ANALYTICAL CHEMISTRY LABORATORY AND INSTRUMENTAL - MOD.2

The course of Instrumental Analytical Chemistry is part of the training activities characterizing the three-year degree course in Chemistry and Sustainable Technologies, and is aimed at providing students with the appropriate preparation to deal with a chemical problem in its various aspects and with the appropriate use of the current technical-scientific language.

The course is divided into two modules (defined Module 1 and Module 2), each of them divided into theory classes (held in the classroom) and laboratory lessons. Both modules have common training objectives listed below:

1. To provide knowledge of the general principles on which the instrumental analytical techniques most commonly used in chemical analysis laboratories are based.
2. To provide knowledge on the functioning of the instrumentation and on the modality of reading the responses obtained from the different types of instruments and their correlation with the relevant theoretical aspects
3. Develop critical mind that allows students to evaluate the potentials, advantages and limits of the different instrumental analytical techniques studied
4. Introduce the students to the conscious evaluation of the role of instrumental analytical methods in the specific area of quality control of a good
5. Develop skills in the evaluation and reliability of analytical data.
6. Develop manual skills and ability to conduct experiments autonomously, working both alone and in groups.
7. To develop the ability to apply an analytical method in coherence with protocols already defined and / or established by specific laws.
8. Develop skills in the collection, organization and processing of experimental data and the ability to present them in written and / or graphic form, using the appropriate scientific language.
9. Develop skills to critically interpret and evaluate the experimental results and verify their congruence with the theoretical laws that underlie the techniques used.

The expected results are defined according to the different contents of the two modules in which the Instrumental Analytical Chemistry course is divided.

Knowledge and understanding
A) Knowledge and understanding of the fundamental principles of separation instrumental analytical techniques and of the laws that govern them.
B) Knowledge and understanding of the elements that make up the instruments with which analytical measurements are performed by means of chromatographic and mass spectrometric techniques and combinations thereof.

2. Ability to apply knowledge and understanding
A) Ability to use the laws and knowledge learned to establish, from a theoretical point of view, the performance of the tools and the results expected from their use.
B) Knowing how to choose the most suitable instrumental apparatus to perform an analytical measurement on samples characterized by different degrees of complexity.

3. Ability to judge
A) Ability to evaluate the quality of the responses obtained from the different analytical instrumentation considered.
B) Knowing how to identify anomalous instrumental responses generated by the electronic and electrical components that constitute the considered instrumentation.

4. Communication skills
A) Knowing how to describe, both in written and oral form, the theoretical aspects treated using an appropriate language, scientifically correct and with consistent logic.
B) Knowing how to describe, in both written and oral form, the different parts that make up standard tools in relation to the analytical techniques considered.

5. Learning skills
Develop the ability to take notes identifying autonomously the salient aspects of the analytical techniques and methods based on the different instrumental analytical techniques considered.

To have achieved the training objectives of: Institution of mathematics 1 and 2; Physics 2, Analytical chemistry, General and inorganic chemistry, possibly (but not necessarily) having passed the examination of these teachings.

In order to achieve the training objectives and the expected learning outcomes, in relation to the theoretical part performed in the classroom, the contents developed in Module 2 are summarized as follows.

Introduction: General aspects of the course; exam methods; indications of texts and handouts on which to study.
General aspects of an analytical instrumental method: selective and specific analytical methods. Importance of separation analytical methods and Classification.
Solvent extraction methods. partition and distribution coefficient. Theory of extraction: batchwise single stage and multistage countercurrent extraction.
Chromatographic methods and solvent extraction: similarities and differences. Stationary phase and mobile phase. Chromatographic methods on the column and chromatogram.
Theoretical aspects of chromatography. Distribution coefficient; linear chromatography; average velocity of the molecules of the mobile phase and of the solute; retention time and dead time; capacity factor (or retention factor); selectivity; efficiency and number of theoretical plates. Theory of the theoretical plate and shape of the chromatographic peak; determination of efficiency in linear chromatography; kinetic theory and factors affecting the peak shape; van Deemter's equation. Resolution and its relationship with other chromatographic parameters. Optimization of a chromatographic procedure: effect of the capacity factor on retention time and resolution. Peak asymmetry: effect of isotherms in tailing and fronting phenomena; efficiency calculation in non-linear chromatography. Qualitative and quantitative analysis. Internal standard method.
Gas-chromatography. Classification: liquid (or breakdown) gas (GLC) and solid gas (GSC). GLC: Packaged and capillary chromatographic columns; supports for the stationary phase for packed columns; stationary phases and their choice on the basis of the characteristics of the solute; mobile phases and their characteristics. Typical applications. Effect of temperature on the elution of the analytes: isothermal and programmed temperature. GSC: stationary phases; typical applications. Injection systems: syringe and split-splitless injectors. Detectors: thermal conductivity; flame ionization; electronic capture. Derivatization methods.
High performance liquid chromatography (HPLC): General aspects of the technique: HPLC columns; mobile phases and isocratic and gradient elution; types of particles used as supports for stationary phases. Adsorption chromatography: types of stationary phases and mobile phases; solvent force elution mechanism; typical applications. Liquid-liquid chromatography: normal phase (or direct) inverse phase elution. Columns with bounded phases and methods of preparation. Choice of the stationary phase and mobile phase; polarity index. Reverse phase chromatography and solvophobic theory. Ion-pair chromatography. Ion-exchange chromatography: selectivity coefficient; selectivity scale; ion exchange chromatography with suppression. Size exclusion chromatography: distribution coefficient; calibration curve for the determination of molecular weights. Injection systems. Pumps. Detectors: photometric and spectrophotometric; refractive index; conductometric.
Mass Spectrometry: General aspects of the technique. Ionization sources systems: electron impact; chemical ionization; field ionization and field desorption; spark sources ionization. Mass analyzers: time of flight; single and double focusing magnetic deflection; quadrupole. Ion collectors. Resolution and mass spectra. Examples of spectra and modes of representation.
Brief outline of hyphenate methods: types of interfaces for GC-MS and HPLC-MS.

As support to the study, various texts of analytical instrumental Chemistry can be used at university level and in particular, the following texts are suggested:

- Skoog D.A., Holler F.J., Crouch S.R., Chimica Analitica Strumentale, EdiSES, Napoli, 2009.
- Skoog D.A. , Leary J.J, Chimica Analitica Strumentale, EdiSES, Napoli, 2000.
- Harris D.C., Chimica Analitica Quantitativa, seconda edizione, Zanichelli, Bologna, 2005.
- Rubinson K.A., Rubinson J.F., Chimica Analitica Strumentale, Zanichelli, Bologna, 2002.
- Skoog D.A., West D.M., Holler F.J., Crough S.R., Fondamenti di Chimica Analitica, EdiSES, Napoli, III ed. (2015), op. II Ed.(2005).

It is also advisable to check details by taking into account also of lecture notes and material supplied by the teacher.

The assessment of learning of the teaching activities is carried out through an oral test on the topics covered during the lectures. In particular, the exam consists of a series of open questions on the theoretical aspects of the techniques, the different instrumental parts that characterize each of the techniques studied, the classification of specific methods within the various techniques studied. The student will have to explain the various topics in a formally and scientifically correct language, demonstrating at the same time that he understood the link between the different aspects treated, as well as their differences. Depending on the ability to illustrate the required topics, the exam lasts between 45 to 60 minutes.


The final mark of the Instrumental Analytical Chemistry course is composed of the arithmetic mean between:
- vote of the written exam of Module 1;
- the oral examination of Module 2;
- laboratory mark (the mode of verification and evaluation of the experiences carried out in the laboratory is defined in the corresponding Syllabus of the laboratory teaching).

The different modality of verification of learning of the didactic activity, i.e. written for Module 1 and oral for Module 2, is consistent with the different development of the topics addressed: more quantitative / mathematical in Module 1 compared to Module 2. Furthermore, this choice is consistent with one of the expected results concerning the development of communication skills both in written and oral form.

Teaching will take place through lectures in which the theoretical principles concerning instrumental analytical techniques of chromatography, mass spectrometry will be presented. During the lessons examples of types of questions that could be posed to the students during the examination will be will also be made. Moreover texts / notes / handouts where better to study / deepen the topics covered will be suggested from time to time.

Italian

Accommodation and support services for students with disabilities and students with specific learning impairments:
Ca’ Foscari abides by Italian Law (Law 17/1999; Law 170/2010) regarding support services and accommodation available to students with disabilities. This includes students with mobility, visual, hearing and other disabilities (Law 17/1999), and specific learning impairments (Law 170/2010). In the case of disability or impairment that requires accommodations (i.e., alternate testing, readers, note takers or interpreters) please contact the Disability and Accessibility Offices in Student Services: disabilita@unive.it

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