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ANALYTICAL CHEMISTRY II + LABORATORY OF ANALITYCAL CHEMISTRY II

Academic year and teacher
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Versione italiana
Academic year
2022/2023
Teacher
MARIA CHIARA PIETROGRANDE
Credits
12
Didactic period
Secondo Semestre
SSD
CHIM/01

Training objectives

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Modulo: 016801/1 - CHIMICA ANALITICA II
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The main goal of the course is to provide students a background knowledge on the more common analytical techniques fundamental to set up qualitative and quantitative analysis according to standard procedures.
The main knowledge that wil be acquired with the module of Analytical Chemistry II will be:
- basic aspects and common applications of the mosre important instrumental analytical technqiues, with particular focus on separation science and kinetic methods;
- different steps of analytical methods and their characteristics: sampling, purification, clean-up, analysis, data processing;
- issues about handling of real samples, such as complex environmental, industrial, biological matrixes.
During the module of Laboratory of Analytical Chemistry II, students will acquire:
- knowledge on main electrochemical, spectroscopic and chromatographic techniques;
- ability on electroanalytical, spectroscopic and chromatographic instruments;
- competence on the choice of the optimal analytical method;
- competence on the evaluation of experimental data and their processing.

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Modulo: 016801/2 - LABORATORIO DI CHIMICA ANALITICA II
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The main goal of the course is to provide students a background knowledge on the more common analytical techniques fundamental to set up qualitative and quantitative analysis according to standard procedures.
The main knowledge that wil be acquired with the module of Analytical Chemistry II will be:
- basic aspects and common applications of the mosre important instrumental analytical technqiues, with particular focus on separation science and kinetic methods;
- different steps of analytical methods and their characteristics: sampling, purification, clean-up, analysis, data processing;
- issues about handling of real samples, such as complex environmental, industrial, biological matrixes.
During the module of Laboratory of Analytical Chemistry II, students will acquire:
- knowledge on main electrochemical, spectroscopic and chromatographic techniques;
- ability on electroanalytical, spectroscopic and chromatographic instruments;
- competence on the choice of the optimal analytical method;
- competence on the evaluation of experimental data and their processing.

Prerequisites

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Modulo: 016801/1 - CHIMICA ANALITICA II
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Students should already have acquired fundamental knowledge on volumetric analysis and on characteristics and requisites of quantitative and qualitative analysis methods. These notions are provided in the course of Analytical Chemistry I and Laboratory of Analytical Chemistry I.

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Modulo: 016801/2 - LABORATORIO DI CHIMICA ANALITICA II
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Students should already have acquired fundamental knowledge on volumetric analysis and on characteristics and requisites of quantitative and qualitative analysis methods. These notions are provided in the course of Analytical Chemistry I and Laboratory of Analytical Chemistry I.

Course programme

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Modulo: 016801/1 - CHIMICA ANALITICA II
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The course is made up of two parts: the module of Analytical Chemistry II (48 hours of frontal lessons and exercises) and the module of Laboratory of Analytical Chemistry II (16 hours of frontal analysis and 48 hours of lab activities).

Module of Analytical Chemistry II:

- Kinetic methods: basic principles and characteristics of quantitative methods based on the measurement of reaction velocity; enzymatic methods for the determination of enzymes and substrates; quantification of enzymes as markers; main characteristics and application in biological and environmental.

- Separation techniques and their use for chemical analysis:

theoretical principles of chromatography:
thermodynamic aspects: chemical equilibria and parameters driving retention and; kinetic aspects: efficiency, Van Deemter equation, chromatographic resolution and choice of the best instrumental parameters to optimize it; calculation of the principal chromatographic parameters from an experimental chromatogram.

Gas-chromatography (GC): separation mechanisms; characteristics of packed and capillary columns; Golay equation; basic information on GC instrumentation.

Liquid chromatography (LC): retention mechanisms in LC; normal phase and reversed-phase LC; planar (TLC) and column liquid chromatography (HPLC); basic characteristics of columns and instrumentation; separations under gradient elution conditions.

Brief mention about ion chromatography, size exclusion chromatography and electrophoresis.

- Principal steps of analytical methods: sampling, pre-treatment, purification, analysis, data processing. Analytical methods for the purification of samples: liquid-liquid extraction, solid-phase extraction (SPE), liquid-liquid extraction, extraction with solvents.

- Basic principles for the choice and optimization of the best analytical method: theoretical aspects and examples of application to complex environmental, industrial and biological samples.

Module of Laboratory of Analytical Chemistry II:

Frontal lessons will be about:
- Redox equilibria, Nernst equation, direct potentiometry and titration by potentiometry, ion-selective electrodes, potenziometric analysis methods. Conductance: principles, instrumentation and application. Direct methods and titrations-
- Calibration: external standard method, internal standard method, standard additions method. Dynamic range and linear dynamic range, selectivity, sensitivity e limit of detection.
- Electrogravimetric with or without potential control. Coulometric titrations (2 h).
- Spectroscopic methods: properties of electromagnetic radiations. UV-Vis spectroscopy. Molecular absorption spectroscopy: principles, instrumentation, Lambert-Beer law and its limitations, spectroscopic analysis methods.
- Atomic absorption and emission spectroscopy: principles, instrumentation and analytical methods. Atomizers: flame emission and atomic absorption, graphite furnace atomizer, atomic emission spectrometry with plasma.

Practical lab activities will be on:
- Direct potentiometry and titrations, direct conductance and titrations, ion-selective electrodes, couometric titrations, electrogravimetric analysis;
- Gas-chromatography (GC) and high-performance liquid chromatography (HPLC);
- UV-Vis spectroscopy;
- Atomic spectroscopy (flame, graphite furnace atomizer and plasma).
Calibrations will be done according to different methodologies (external standard method, internal standard method, standard additions method).
Lab experiences are done on environmental, industrial, food and pharma samples. Students will work in in groups in order to increase their capacity to work in a team. Data processing will be done on Excel sheets provided by the teachers.

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Modulo: 016801/2 - LABORATORIO DI CHIMICA ANALITICA II
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The course is made up of two parts: the module of Analytical Chemistry II (48 hours of frontal lessons and exercises) and the module of Laboratory of Analytical Chemistry II (16 hours of frontal analysis and 48 hours of lab activities).


Module of Analytical Chemistry II:
- kinetic methods: basic principles and characteristics of quantitative methods based on the measurement of reaction velocity; enzymatic methods for the determination of enzymes and substrates; quantification of enzymes as markers; main characteristics and application in biological and environmental field (4 hours);
- separation techniques and their use for chemical analysis: theoretical principles of chromatography; thermodynamic (retention and selectivity) and kinetic (efficiency) aspects. Exercises on the calculation of the principal chromatographic parameters from an experimental chromatogram. Commonly used detectors in chromatography. Qualitative and quantitative chromatographic analysis (10 hours).
Gas-chromatography (GC): separation mechanisms; characteristics of columns and instrumentation; separations under temperature gradient conditions (7 hours);
Liquid chromatography (LC): retention mechanisms in LC; normal phase and reversed-phase LC; characteristics of columns and instrumentation; separations under gradient elution conditions. Brief mention about ion chromatography and size exclusion chromatography. Examples of separations (9 hours).
- Principal steps of analytical methods: sampling, pre-treatment, purification, analysis, data processing. Analytical methods for the purification of samples: solid-liquid extraction, solid-phase extraction (SPE), liquid-liquid extraction, extraction with solvents (10 hours).
- Sensors for chemical analysis: operating principles of chemical sensors; electrochemical sensors: amperometric, conductimetric, potenziometric sensors; optical sensors; applications (4 hours).
- How to choose and optimize and analytical method: theoretical aspects and examples of application to complex environmental, industrial and biological samples (4 hours).
.

Module of Laboratory of Analytical Chemistry II:
Frontal lessons will be about:
- Redox equilibria, Nernst equation, direct potentiometry and titration by potentiometry, ion-selective electrodes, potenziometric analysis methods. Conductance: principles, instrumentation and application. Direct methods and titrations (6 h).
- Calibration: external standard method, internal standard method, standard additions method. Dynamic range and linear dynamic range, selectivity, sensitivity e limit of detection (2 h).
- Electrogravimetric with or without potential control. Coulometric titrations (2 h).
- Spectroscopic methods: properties of electromagnetic radiations. UV-Vis spectroscopy. Molecular absorption spectroscopy: principles, instrumentation, Lambert-Beer law and its limitations, spectroscopic analysis methods (2 h).
- Atomic absorption and emission spectroscopy: principles, instrumentation and analytical methods. Atomizers: flame emission and atomic absorption, graphite furnace atomizer, atomic emission spectrometry with plasma (4 h).

Practical lab activities will be on:
- Direct potentiometry and titrations, direct conductance and titrations, ion-selective electrodes, couometric titrations, electrogravimetric analysis;
- Gas-chromatography (GC) and high-performance liquid chromatography (HPLC);
- UV-Vis spectroscopy;
- Atomic spectroscopy (flame, graphite furnace atomizer and plasma).
Calibrations will be done according to different methodologies (external standard method, internal standard method, standard additions method).
Lab experiences are done on environmental, industrial, food and pharma samples. Students will work in in groups in order to increase their capacity to work in a team. Data processing will be done on Excel sheets provided by the teachers.

Didactic methods

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Modulo: 016801/1 - CHIMICA ANALITICA II
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Theoretical/practical lessons.
Theoretical lessons will be held in classroom with the support of PowerPoint slides. Some lessons will be devoted to numerical exercitation concerning numerical problems on some topics.
Blackboard is used for the lesson of the Laboratory part.

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Modulo: 016801/2 - LABORATORIO DI CHIMICA ANALITICA II
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Theoretical/practical lessons.
Theoretical lessons will be held in classroom with the support of PowerPoint slides. Some lessons will be devoted to numerical exercitation concerning numerical problems on some topics.
Blackboard is used for the lesson of the Laboratory part.

Learning assessment procedures

Scope of the exam is to verify the knowledge of students on the main concepts of the course and their ability to apply them to analysis of real samples.

Module of Analytical Chemistry II
Written exam with open questions and numerical exercises:
- 14 open questions on specific arguments: short answer (max 5 lines)
- 2 open questions on general arguments: long answer (max 1 page)
- 2 numerical exercises

Module of Laboratory of Analytical Chemistry II
The evaluation of this module is made on the base of two different parts:
1) Written exam (which have a weight of 70% on the final evaluation of the Laboratory module) with 7 open questions:
- 5 open questions on specific arguments: short answer (max 5 lines)
- 2 open questions on general arguments: long answer (max 1 page).
2) Evaluation of the reports on lab experiments (one for each experiment) which will have a weight of 30% on the final evaluation of the Laboratory module). The evaluation will be based also on the conduct of the student during lab activities.

The overall result of the course of Analytical Chemistry II and Laboratory of Analytical Chemisrty II is collaboratively defined by the teachers on the basis of scores obtained in the two modules.

Reference texts

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Modulo: 016801/1 - CHIMICA ANALITICA II
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The reference textbook is:
D.A. Skoog, D.W. West, F.J. Holler, S.R.Crouch,
Fundamentals of Analytical Chemistry,
2014, 9th edition
Brooks/Cole, Cengage Learning.

The teachers provide the slides used for the classroom lessons.

The teachers provide the slides used for the classroom lessons.




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Modulo: 016801/2 - LABORATORIO DI CHIMICA ANALITICA II
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The reference textbook is:
D.A. Skoog, D.W. West, F.J. Holler, S.R.Crouch,
Fundamentals of Analytical Chemistry,
2014, 9th edition
Brooks/Cole, Cengage Learning.

The teachers provide the slides used for the classroom lessons.

The teachers provide the slides used for the classroom lessons.