In accordance with the specific aim of the course, this teaching will provide the students with: i) the knowledge and skills of "problem solving" related to the quantitative determination of different analytes in complex matrices; ii) the analytical skills needed to design and carry out instrumental analyses on different matrices and analytes, as well as the presentation of the analytical results.

a) conoscenze e capacit di comprensione nel settore della chimica analitica strumentale con particolare riferimento alle tecniche di preparazione del campione, ai principi di funzionamento e alla fenomenologia fisica delle principali moderne tecniche strumentali di cromatografia e di spettroscopia atomica diffuse nei laboratori di analisi, agli approcci metodologici per l'analisi quantitiva, all'elaborazione statistica dei dati sperimentali e alla presentazione dei risultati in accordo con le regole della metrologia chimica.

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b) capacit di applicare conoscenza e comprensione coniugando aspetti teorici con prassi e metodologie sperimentali, permettendo l'applicazione pratica del sapere acquisito nell'ambito della chimica analitica strumentale al fine di affrontare e risolvere tutte le problematiche direttamente o indirettamente collegate ad esso.

c) autonomia di giudizio e sviluppo dell'apprendimento critico perseguito attraverso l'interazione tra docenti e studenti in virt del bilanciamento delle attivit formative a carattere teorico e quelle a carattere pratico-sperimentale svolte durante il laboratorio didattico.

d) abilit comunicative basate sulla capacit di comunicare le conoscenze acquisite attraverso l'individuazione di soluzioni a problematiche inerenti l'analisi chimica strumentale e l'esposizione chiara e comprensibile di valutazioni e motivazioni a interlocutori specialisti e non specialisti, derivate dall'adeguata conoscenza delle tematiche oggetto della comunicazione, sviluppate attraverso il confronto e l'interazione docente-studente.

a) Knowledge and understanding skills in instrumental analytical chemistry with specific reference to sample preparation techniques, to the operating principles and physical phenomena of the main modern instrumental chromatographic and atomic spectroscopy techniques used in analytical laboratories, to the methodological approaches to quantitative analysis, to the statistical processing of experimental data and presentation of results in accordance with the rules of the chemical metrology.

b) Ability to apply knowledge and understanding by combining theoretical aspects with experimental practices and methodologies, allowing practical application of acquired knowledge in instrumental analytical chemistry in order to address and solve all issues directly or indirectly related to it.

c) Autonomy of judgment and development of critical learning pursued through interaction between teachers and students and by balancing the theoretical and practical activities carried out during the laboratory.

d) Communication skills based on the ability to communicate the acquired knowledge through the identification of solutions to issues related to instrumental chemical analysis and the clear and understandable exposure of assessments and motivations to specialists and non specialists, derived from the adequate knowledge of the subjects developed by teacher-student interaction.

Metodi di taratura: calibrazione esterna, con standard interno e mediante il metodo delle aggiunte standard. Limite di Rivelabilit e di Quantificazione. Intervallo Dinamico Lineare. Incertezza del dato.

Cromatografia: il processo di eluizione cromatografica e le propriet dei picchi cromatografici: risoluzione, selettivit, fattore di capacit, efficienza. La teoria cinetica della cromatografia, principi di fluidodinamica ed equazione di Van Deemter. Gascromatografia (GC): colonne e fasi stazionarie, parametri di flusso e fast-GC, indici di Kovats e costanti di McReynolds. Iniettori per GC. Rivelatori per GC: FID, PID, ECD, a termoconducibilit, spettrometria di massa. Cromatografia liquida (LC): pompe, iniettori, colonne, fasi stazionarie e mobili, gradienti binari e ternari. Rivelatori per LC: spettrofotometrico, spettrofluorimetrico, a indice di rifrazione, elettrochimico. Cromatografia ionica: principi di separazione e rivelazione conduttimetrica. Cromatografia chirale, di coppia ionica, di esclusione dimensionale e ionica: principi, fasi stazionarie ed eluenti, applicazioni.

L'attivit di laboratorio organizzata in gruppi di lavoro che svolgono diverse tipologie di analisi quantitative su campioni complessi. Le esperienze sono descritte in procedure fornite agli studenti in forma di dispense e prevedono lo svolgimento completo di un'analisi dal trattamento del campione, alla misura sperimentale e all'elaborazione dei dati in forma di relazione. La tipologia di esperienze di seguito descritta: 1) determinazione di anioni inorganici in acque minerali commerciali mediante cromatografia ionica; 2) determinazione del contenuto dei metalli in matrici complesse (alimentari e ambientali) mediante AAS e ICP-OES; 3) identificazione dei metalli presenti in campioni solidi di varia natura mediante LIBS; 4) estrazione e determinazione di micronutrienti e contaminanti in alimenti mediante spettrofotofluorimetria e HPLC; 5) estrazione di plastificanti da materie plastiche e loro determinazione mediante GC/MS.

The teaching will outline theoretical principles and the experimental use of the main instruments present in the modern chemical laboratory. The used teaching methodology includes: (1) the description of physical chemical principles and the features of the analytical instrumentation with reference to the type of samples to be analyzed; (2) the analysis of a real analytical problem (case of study) and the identification of strategies for its resolution by choosing the appropriate methodological approach in terms of sampling, sample preparation, analysis and processing of results.

Main topics are showed below.

The stages of the chemical analysis instrument: from sampling to measurement of an instrument signal, until the presentation of the analytical result.

Sample preparation for analysis: attack and acid dissolution of samples for elemental analysis. Methods of extraction, clean-up and separation for compositional analysis. Liquid-liquid extraction: quanitative relations, extraction of metal ions, extraction of ion association complexes, extraction by Soxhlet; accelerated solvent extraction, supercritical fluid extraction, microwave assisted extraction. Solid Phase Extraction.

Inorganic elemental analysis: atomic absorption spectroscopy, atomic emission spectroscopy and fluorescence equipment (optical materials, sources, wavelength selectors, detectors). Effect of bandwidth and the slit on the measures. Atomization systems: flame, graphite furnace, plasma. Fields of application, limits, yields, interferences and measurement strategies. Memory effect; method hydride and cold vapor. Techniques for background correction. Nebulization systems. Applications and comparison of spectroscopic techniques.

Chromatography: application of equilibrium distribution of gas-liquid and liquid-liquid. The chromatographic elution process and the properties of the chromatographic peaks: resolution, selectivity, capacity factor and efficiency. The kinetic theory of chromatography, principles of fluid dynamics and the Van Deemter equation. Gas chromatography (GC) columns and stationary phases, flow parameters and fast-GC, Kovats indices and McReynolds constants. Injector for GC. GC detectors: FID, PID, ECD, thermal conductivity, mass spectrometry. Derivatization reactions. Liquid chromatography (LC): pumps, injectors, columns, stationary and mobile phases, binary and ternary gradients. Detection in HPLC: spectrophotometric, spectrofluorometric, refractive index, electrochemical detectors. Derivatization reactions. Ion chromatography: principles of separation and conductivity detection. Chiral chromatography, ion pairing, size exclusion and ion: Principles, stationary phases and eluents, applications.

The lab activity is organized in working groups that will perform various types of quantitative analysis on complex samples. The experimental procedures are described in details and will be provided to students. The students are required to complete the whole procedure of analysis including proper sample handling, experimental measurements, and data processing. The type of experience is described below: 1) Determination of inorganic anions in commercial mineral waters by ion chromatography; 2) determination of the metal content in complex matrices (food and environmental) by AAS and ICP-OES; 3) identification of metals present in different solid samples through LIBS; 4) extraction and determination of micronutrients and food contaminants by spectrophotometry and HPLC; 5) extraction of plastics plasticizers and their determination by GC / MS.

For each experience, the work group is required to process the experimental data according to statistical tools showed during classroom lessons and that will be evaluated by the teachers.

A) Lectures (7 CFU) - The examination is divided in two exemptions relating to Module 1 (Elemental analysis - 5 CFU) and Module 2 (Chromatographic techiniques - 2 CFU). Each exemption is normally carried out as a written exam with 4-5 questions, each covering a topic of the program, plus 1-2 numerical exercises relating to statistical processing and evaluation of the uncertainty of the analytical result and/or the calculation of the parameters of interest for chromatographic techiniques. Both the understanding of the topics and the ability to connect the interdisciplinary subjects will be evaluated.

La chimica analitica strumentale, o semplicemente chimica strumentale, una branca della chimica analitica che indaga gli analiti utilizzando strumenti scientifici. Rientrano in questo campo la spettrofotometria, la spettrometria di massa, la cromatografia, l'elettroforesi, la potenziometria, la voltammetria. 152ee80cbc

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