90962 - Analytical Chemistry (GR.B)

Course Unit Page

SDGs

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

Good health and well-being

Academic Year 2021/2022

Learning outcomes

At the end of the course the student will:

- acquire (also through laboratory and exercise activities) the basics of analytical chemistry which are required for performing and evaluating quality control analyses of pharmaceutical principles and formulations and which may be helpful to the comprehension of drugs validation studies;

- achieve a comprehensive understanding of the analytic process (from the choice of method of analysis to results elaboration and interpretation) and of the main classical and instrumental methods of analysis, being able to clearly and unambiguously communicate to specialist and non-specialist audiences the analytical results and their critical interpretation;

- have the knowledge that enables him/her to critically evaluate (also employing statistical and chemometric tools) the obtained experimental results and those reported in drugs development or application studies and obtained in the quality control of medicines and health products;

- have 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).

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

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 Module 1, 2 online (https://www.unibo.it/en/services-and-opportunities/health-and-assistance/health-and-safety/online-course-on-health-and-safety-in-study-and-internship-areas), while Module 3 on health and safety is to be attended in class. 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: 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.

The course is divided into two modules:

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

- 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

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.

- UV-Vis spectroscopy

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).

 

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

- The Analytical Process

- The Analytical Chemist’s Job: General Steps in a Chemical Analysis

- Basic Tools:

The Lab Notebook, Analytical Balance, Burets, Volumetric Flasks, Pipets and Syringes, Calibration of Volumetric Glassware, Introduction to Microsoft Excel®, Graphing with Microsoft Excel, Safe, Ethical Handling of Chemicals and Waste.

- SI Units

- Chemical Concentrations

- Preparing Solutions

- Data treatment – Statistics:

Experimental Error, Significant Figures, Significant Figures in Arithmetic, Types of Error, Propagation of Uncertainty from, Random Error, Means, Comparison of Means with Student’s t, Comparison of Standard Deviations with the F Test, t Tests with a Spreadsheet, Grubbs Test for an Outlier, Propagation of Uncertainty from, Systematic Error, Gaussian Distribution, Confidence Intervals.

- Method validation

Accuracy, Precision, Sensibility (Limit of Detection, LOD, Limit of Quantitation, LOQ) Linearity, Recovery, Robustness, The Method of Least Squares, Calibration Curves, Dynamic range and linear (dynamic) range, Standard Addition, Internal Standards, Classification of standards (for atomic weights, definitive, primary, working, secondary), methods of analysis (definitive, reference, known error, unknown error), Ways to express the result of the analysis, Limits (or ranges) of reliability or trust of true value.

- Quality Assurance

The Need for Quality Assurance, Basics of Quality Assurance, Quality System (ISO 9000: 2015) and Analytical Quality Control, Reliability, Switchability, Traceability, Validation, Standard and reference material (certified and non-certified), Degree of water purity, Control standards, Control cards, Good Laboratory Practice, Qualitative and quantitative analysis, Choice and validation of an analytical method, Security measures.

- Exercises applied to the main topics.

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:

- Quantitative Chemical Analysis, by Daniel C. Harris, Charles A. Lucy

- Analytical Chemistry and Quantitative Analysis, by David S. Hage, James R. Carr

- Fundamentals of Analytical Chemistry, by Douglas A. Skoog, Donald M. West, F. James Holler, Stanley R. Crouch

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 held in the classroom (or available at the same time for students in class and students in teleconference, depending on the sanitary situatuon). In these lessons, topics are presented and discussed, with explanatory numerical exercises executed at the blackboard. Exercises on statistical applications of analytical data. Practical tests. 

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 are 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 or jessica.fiori@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 discussion of the laboratory reports. 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.

Office hours

See the website of Mara Mirasoli

See the website of Jessica Fiori

See the website of Jessica Fiori