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 drugs 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

RIMINI

- 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 “Instrumental Analytical Chemistry”. Teacher: Dr. Mara Mirasoli.

Instrumental Analytical Chemistry
Fundamentals of analytical chemistry

Activity and concentration: ionic strength; activity; determination of activity coefficients. Equilibrium systems. Equilibria in solution. Principles of volumetric analysis. Main applications in the pharmaceutical field.

Instrumental analytical techniques

The analytical signal, qualitative and quantitative aspects: signal-to-noise ratio; methods for noise elimination. Instrumentation in analytical chemistry: principles of instrumental analytical chemistry; main components of instrumentation for analytical chemistry.

Atomic and molecular spectroscopy

Definition of electromagnetic radiation; interaction between radiation and matter: absorption and emission, energy levels and transitions; qualitative aspects: absorbance and emission spectra; quantitative aspects: Lambert-Beer law. Absorbance and emission atomic spectroscopy: principles and instrumentation; flame, electrothermal and plasma (ICP) sources. Molecular absorption spectroscopy (UV-Vis): principles and instrumentation; definition of chromophore group. Molecular emission spectroscopy: principles and instrumentation; photoluminescence and bio-chemiluminescence. Applications in the pharmaceutical field.

Electroanalysis. Introduction. Potentiometry. Voltammetry.

Principles of separation. Liquid-liquid extraction. Solid phase extraction. Solid phase microextraction. Principles of chromatography. Liquid chromatography. Gas-chromatography.

Bioanalytical methods. Methods for quantitative analysis based on biosepcific molecular recognition. Enzymatic methods. Immunoassays and nucleic acids hybridization methods: principles and applications. Tracers and their use.

 

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 Mara Mirasoli