inaccuracy and imprecision). Trueness

Repeatability, reproducibility

How to measure inaccuracy and imprecision. Recovery test for addition and for additions (line slope); dilution test

Imprecision (uncertainty) propagation

Correlation and regression: Least squares method, correlation and regression coefficients

Detection limit and quantification limit

Sensitivity and analytical sensitivity

Dynamic interval and linear (dynamic) interval

Figures of merit

Calibration and Sizing; Comparators, transducers, sensors and biosensors

Scientific Method: Placebo Effect and Alternative Medicines

Calibration diagram method

Standard addition method, standard additions method, percentage recovery

Internal standard method

Student t Test

Statistical decisions: null hypothesis Ho

Ways of expressing the analysis result

Reliability or confidence limits (or intervals) of true value

Application of t Test: Comparison between true and mean value, comparison between means, comparison for paired samples (measurement on the same sample, comparison for multiple or different samples), application for corticosteroid analysis. Correlation check by means of t-Test

Test F (significance tests)

test (or Q-test)

- Quality control:

Quality System, Analytical Quality Control

Validation, Reliability, Commutability, Traceability

Classification of standards (for atomic weights, definitive, primary, working, secondary) and of analysis methods (definitive, reference, known error, unknown error)

Standard and Reference Materials (certified and not)

Control standards (control serum)

Control cards

Good Laboratory Practice

Qualitative and quantitative analysis

Choice and confirmation of an analytical method

Safety measures

- Processing of the sample:

Pre-analytical variability

Chemical-physical characteristics

Analyte-matrix interaction

Sampling of homogeneous and segregated materials

Sampling constant

Number of Samples and sampling error

Sampling error and analytical error

Reference intervals

- Radiochemistry:

Radioactivity: Principles and applications

Measurements units: Becquerel (Bq), Gray (Gy) and Sievert (Sv)

Decay modes: Alpha, beta-, beta+, electronic capture, spontaneous fission

Radiation associated with nuclear decay: gamma emissions, conversion and Auger electrons, X radiation

Decay laws: Half-life time, average life and kinetics of decay

Radiation detectors, Photographic emulsions: examples of qualitative and/or quantitative analyses

Radiation safety

Applications of Radiochemistry: Analysis by activation with neutrons, Analysis by isotope dilution (Analysis of body water volume), Radioimmunological analysis, Analysis and determination of enzymatic activities

- Main applications in the chemical, pharmaceutical, environmental and food sectors of the analytical methods listed above.

- Practical exercises applied to the main topics.

- Practical tests. Bibliographic research on how to find scientific journals.

Programme of the Module “Exercises of Analytical Chemistry”. Teacher: Dr Andrea Zattoni.

1.1)    Calculus in Analytical Chemistry

1.1)    Units

1.2)    Solutions and their concentration

1.3)    Chemical stoichiometry

1.4)    Exercises

2.0)    Chemical equilibria in aqueous solutions

2.1)    Acid-base conjugate pairs

2.2)    Buffer solutions

2.3)    Exercises

3.0)    Equilibrium problems for complex systems

3.1)    Solution of equilibrium problems with the systematic method

3.2)    Solubility calculations with the systematic method

3.3)    Exercises

4.0)    Titrations

4.1)    Titration glossary and volumetric calculations

4.2)    Exercises

5.0)    Neutralization titrations: theory

5.1)    Acid-base titration curves

5.2)    Titration curves for strong acids and bases

5.3)    Titration curves for weak acids

5.4)    Titration curves for weak bases

5.5)    Composition of buffer solutions as a function of pH

5.6)    Exercises

6.0)    Titration curves for complex acid-base systems

6.1)    Strong-weak acid of base mixtures

6.2)    Polyfunctional acids and bases

6.3)    Buffer solutions with polyprotic acids

6.4)    Calculation of pH for amphiphilic salts

6.5)    Titration curves for polyfunctional acids and bases

6.6)    Titration curves for amphiprotic species

6.7)    Composition of a polyprotic acid as a function of pH

6.8)    Exercises

7.0)    Applications of neutralization titrations

7.1)    Exercises

8.0)    Precipitation titrations

8.1)    Titration curves

8.2)    Argentometry

8.3)    Mohor,Volhard and Fajans methods

8.4)    Exercises

9.0)    Complexation titrations

9.1)    Titrations with EDTA

9.2)    Exercises

10.0)    Introduction to electrochemistry

10.1)    Redox reactions

10.2)    Electrochemical cells

11.1)    Electrodic potentials

11.2)    Thermodynamic potential of electrochemical cells

11.3)    Redox titration curves

12.1)    Oxidizing and reducing agents

12.2)    Applications of oxidizing and reducing agents

12.3)    Exercises

12.4)    Potentiometry

12.5)    Reference electrodes

12.6)    Indicator electrodes

13.1)    Potentiometric titrations

13.2)    Electrolysis

13.3)    Effect of current on electrodic potentials

14.0)    Electrogravimetry

14.1)    Coulometry

14.2)    Exercises

 

Readings/Bibliography

- Transparencies of the lessons can be downloaded from the site: http://bomet.fci.unibo.it/girotti/Socrates/didattica/lucidi.html

- "Chimica Analitica: una Introduzione", D.A. Skoog, D.M. West, F.J. Holler, (EdiSES, S.r.l., Napoli, 1996).

- "Elementi di Chimica Analitica", Daniel C. Harris (Zanichelli Editore, Bologna, 2005).

- "Chimica Analitica, teoria e pratica", F.W. Fifield, D. Kealey (Zanichelli Editore, Bologna, 1999).

- "Fondamenti di Chimica Analitica", D.A. Skoog, D.M. West, F.J. Holler, S.R. Rouch (EdiSES, S.r.l., Napoli, 2005).

- "Chimica Analitica Strumentale", F.J. Holler, D.A. Skoog, S.R. Crouch, (EdiSES, S.r.l., Napoli, 2009).

Teaching methods

Lessons in which the course topics will be presented and discussed, with explanatory numerical exercises. Exercises on the use of a scientific calculator for statistical applications. Practical tests. Bibliographic research on how to find scientific journals, in-depth seminars.

Assessment methods

N.B.To pass the exam it is necessary to know how to use a calculator in the subjects covered in the course (e.g. standard deviation, least squares, etc.). This test, together with discussion on the results of the bibliographic research, is preparatory to the continuation of the oral exam and will take place individually at the start of the oral exam.
Oral exam on the entire programme. Assessment is based on the student being able to demonstrate that he/she knows how to use and apply the knowledge, information and cultural means provided by the course, also checking bibliographic research. The threshold of learning sufficiency is represented in particular by the demonstration of critical understanding and the ability to discuss the course topics.
The lecturer is available for further clarification and to asses the level of pre-exam preparation.

Teaching tools

Video projector, PC, beamer, Internet and You Tube links.

Links to further information

http://bomet.fci.unibo.it/girotti/

Office hours

See the website of Stefano Girotti

See the website of Andrea Zattoni