27604 - 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

- 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). Correlation check by means of t-Test

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

Programme

- 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)

Absolute error and relative error

Absolute and relative uncertainty

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

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

Calibration diagram method

Standard addition method, standard additions method, percentage recovery

Internal standard method

test (or Q-test)

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

- Practical exercises applied to the main topics.

Volumetric titrations:

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.

Potentiometry and conductivity:

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.

Conductimetric measurements and their use in volumetric titrations.

LABORATORY:
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, writing of a relationship.
SECOND EXPERIENCE - TITLE: Potentiometric pH measurement ,. PURPOSE: Use of pads, glass electrode, pH meter and analysis of a real matrix (vinegar or lemon juice).
THIRD EXPERIENCE - TITLE: Conductimetric measurements. PURPOSE: Measurements with conductivity meter of various water samples

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 will be available in parallel for students present in the classroom and students in teleconference. During lessons, the course topics are presented and discussed, with explanatory numerical exercises. 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. Cancellations must be made before the time end of the list or via email to mara.mirasoli@unibo.it.

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 teachers are 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. Teams platform for students in teleconference.

Office hours

See the website of Mara Mirasoli

See the website of Maria Maddalena Calabretta