27604 - Analytical Chemistry

Learning outcomes

At the end of the course the student:

- acquires the fundamental notions of analytical chemistry useful for the completion and evaluation of medication controls and for the understanding of drug validation studies, also through laboratory and practical activities and experiences;

- reaches a global vision of the analytical process, starting from the choice of the method of analysis up to the elaboration of the results, and of the typologies of classical and instrumental methods of analysis, communicating their conclusions and the knowledge in a clear and unambiguous way and the rationale underlying them, to specialist and non-specialist interlocutors;

- has the tools to be able to critically evaluate (also by statistical and chemometric means) both the experimental results obtained and those reported in the drug application studies and in the quality control of medicines and health products;

- possess the necessary knowledge to face the courses of the following years.

Course contents

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. Mean values of a series of data, mode, median and weighted mean. Standard deviation, relative standard deviation and coefficient of variation, variance. 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).

Mathematics: Logarithms: significance, use and calculations, Calculation with exponential numbers, Quadratic equations.

Statistics: Basic concepts, Correlation check by means of t-Test

The course is divided into two modules:

Programme of the Module “Analytical Chemistry 1” (Mara Mirasoli).

Chemical equilibria in aqueous solution, acid - base conjugate pairs, buffer solutions. Titrations: introduction, volumetric calculations. Neutralization titrations: titration curves for strong acids and bases, titration curves for weak acids and bases, buffer solutions composition as a function of pH, titration of a polyprotic acid, of a polyfunctional base, of an amphiprotic species, chemical indicators for neutralization titrations, applications of neutralization titrations.

Introduction to potentiometry: junction potential, reference electrodes, indicator electrodes (metallic electrodes of first kind, of second kind and inert; ion-selective electrodes), direct potentiometric analysis, glass electrode, errors and use of glass electrode, combined glass electrodes and electrodes selective for other ions with crystalline, liquid or polymeric membrane.

Spectrophotometric analysis methods: electromagnetic radiation, absorption spectra in gaseous and condensed phase (electronic, rotational and vibrational spectra), absorbance and transmittance, Lambert-Beer law, deviations from the Lambert-Beer law, analysis of mixtures, spectrophotometric error, spectrophotometry instrumentation (sources, filters and monochromators, sample cells, detectors, instrument configurations).

LABORATORY:

The laboratory experiences will be held in three days in the week from December 2nd to December 5th, 2019. Students will be divided into two groups, according to their organizational needs. Group A will attend the workshop in the morning and group B in the afternoon of the same day.

To attend the laboratory, it is requested that students have completed the compulsory course on safety at work and they have handed over to the teacher (or sent by e-mail to mara.mirasoli@unibo.it) a copy of the certificate of passing the final exam.

Each student is required to procure and wear the chemical lab coat.

FIRST EXPERIENCE - TITLE: Equipment calibration. PURPOSE: Become familiar with the laboratory, verify that the instrumentation to be used is in optimal condition, use of the simplest statistical parameters, use of the regression method to build a linear calibration curve, writing a laboratory report.

SECOND EXPERIENCE - TITLE: Preparation of a buffer solution and potentiometric pH measurement. PURPOSE: Use of buffer solutions, glass electrode, pH meter and analysis of a real matrix (vinegar or lemon juice).

THIRD EXPERIENCE -TITLE: Titration of a weak acid and construction of a titration curve by potentiometric measurement of pH. PURPOSE: Verify the shape of the titration curve and identify the characteristic points.

Programme of the Module “Analytical Chemistry 2” (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).

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

Calibration; Comparators, transducers, sensors and biosensors, calibration of a balance, a micropipette, a pipette, calibration of the pH meter.

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)

Choice of an instrumental method.

Absolute and relative uncertainty.

Accuracy: trueness and precision (inaccuracy and imprecision), Repeatability, reproducibility.

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

Absolute error, relative error and relative percentage error

Standard deviation, relative standard deviation and coefficient of variation.

Scientific method: Placebo effect and Alternative Medicines, Meta-research

Discussion of the application of the scientific method to a case/real research: *La trappola di Science, *Olio di Palma, *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.

- On-line course 7.1 Patents and patent application of the TOX-OER Project (https://toxoer.com/): Patents and patent applications, examples of patenting, patentability, the right to priority, patenting in the chemical field, international conventions such as the European patent convention.

- Practical exercises applied to the main topics.

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

Readings/Bibliography

Material: the material presented in class is made available to the student in electronic format.

The course material and notes taken in class are essential for the exam, as well as one of the following texts:

- Fondamenti di Chimica Analitica Quantitativa", Daniel C. Harris (Zanichelli Editore, Bologna, 2017).

- "Fondamenti di Chimica Analitica di Skoog e West”, F. J. Holler, S. R. Crouch (Edizione: III, EdiSES, S.r.l., Napoli, 2015).

- “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, 2017).

Other university-level analytical chemistry texts can be freely chosen by the student.

The following text, in which the theoretical part is only recalled to great signs, contains numerous exercises with detailed explanation for their execution:

- "Esercizi per la Chimica Analitica, con richiami di teoria", S. Araneo, (Progetto Leonardo, Esculapio, Bologna, edizione 2012 e edizione 2018). 

Teaching methods

Lessons in which the course topics are presented and discussed, with explanatory numerical exercises executed at the blackboard. 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 learning takes 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 on Almaesami, in compliance with mandatory deadlines. Students are invited to unsubscribe if they are not interested in taking the examination. Cancellations must be made on Almaesami or, in alternative, by writing an email to the teacher at mara.mirasoli@unibo.it [mailto:mara.mirasoli@unibo.it] or stefano.girotti@unibo.it [mailto:stefano.girotti@unibo.it] .

To pass the exam of the Module “Analytical Chemistry 2” (Stefano Girotti) it is necessary to to know how to use a calculator in the subjects covered in the course (least squares). Such a test together with the discussion of bibliographic research carried out, discussion and certification (carry the certificate) relating to the attendance and passing of the online course “7.1 Patents and patent application” of the TOX-OER Project (https://toxoer.com/) and the application of the scientific method to a case/real research, 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 and discussion of the laboratory report. 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.

Office hours

See the website of Mara Mirasoli

See the website of Stefano Girotti