Learning outcomes of the course unit
One of the main objectives is to make the student learn the main analytical techniques, their potential in the various fields of application, in particular the pharmaceutical one. A further objective will be to provide the student with the understanding and use of a scientific-analytical descriptive language.
The understanding of the theoretical bases on which the main analysis systems are based will be fundamental.
In addition, the student will develop the ability to correctly process data according to the validation and statistical criteria, in order to provide a reliable analytical result.
Regarding the skills that the student will acquire,
they include the application of the theoretical foundations concerning the development of analytical methodologies and the choice of the technique suitable for solving an analytical problem, considering possible advantages and disadvantages and an analytical language.
The student must develop the necessary critical skills to set up an analysis protocol, starting from the sampling, taking into account the possible phases of sample preparation and analysis.
It will also have the possession of the cognitive tools for the interpretation of analytical data with the help of statistical principles in order to be able to assess the reliability of the data obtained from a series of analyzes.
The candidate must have knowledge of General Chemistry exam.
Course contents summary
A first part of the course concerns the presentation of the role of analytical chemistry in research and industry, underlining the importance that its application finds in various sectors in an interdisciplinary manner with connections with the other lectures and in particular in the pharmaceutical sector. This section will deal with topics such as: the validation of analytical methods, sampling, sample treatment techniques and the theory of errors related to obtain reliable analytical data.
In a second part, the application of some basic concepts of general chemistry that the student already knows, by reviewing fundamental references to topics such as chemical balance, pH, buffer solutions, salt hydrolysis, titrations, solubility and electrochemistry will be shown. This in order to provide the basis for the understanding of analytical methods based on these principles, such as volumetric and gravimetric analysis.
The third part is dedicated to analytical instrumental chemistry for qualitative and quantitative determination. The main topics that will be explored are the spectrophotometric methods and the chromatography.
The main instruments and potentials of modern analytical techniques will be described, focusing attention on applications in the pharmaceutical field.
The role of Analytical Chemistry. Concept of analytical procedure and qualitative and quantitative analysis.
Stages of a typical quantitative analysis. Sampling. Sample treatment. Extraction.
Uncertainty associated with a measure: types of error; sensitivity, accuracy and precision. Expression of the analytical data.
Gaussian distribution. Standard deviation. Significance test. Quality of the analytical data.
Basic general concepts
Unit of measurement of solution concentration. Preparation of weighing and dilution solutions. Calculation exercises.
Ionic product of water. Chemical equilibrium.
Acids and bases. Calculation of the pH and concentration of the species present at the equilibrium of solutions of acids and strong bases. Calculation of the pH and of the concentration of the species present at the equilibrium of weak acid and base solutions. Polyprotic acids. Ionisation according to pH.
Salt hydrolysis. Calculation of the pH of saline solutions.
Buffer solutions. Calculation of the pH of buffer solutions. Buffering capacity.
Precipitation balances. Solubility product. Types of precipitates. Ion to common. Effect of pH on solubility.
Standard potential, eq by Nernst. Stack, pH meter
General principles. Determination of the title of a solution. Definition of primary standard.
Acid-base titrations. Titration curves of strong acids with strong bases and vice versa. Titration curve of weak acids with strong bases and vice versa. Indicators for acid-base titrations.
Complexometric titrations. EDTA.
Precipitation titrations (Mohr method and Volhard method).
Spectroscopic methods of analysis
Electromagnetic waves. Property. Absorption and emission. Origin of spectra, relationship between electronic structure and absorption bands. Spectral fields of analytical interest and types of energy transitions.
UV-visible spectrophotometry. Lambert-Beer Law. Limitations. Instrumentation. Quantitative analysis.
Molecular fluorescence. Characteristics of fluorescent substances. Derivatizing. Instrumentation.
Molecular spectrophotometry in Infrared absorption. Origin of the spectra. Bands characteristics. Instrumentation.
Atomic spectroscopy. Instrumentation: sources, atomization systems.
Chromatographic analysis methods
Introduction to chromatographic methods. Principles. General description of the chromatographic techniques. Liquid chromatography. Qualitative and quantitative analysis. Mechanisms of separation. Adsorption and breakdown chromatography. Direct and inverse phase, ion exchange, molecular exclusion.
Chromatographic parameters. Van Deemter's equation.
Instrumentation for HPLC. Injector, columns, pumps. Refractive index detector; ELSD; UV-DAD; fluorescent; electrochemical detectors. Isocratic and gradient elution.
Gas chromatography. Principles. Instrumentation: injectors, columns, detectors.
Mass spectrometry and combined techniques. Acquisition mode.
Construction of a calibration line. Method to external and internal standards. Linearity. Detection limit, quantification limit.
- Harris, Chimica Analitica Quantitativa, Ed. Zanichelli
- Skoog, West, Holler, Crouch, Fondamenti di Chimica Analitica. EdiSES.
- Hage, Carr, Chimica Analitica e Analisi Quantitativa. Ed. Piccin
PowerPoint files used for lessons
For the first part of the program the explanations will be based on frontal lessons with the help of the chalkboard for the implementation of examples and explanatory charts.
For the instrumental part during the lessons the teacher will use the projection of schemes, video and photographs that will help the description of the instrumentation.
Exercises: Simple exercises will be proposed in order to reproduce some common procedures that may occur in a laboratory for the preparation of solutions and so on.
Other tutorials will be devoted to showing the use of common software dedicated to analytical data processing, for example for building calibration lines, charts, or for computing results using some of the statistical notions.
Assessment methods and criteria
The exam includes a written test lasting 3 hours with both exercises and theory questions. If the written exam is passed the student will be able to accept the vote as definitive or access the optional oral exam to improve the grade of the written exam. The questions will cover the theoretical principles but also the processing of data by exercises, and the construction of graphs.
For the purposes of evaluation, the teacher's attention will be focused on the training aspect rather than on the descriptive and informative one, in order to verify if the student, in addition to acquiring knowledge, has acquired awareness of the usefulness of them for the solution of common problems that can be encountered in practical laboratory work.
For the overall opinion, reference can be made to the following items: Knowledge and understanding of the subject: 80%
- Ability to apply knowledge and understanding: 15%
- Communication skills: 5%
The written exam will be passed if both the exercises and the theory questions are sufficient. They result sufficient when more than the half of the questions are correct.