Analytical Chemistry III

Course objectives

The educational objectives that this course intends to achieve include: - Learning of the problems related to the sampling and extraction techniques preliminary to liquid chromatography. - Understanding of the fundamentals of the main instrumental techniques (chromatographic, spectrophotometric and electrochemical). - Revision and improvement of the knowledge about the key parameters necessary for the validation of an analytical method. After completing the course, organized in lectures followed by practical lab exercises, students will be able to: - organize the development and validation of an analytical method for trace analysis in different types of real matrices, planning the extraction procedure, chromatographic separation and detection; - carry on a quantitative analysis and statistical treatment of results. - interpret UV-Vis and MS spectra.

Channel 1
ALESSANDRA GENTILI Lecturers' profile

Program - Frequency - Exams

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.
Channel 2
FRANCESCA BUIARELLI Lecturers' profile

Program - Frequency - Exams

Course program
The instrumental measurement through separative techniques 3 frontal credits and 1 laboratory credit. 1. extraction techniques. Principles of liquid-liquid extraction. Solvent extraction, Solid-liquid extraction, Soxhlet; Accelerated solvent extraction (ASE; Accelerated Solvent Extraction); 2. Introduction to instrumental analysis methods: Classification of instrumental analytical techniques. 3 Chromatographic techniques. - Fundamental principles. Distribution coefficient; capacity factor; column efficiency; symmetry parameter; van Deemter equation; selectivity; sample capacity; resolution. - Gas chromatography. Instrumentation; types of columns and stationary phases; detectors (flame ionization, thermal conductivity, electron capture, thermionic, atomic emission, flame photometry, MS). - Liquid chromatography. Main chromatographic techniques (adsorption chromatography, liquid-liquid partition chromatography, size exclusion, ion exchange). Instrumentation for HPLC (High performance Liquid Chromatography). Elution in isocratic and elution gradient. Detectors (UV / Vis, fluorescence, refractive index, MS). Spectroscopic methods Atomic and molecular absorption spectroscopy (IR, UV, Vis, Fluorescence) Atomic Emission Spectroscopy (UV Fluorescence XRF) ICP-MS notes on electrochemical methods
Prerequisites
The course "ANALYTICAL CHEMISTRY III WITH LABORATORY" is included in the course of three-year degree in Chemical Sciences, in the third year. The necessary knowledge, acquired in the first two years of the course, is provided by the basic teachings of Chemistry, Organic Chemistry, Physical Chemistry and Analytical Chemistry with particular regard to the teachings of Analytical Chemistry I and Analytical Chemistry II (qualitative and quantitative analysis).
Books
- On the e-learning platform, the teacher makes available the course handouts, supplementary material and support material to the lab experiences. - Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009 (Dept Chemistry library) -R. Cozzi, P. Protti, T Ruaro, Analisi Chimica Strumentale volume C Metodi cromatografici, Zanichelli - J W Robinson, E M Skelly Frame, G M Frame IIInstrumental Analytical Chemistry, An Introduction CRC Press
Teaching mode
The 4 credits of Analytical Chemistry III with laboratory are divided into 3 credits of frontal teaching, equal to 24 hours, and a credit of laboratory exercises, equal to 12 hours. Frontal lessons Section I (4 hours): Principles and theory of the science of separations and chromatography Section II (16 hours)): Separative Techniques + Diagram of the instruments Section III (4 hours)): Qualitative / quantitative analysis and applications In addition, Laboratory exercises in HPLC-UV and GC-FID (12h)
Frequency
Attendance is useful, not mandatory, but free. Students are invited to participate and take an active part in the lessons. In order to make the content more comprehensible, slides are projected. Attendance at least to didactic experiences is strongly recommended
Exam mode
The exam test aims to verify the level of knowledge and in-depth study of the topics of the teaching program and the reasoning ability developed by the student. The evaluation is expressed in thirtieths (minimum mark 18/30, maximum mark 30/30 with honors). The assessment consists of an oral test (questions on different parts of the program). The exam allows to verify the achievement of the objectives in terms of knowledge and skills acquired as well as communication skills. Very important is the property of language, the clarity of exposition and the critical ability shown for the resolution of real analytical problems.
Lesson mode
The 3 credits of Analytical Chemistry III with laboratory are of frontal teaching, equal to 24 hours, Frontal lessons Section I (4 hours): Principles and theory of the science of separations and chromatography Section II (16 hours): Separative Techniques + Diagram of the instruments and qualitative / quantitative analysis Section III (4 hours): spectroscopic techniques
MANUEL SERGI Lecturers' profile

Program - Frequency - Exams

Course program
1. Introduction to Analytical Chemistry, principles and definitions. Analytical data and statistical analysis. 2. Sample treatment and the main extraction techniques 3. The main analytical techniques: spectroscopy and related techniques (molecular and atomic); potentiometry. 4. Separative techniques: chromatography and detectors.
Prerequisites
The knowledge related to General Chemistry, Organic Chemistry and Analytical Chemistry I and II course
Books
- Skoog, West, Holler,Crouch, Fondamenti di Chimica Analitica, EdiSES - Robinson, Skelly, Frame, Chimica Analitica Strumentale, Piccin
Frequency
Attendance in this course is not mandatory, but strongly suggested especially for Lab experiences
Exam mode
Interview and discussion on Lab experiences
Lesson mode
Classroom lessons and Laboratory experiences
Channel 3
MANUEL SERGI Lecturers' profile

Program - Frequency - Exams

Course program
1. Introduction to Analytical Chemistry, principles and definitions. Analytical data and statistical analysis. 2. Sample treatment and the main extraction techniques 3. The main analytical techniques: spectroscopy and related techniques (molecular and atomic); potentiometry. 4. Separative techniques: chromatography and detectors.
Prerequisites
The knowledge related to General Chemistry, Organic Chemistry and Analytical Chemistry I and II course
Books
- Skoog, West, Holler,Crouch, Fondamenti di Chimica Analitica, EdiSES - Robinson, Skelly, Frame, Chimica Analitica Strumentale, Piccin
Frequency
Attendance in this course is not mandatory, but strongly suggested especially for Lab experiences
Exam mode
Interview and discussion on Lab experiences
Lesson mode
Classroom lessons and Laboratory experiences
  • Lesson code10596341
  • Academic year2024/2025
  • CourseChemical Sciences
  • CurriculumSingle curriculum
  • Year3rd year
  • Semester2nd semester
  • SSDCHIM/01
  • CFU6
  • Subject areaDiscipline chimiche analitiche e ambientali