Analytical Chemistry

The aim is to provide background information on instrumental analytical chemistry with specific reference to spectroscopy and separation techniques.

Knowledge and understanding

Knowledge of the basics, operating principles and applications of the main spectroscopic and separation techniques. Knowledge of statistics and final data processing.

 Applying knowledge and understanding

Ability to apply and organize the analitical chemistry knowledges referring to the different topics covered in the course.

 Making judgements

Ability to analyze and critical evaluations of different topics learned during the course.

 Communication skills

Ability to expose the topics covered with terminological rigor and language properties.

 Learning skills

Ability to tackle advanced studies with good autonomy.

Lectures and numerical exercices.

Should teaching be carried out in mixed mode or remotely, it may be necessary to introduce changes with respect to previous statements, in line with the programme planned and outlined in the syllabus.

Learning assessment may also be carried out on line, should the conditions require it.

Knowledge of fundamentals of chemistry, physics and mathematics.

As stated in the University Teaching Regulations and Course Regulations.

Spectroscopy. Electromagnetic radiation: wave-particle dualism, photoelectric effect and diffraction, Heisenberg's principle. Electromagnetic spectrum. Refraction, refractive index, Snell's law, total internal reflection. Interaction of radiation with matter: reflection, transmission/absorption, diffusion. Absorption and emission of radiation. Atomic absorption. Molecular absorption. Vibrational and rotational motions. Fluorescence, phosphorescence.

Molecular spectroscopy - UV-vis. Transmittance, absorbance, Beer's law. Limitations of Beer's law. Photometer and spectrophotometer. Single beam spectrophotometer, Double beam spectrophotometer. Sources. Wavelength selectors.

Molecular spectroscopy – infrared. General characteristics. Harmonic and anharmonic oscillator, dipolar moment of transition. Molecular vibrational modes. Main IR signals: functional groups area, fingerprint area. Dispersion spectrophotometers. Fourier transform spectrophotometers: Time domain and frequency domain, Fourier transform, Michelson interferometer. Sources. Detectors. IR spectrum characteristics and interference. Cells for gas and liquid analysis. Solids analysis. 

Atomic spectroscopy. Instrumentation for atomic absorption, emission and fluorescence. Atomic absorption. Atomic absorption instrumentation. Atomic emission spectrometry: inductively coupled plasma sources.
 

Mass spectrometry. Fundamentals – Ion sources: electron impact (EI), chemical ionization (CI), field ionization (FI), field desorption (FD), fast atom bombardment (FAB), matrix assisted laser ionization-desorption (MALDI), electrospray – Fragmentation pattern – Metastable ions -  Mass analyzer: magnetic sector, electrostatic sector, quadrupole, ion trap, time of flight  (ToF), orbitrap – Detectors - Approximate and exact masses – Resolution – Isotopic abundances of C, S, Cl, Br and their effects on mass spectrum – Nitrogen rule – Unsaturation degree – Recognition of simple organic compounds. 

Separation techniques. Chromatography – Generality - Chromatographic plate theory - Chromatographic velocity theory - Partition and adsorption chromatography: on paper, thin film, columns.  High performance liquid chromatography - Ionic chromatography - Size exclusion chromatography - Instrumentation. Gas chromatography: principles and comparison with liquid chromatography; instrumentation. 

Statistics. Absolute and relative error. Types of errors. Accuracy and precision. Variance, standard deviation, standard error, relative standard deviation. Normal Distribution, Student Distribution, χ2 Distribution. Matrix effect, recovery, method of standard additions. Sensitivity. Limit of detection and quantification.

1.      D. A. Skoog, Holler, Crouch, Chimica Analitica Strumentale II edizione, EdiSES, Napoli, 2009.

2.      D. C. Harris, Chimica Analitica Quantitativa, III edizione, Zanichelli, 2017.

3.      Skoog, West, Holler, Crouch, Fondamenti di Chimica Analitica, III edizione, EdiSES, 2015.

4.      D. C. Harris, Quantitative Chemical Analysis, 9th ed. W.H. Freeman and Company, New York, US, 2016.

Oral interview. The exam is designed to ascertain the acquisition of the concepts covered during the lectures and the ability to expound concepts using appropriate scientific language.

Unsuitable

Knowledge and understanding of the topic: Modest shortcomings.

Ability to analyze and synthesize: Irrelevant. Frequent generalizations.

Use of references: Completely inappropriate.

18-20

Knowledge and understanding of the topic: very modest. Obvious imperfections.

Ability to analyze and synthesize: just enough skills.

Use of references: just suitable.

21-23

Knowledge and understanding of the topic: more than enough.

Analysis and synthesis skills: It is capable of discrete analysis and synthesis. Argue logically and consistently.

Use of references: Use standard references.

24-26

Knowledge and understanding of the topic: good knowledge.

Analysis and synthesis skills: Has good analysis and synthesis skills. The arguments are expressed consistently.

Use of references: Use standard references.

27-29

Knowledge and understanding of the topic: knowledge more than good.

Ability to analyze and synthesize: considerable abilities of analysis and synthesis.

Use of references: exploring of the topics.

30-30L

Knowledge and understanding of the topic: excellent knowledge.

Ability to analyze and synthesize: considerable abilities of analysis and synthesis.

Use of references: important insights.

Verification of learning may also be conducted electronically, should conditions require it.

Information for students with disabilities and/or DSA:

To ensure equal opportunity and in compliance with current laws, interested students may request a personal interview so that any compensatory and/or dispensatory measures can be planned, based on educational objectives and specific needs.

Theory and applications of atomic absorption spectroscopy.

Separation techniques.

Molecular fluorescence spectroscopy.

Description of theoretical principles relating to a mass analyser.