27604 - Analytical Chemistry

Academic Year 2022/2023

  • Docente: Mara Mirasoli
  • Credits: 6
  • SSD: CHIM/01
  • Language: Italian
  • Moduli: Mara Mirasoli (Modulo 1) Maria Maddalena Calabretta (Modulo 2)
  • Teaching Mode: Traditional lectures (Modulo 1) Traditional lectures (Modulo 2)
  • Campus: Bologna
  • Corso: Single cycle degree programme (LMCU) in Pharmacy (cod. 9219)

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.

Statistics: 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

Module 1

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, preparation of buffer solutions, 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:

The laboratory experiences will be held in groups, programmed on the basis of the rules on the sanitary situation.

As concerns the teaching methods of this course unit, all students must attend Modules 1 and 2 online, while Module 3 on health and safety is to be attended in class or on Microsoft Teams according to the modality chosen by the teacher. Information about Module 3 attendance schedule is available on the website of your degree programme.

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: Calibration of volumetric equipment. PURPOSE: To become familiar with the laboratory, verify that the instrumentation to be used is in optimal condition, use of the simplest statistical parameters, write a report.
SECOND EXPERIENCE - TITLE: Preparation of a buffer solution and potentiometric measurement of the pH. PURPOSE: Design the preparation of a buffer solution given pH and concentration, use the pH meter, measure the buffering capacity of the buffer solution.
THIRD EXPERIENCE - TITLE: Potentiometric titration of a strong acid and a weak acid. PURPOSE: To become familiar with the use of the burette, to produce potentiometric titration curves, to compare the titration curve of a strong acid and a weak acid

Module 2

Purpose of Analytical Chemistry.
Sampling: Generalities, definitions and role in the analytic process. Randomized sampling and sampling plan. Sampling of solids, liquids and gases. Effect of sampling on the uncertainty of the results.
Laboratory glassware.

Statistical treatment of experimental data and quantitative analysis: errors in analytical chemistry (systematic and random errors). Absolute error and relative error, statistics of errors and probability distribution: Gaussian curve. Tests of significance (test t, test f, test q), error propagation, significant figures, reporting experimental data in accordance to the error, calibration (external calibration, standard additions, internal calibration).
Correlation and regression: Method of least squares, correlation coefficient, characteristics of an analytical procedure (accuracy, precision, specificity and selectivity, linearity range, limit of detection and limit of quantification, robustness). Sensitivity and analytical sensitivity.
Standards and reference materials (certified or not).
Ways of expressing the analysis results
Comparison between true value and average comparison between means, paired samples for comparison.

 

Readings/Bibliography

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

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

- 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 books can be freely chosen by the student.

The following book contains both the theoretical part and numerous exercises with detailed explanation for their execution, only for the subjects of Module 2:

"Il Laboratorio di Chimica Analitica - Concetti di base ed esercizi svolti" M. Grotti, F. Ardini (EdiSES, S.r.l., Napoli, 2022).

The following book, 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

Lectures in which the topics of the course are presented and discussed, with explanatory numerical exercises. Students are assigned exercises to be performed independently and delivered via VIRTUALE for correction by the teacher.


Laboratory activities with practical exercises in single place, preparation of a report, with discussion at the exam. As an introduction to the laboratory activities, information material (including videos) and self-assessment tests are available on VIRTUALE.

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 and/or maria.calabretta2@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 Youtube links, video of laboratory experiences.

Office hours

See the website of Mara Mirasoli

See the website of Maria Maddalena Calabretta

SDGs

Good health and well-being Quality education

This teaching activity contributes to the achievement of the Sustainable Development Goals of the UN 2030 Agenda.