Analytical techniques for characterizing compounds of synthetic or natural origin.

This à la carte module enables students to deepen their skills in molecular and macromolecular synthesis chemistry. It also enables them to acquire the skills needed to characterize (macro)molecules. The theoretical aspects of this module will be complemented by practical experience.
This module will be useful, on the one hand, for students wishing to pursue careers in fields linked to molecular and polymer chemistry (drugs, (bio)plastics, biotechnologies etc.) and, on the other hand, for those attracted by analytical and characterization techniques. Here, these techniques will be used to characterize synthetic compounds, but they are commonly used to characterize natural molecules (peptides, proteins, lipids, molecules extracted from plants, etc.) and in the agri-food industry (quality control, fraud control, etc.)
This module is recommended for students wishing to take the S8 module "Chemistry applied to health" and the LAI specialization. It is compulsory for students wishing to follow the CBI specialization.

On completion of this module, students should be able to:

- describe the fundamentals of NMR
- give and explain the schematic diagram of an NMR experiment
- determine a molecular structure from 1D 1H and 13C spectra of simple organic molecules.
- identify 15N NMR signals from proteins
- describe the basic components of an NMR spectrometer
- set up a simple liquid-phase NMR experiment: sampling, type of experiments to be carried out
- know the limits and potential of a mass spectrometer so as to be able to make a choice of instrument depending on the molecule studied
- determine the mode of sample introduction, direct or by coupling, depending on the problem
- know how to interpret a mass spectrum
- know the principles of the IRMS technique: Isotopic Ratio Masse Spectrometry
- understand the applications of this technique in the agri-food sector
- critically analyze a research article on physico-chemical analysis in the agri-food sector (measurement principle, experimental limits, reliability, precision, application potential).

At the end of the course, students will have a basic knowledge of polymer synthesis, polymerization processes and characterization of polymer materials. They will be able to identify the reactivity of different monomers, synthesize polymers and apply appropriate techniques to characterize them.

- Atomistics - Spectroscopy from S6 - Reactivity course from the CHIAP in-depth chemistry module - Structure and general properties of polymers course from S5 (SPPOL).

Part I: Analysis and characterization techniques 17.33h

Nuclear magnetic resonance spectroscopy: 8h (4CM + 2TD) Fernando Leal Calderon
1. Introduction: NMR spectroscopy (nuclear spin, spin magnetic moment, energy levels, gyromagnetic ratio)
2. Principle of NMR (static, rotating magnetic field, nuclear magnetization)
3. 1D liquid-phase NMR (1H, 13C), chemical shift, NMR signal pattern.
4. NMR applications for molecular structure determination
5. Application of NMR to food analysis

Mass spectroscopy: 6.66h (2CM + 3TD) Corinne Buré
1. Apparatus: description/mechanisms/technical limitations (generalities, ionization process and different sources, analyzers, detectors)
2. Analysis (raw formula/unsaturation, ion charge state, tandem mass spectrometry, fragmentation processes, sample introduction, analysis strategy, practical advice)
3. Application examples.

Assessment: 1h30 written exam common to both courses at the end of the module
(course MCQ + determination of a molecular structure from various spectra (IR, 1H, 13C, mass)).

IRMS mass spectroscopy: 2.66h (1CM + 1TD) Fernando Leal Calderon
1. Presentation of the IRMS technique
2. Applications of the technique in the food industry: traceability, authenticity control, fraud control, quality control.
3. Case study: analysis of a scientific article in English
4. Oral presentation of the article in English and discussion with the teacher

Assessment: Oral presentation (10 min)

Part II: From (macro)molecular synthesis to characterization 32.66 h

Synthesis of compounds of interest and characterization on a molecular scale 10h
A) Preparation of organic chemistry practical work from data provided to students 1.33h (autonomous, Sandra Pinet)
- Choice of synthesis
- Choice of analytical methods to monitor the reaction
- Choice of characterization methods to be used

B) Organic chemistry laboratory work 8.66h (Sandra Pinet, Yohann Nicolas)
- Synthesis of a plasticizer from a bio-based compound
- Isolation of the product of interest
- Analysis and characterization (IR, NMR, etc.).) 

C) Macromolecular synthesis and characterization 22,66h (5CM: Audrey Llevot / 12h TP: Audrey Llevot, Stéphane Carlotti + 4h preparation-Restitution-Evaluation of skills: Audrey Llevot, and Sandra Pinet)
- Polymerization methodologies : step-by-step polymerization, chain polymerization
- Polymerization processes: emulsion, suspension, mass
- Thermo-mechanical characterizations

Evaluation: CR (1 sheet: interpretation of main results) + oral presentation on a given topic.

References:

* Mass Spectrometry. Principles and Applications, E. De Hoffmann, J. Charrette, V. Stroobant, Masson Editeur, Paris, 1996. ISBN 2-225-85252-9
* H Prépa. Chimie organique, 2e année PC-PC*, A. Durupthy, D. Cauchy, C. Foures, C. Mesnil, T. Zobiri, Ed. Hachette, Paris, 1997.
* Chimie-Physique (2nd Edition), P. Atkins, J. De Paula, De Boeck Editeur, Bruxelles, 2004. ISBN: 2- 8041-4539-5
* La RMN. Concepts, methods and applications, 2nd edition, D. Canet, J.C. Boubel, E. Canet-Soulas, Ed. Dunod, Paris, 2002.
* Actualité Chimique N°364-365. NMR in chemistry.
* Structural Biology. Practical NMR Applications, 2nd edition, Q. Teng, Ed. Springer, , New York, 2013.
* Chimie et Physico-Chimie des Polymères, , M. Fontanille and Y. Gnanou, Ed. Dunod 2002.
* Polymer synthesis, P. Rempp and E.W. Merrill, Huetig and Wepf Verlag, Basel-New York-Heidelberg, 1986 ISBN 3-85739-116-2.
* Textbook of Polymer Science, F.W. Billmeyer, John Wiley et sons, 1984 ISBN 0-471-82835-3.