IDENTIFYING DATA

2020_21

Subject (*)

STRUCTURAL DETERMINATION TECHNIQUES

Code

13685102

Study programme

Synthesis, Catalysis and Molecular Design (2013)

Cycle

2nd

Descriptors

Credits

Type

Year

Period

Compulsory

First

Language

Anglès

Department

Analytical Chemistry and Organic Chemistry
Physical and Inorganic Chemistry

Coordinator

GODARD , CYRIL

E-mail

cyril.godard@urv.cat
noemi.cabello@urv.cat

Lecturers

GODARD , CYRIL

CABELLO SÁNCHEZ, NOEMÍ

Web

General description and relevant information

Learning the new techniques of Nuclear magnetic Ressonance and Mass Spectrometry and their applicaiton in the structural elucidation of structures and characterization of molecular compounds.

Competences

Type A	Code	Competences Specific
		Common
	AC1	CE1-Make correct use of modern techniques for characterizing chemical compounds.
	AC3	CE3-Correctly apply the most advanced methodologies in synthesis and catalysis.
	AC6	CE6-Have a fluent command of the specialized terminology in English related to the fields of synthesis, catalysis and molecular design.
	AC8	CE8-Design synthesis routes for new products using modern techniques of chemical synthesis, chemical and physical structural characterization, high performance experimentation, data analysis and computational chemistry.
Type B	Code	Competences Transversal
		Common
	BC1	CT1- Become sufficiently independent to work on research projects and scientific or technological collaborations within their thematic area
	BC3	CT3-Solve complex problems critically, creatively and innovatively in multidisciplinary contexts
	BC7	CT7-Apply ethical principles and social responsibility as a citizen and a professional
Type C	Code	Competences Nuclear

Learning aims

Objectives	Competences
	AC1 AC3 AC6 AC8	BC1 BC3 BC7
Understanding the instrumental aspects and advanced applications of mass spectrometry.
Understanding the physical principles and the instrumental aspects of pulsed nuclear magnetic resonance and its application to the resolution of complex structures.
Evaluating and obtaining the information that can be provided by using mass spectrometry with other techniques.
Combining mass spectrometry with other techniques to determine structures and to solve chemical problems.
Description of the NMR spectral parameters. Effects of the molecular symmetry of the spectral parameters.
Applying different experiments of pulsed NMR and two-dimensional resonance to the characterization of molecular compounds.
Interpreting the results obtained by characterizing samples with different characteristics.
Choosing the correct characterization techniques for obtaining the desired information.
Critically evaluating information and incorporating it into the knowledge base.

Contents

Topic	Sub-topic
MASS SPECTROMETRY
1. Introduction. Definitions. High resolution, low resolution.
2. Ionization methods.	2.1.- Electron Ionization. Fundamentals. Mechanisms, fragmentations. 2.2. Chemical ionization. Fundamentals. Examples. 2.3. FAB, SIMS, MALDI. Fundamentals. Examples. 2.4. Atmospheric Pressure Ionization (API) techniques. ESI and APCI: Fundamentals. Description.
3.- Instrumentation	3.1.- Analyzers: Quadrupole, Magnetic Sector, Ion Trap, Time of flight (TOF), Fourier Transform Ion Ciclotron Resonance (FT-ICR). 3.1.1.- Mass Spectrometry in tandem: MS/MS, MSn. 3.2.- Detectors: Faraday Cup, Multichannel plate…
4.- Hyphenated Methods: GC-MS, LC-MS
MAGNETIC NUCLEAR RESONANCE
5. Presentation. Aims. Bibliography.
6. Theoretical basis of NMR. The nucleus in a magnetic field. Vector model. Pulses. Relaxation.
7. Pulse Experiments. Spectra in the time domain and frequency domain. Operators.
8. Instrumental aspects. Acquisition and processing of spectra.
9. Spectral parameters in NMR: Magnetic symmetry and equivalence. Second order effects. Simulation programmes. Exchange processes and dynamical systems.
10. Spectral modifications: Shift reagents. Spin uncoupling. Nuclear Overhauser effect.
11. Multiple pulse experiments.
12. Bidimensional resonance experiments.
13. Other experiments in NMR.
14. Practical cases and problem solving.

Planning

Methodologies :: Tests

Competences

(*) Class hours

Hours outside the classroom

(**) Total hours

Introductory activities

Lecture

Seminars

Presentations / oral communications

Personal attention

Mixed tests

(*) On e-learning, hours of virtual attendance of the teacher.
(**) The information in the planning table is for guidance only and does not take into account the heterogeneity of the students.

Methodologies

Methodologies

	Description
Introductory activities	To introduce the subject.
Lecture	Description of the contents of the subject.
Seminars	In-depth work on a particular topic. Further discussion of the lecture content, which is linked to professional skills. Application to practical cases.
Presentations / oral communications	Oral presentation by students of a particular issue or case studies (previously presented in writing).
Personal attention	Time that each teacher has to speak to pupils and resolve their doubts.

Personalized attention

Personal attention

Description

Time that each professor has to speak to students and solve their doubts. Students can contact either by e-mail or in their offices. In the latter case, appointments have to be made.

Dr. Cyril Godard: cyril.godard@urv.cat

Dra. Noemí Cabello: ncabello@iciq.es

Assessment

	Description	Weight
Mixed tests	System of continuous assessment, divided as follow: -Tests: 55% -Written exams: 45%

Other comments and second exam session
System of continuous assessment, divided as follow: -Tests: 55% -Written exam: 45% During the exams, any mobil telephone, tablet or other device that has not been expressly authorized for the exam must be switched off and out of view. Any attempt to pass any exam of any subject by fraudulent means (be this physical or electronic) will result in the student being awarded a fail for the exam in question. In addition to this, the gravity of the offence may lead the faculty/school to propose that the student be subjected to disciplinary proceedings, which will be initiated by a resolution from the rector.

Sources of information

Basic	Hore, P. J., Nuclear Magnetic Resonance, Oxford Chemistry Primers 32., 1995 Friebolin, Horst, Basic One- and Two-Dimensional NMR Spectroscopy, Wiley-VCH, Weinheim., 2005 Claridge, Timothy D. W., High-Resolution NMR Techniques in Organic Chemistry, Pergamon Press, Oxford., 1999 Sanders, Jeremy K. M.; Constable, Edwin C.; Hunter, Brian K.; Pearce, Clive M., Modern NMR Spectroscopy. A Workbook of Chemical Problems., Oxford University Press, Oxford., 1993 Mitchell, Terence N.; Costisella, Burkhard, NMR – From Spectra to Structures., Springer-Verlag, Berlin., 2004 Bigler, P., NMR Spectroscopy: Processing Strategies, 2nd Ed., Wiley, 2000 Mitchell, T. N., Costisella, B., NMR – from Spectra to Structures an Experimental Approach, 2nd edition, Springer, 2007 Jacobsen, N. E., NMR Spectroscopy Explained, Wiley-Interscience, 2007 Simpson, J. H., Organic Structure Determination Using 2-D Nmr Spectroscopy - a Problem-Based Approach, Elsevier, 2008 McLafferty F.W. , Interpretation of Mass spectra, University Science Books, 1993 Sparkman David, Mass Spec Desk Reference, Global View Publishing, 2006 de Hoffmann Edmond , Stroobant Vincent ,, Mass Spectrometry: Principles and Applications, Wiley-Interscience, 2007 Watson,J. Throck ; Sparkman David , Introduction to Mass Spectrometry: Instrumentation, Applications, and Strategies for Data Interpretation, Wiley, 2007 Dass Chhabil, Fundamentals of Contemporary Mass Spectrometry, Wiley-Interscience, 2007 Desiderio, Dominic M.; Nibbering, Nico M., Mass Spectrometry: Instrumentation, Interpretation, and Applications, Wiley, 2008 Smith, Brian C., Infrared Spectral Interpretation: A Systematic Approach, CRC press, 1999 Stuart, Barbara H., Infrared Spectroscopy: Fundamentals and Applications, John Wiley and Sons, 2004 Brisdon, A. K., Inorganic Spectroscopic Methods, Oxford University Press, Oxford, 1998 Nakamoto, K., Infrared and Raman Spectra of Inorganic and Coordination Compounds, Wiley, New York, 4th Ed, 1986 Heaton, Brian, Mechanisms in Homogeneous Catalysis: A Spectroscopic Approach, Wiley-VCH, 2005

Complementary

Recommendations

(*)The teaching guide is the document in which the URV publishes the information about all its courses. It is a public document and cannot be modified. Only in exceptional cases can it be revised by the competent agent or duly revised so that it is in line with current legislation.