Course program
1. Sample preparation and main extraction techniques.
Notes on sampling and the main extraction techniques.
2. Method validation.
Notes on the main parameters necessary for the validation of an analytical method (sensitivity, LOD, LOQ, precision, accuracy) and on the methods for carrying out a quantitative analysis (external calibration, internal calibration, method of standard additions).
3. Introduction to instrumental analysis methods: Classification of instrumental analytical techniques.
3.1 Spectroscopic techniques.
- Molecular UV-visible spectrophotometry. Instrumentation (sources, monochromators, detectors, diode array detector). Definition of transmittance and absorbance. Beer-Lambert Law.
- Fluorescence spectrophotometry. Fundamentals. Instrumentation. Quantum yield.
- Atomic absorption spectrophotometry. Instrumentation: sources, atomization systems, background correction systems. Spectral and non-spectral interferences.
- Atomic emission spectrophotometry. Instrumentation: ICP source, monochromators, detectors.
- Mass Spectrometry. Principles. Instrumentation: ionisation techniques, analyzers, resolution, mass accuracy. Isotopic distribution. Applications
3.2 Chromatographic techniques.
- Fundamentals: distribution coefficient; capacity factor; column efficiency; symmetry parameter; van Deemter’s equation; selectivity; sample capacity; resolution.
- Liquid Chromatography. Separative techniques in liquid chromatography. Main chromatographic techniques (LAC, liquid adsorption chromatography, liquid-liquid partition chromatography, ion exchange chromatography, size exclusion chromatography, affinity chromatography). Instrumentation for HPLC (high performance liquid chromatography). Isocratic and gradient elution. Detectors (absorbance detectors; fluorescence detectors; refraction index detectors, MS detectors.
- Gas chromatography. Instrumentation. Types of columns and stationary phases. Detectors (flame ionization, thermal conductivity, electron capture).
3.2. Electrochemical methods of analysis. Potentiometry, voltammetry, Polarography, amperometry (just an introduction).
3.3 Sensors and Biosensors. Principles and instrumentation
3.4 Thermal analysis
Practical laboratory exercises:
Experiment 1: quantitative dosage of caffeine by HPLC-UV
Experience 2: alcohol content measurement using GC-FID
Prerequisites
Prerequisites include fundamentals of basic analytical chemistry: equilibrium in a homogeneous and heterogeneous phase; aqueous solutions of electrolytes; activity, concentration, ionic strength and activity coefficient; acids and bases according to Bronsted and Lewis; buffer solutions, buffer power, ampholyte solutions; strong and weak monoprotic acids; complex formation; precipitation, solubility and solubility product; influence of ionic strength, pH and formation of complex species on solubility; distribution equilibria between two phases.
Books
The professor has made available all the teaching material (handouts and power point presentations) used during the course on e-learning platform (require password to the professor).
Recommended Books:
- - James W. Robinson, Eileen M. Skelly Frame, George M. Frame II. Chimica Analitica Strumentale_ Un’introduzione_ Piccin, 2023.
ISBN 978-88-299-3226-9
- Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009.
ISBN 9788879593427
Frequency
Attendance at classroom lessons is optional, but strongly recommended.
Attendance at laboratory exercises is mandatory.
Exam mode
To pass the exam, mark has to be not less than 18/30. The student must prove that he has acquired sufficient knowledge of both chromatographic and mass spectrometric techniques.
To achieve a score of 30/30 cum laude, the student must master all topics covered during the course, being able to link them in a logical and consistent way. Besides the global preparation level, the final mark will be formulated assessing the following elements: logic followed by the student in solving questions, technical language and oral presentation, adequacy of the proposed solution in relation to the skills acquired by the student at the end of the course.
Bibliography
References (.edu) are cited in the handouts uploaded on e-learning
Lesson mode
Teaching activity is organized in lectures, seminars, flipped teaching, laboratory exercises and preparation of reports. All teaching material (power point presentations, handouts, explanation sheets of laboratory exercises) used during the course by the teacher is immediately available by the student on the e-learning platform, especially to facilitate working students.