00090 - Analytical Chemistry

Learning outcomes

At the end of the course the student will: - acquire the basics of analytical chemistry which may be helpful to the evaluation and control of medicines and comprehension of the validation studies of drugs, - achieve a comprehensive understanding of the analytic process, from the choice of method of analysis to the elaboration of the results, and the types of classical and instrumental methods of analysis, communicating clearly and unambiguously their conclusions, and the knowledge and rationale underpinning these, to specialist and non-specialist audiences; - has the tools to be able to critically evaluate (including by statistical and chemometric) the obtained experimental results and those reported in studies of drug application and in the quality control of medicines and health products - has the required knowledge to deal the courses of the following years.

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.). Such a test together with the discussion of bibliographic research carried out and the application of the scientific method to a case / real research, 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: trueness and precision (inaccuracy and imprecision)

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

Discussion of the application of the scientific method to a case / real research: Case Di Bella, Zamboni Care Studies, Cochrane, verification homeopathy, etc..

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:

Sampling of homogeneous and segregated materials

Sampling constant

Number of Samples and sampling error

Sampling error and analytical error

Reference intervals

- 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.

Discussion of the application of the scientific method to a case / real research:  *La trappola di Science, *Caso Di Bella, *Aura Activator, *Cellule staminali e vitamine, *Effetti desiderati, *Chi controlla i placebo, *La medicina bugiarda, *Le verità scadono, *Cosa fare fare in mancanza di piene certezze scientifiche?, *Verità manipolate, *Disinformazione, * Cura Zamboni, *L'ostracismo verso la scienza, *Studi Cochrane, *Come si possono influenzare anche gli animali, *verifica omeopatia, * Le altre medicine , *Farmaci o Medicinali, *Efficacia terapeutica della preghiera, *Aromaterapia, etc.

Programme of the Module “Exercises of Analytical Chemistry”. Teacher:  Dr.  Mara Mirasoli.

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

Readings/Bibliography

Material: the material presented in class is made available to the student in electronic format via the Internet, to obtain educational materials: http://campus.unibo.it/ (restricted access to students enrolled at the University of Bologna ).
The course material and notes taken in class are essential for the exam. As a reference, the student can possibly deepen the arguments of one of the following texts:

 

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

- “Chimica Analitica e Analisi Quantitativa”, D.S. Hage, J.D. Carr, (Piccin Nuova Libraria SpA, Padova, 2012).

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

 

- "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).

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

 

- "Esercizi per la Chimica Analitica, con richiami di teoria", S. Araneo, (Progetto Leonardo, Esculapio, Bologna, 2012).

 

Teaching methods

Lessons in which the course topics are 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

The assessment of learningtakes place only through the final exam, which ensures the acquisition of knowledge and skills expected by conducting an oral interview and the resolution of numerical problems of the entire program, on both modules, which can be broken down into moments of verification separated. The marks obtained in the two modules are then combined to obtain the final grade of the final exam by weighted means and hare valid for one year.

The exam registration is required by Almaesami, in compliance with mandatory deadlines. It invites you to unsubscribe if you do not interested in supporting the examination, otherwise you can not take the exam in the appeal below. Cancellations must be made before the time end of the list.

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.

The evaluation criterion is based on the demonstration by the student to be able to use and apply the knowledge, information and cultural tools provided by the course, with control of the Bibliographic search. The threshold of sufficiency of learning is represented in particular by the demonstration of critical understanding and ability to discuss about the topics of the course, as well as the resolution of numerical problems.

The teacher is available for further clarification, and to verify the level of pre-exam preparation by appointment.

Teaching tools

Video projector, PC, Internet and You Tube links.

Links to further information

http://www.unibo.it/docenti/stefano.girotti

Office hours

See the website of Stefano Girotti

See the website of Mara Mirasoli