2310 Estructura de macromolècules (6 crèdits)

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UIB
Universitat de les
Illes Balears
Masters in Chemical Technology and Science
SUBJECT DESCRIPTION
Details
Subject
Name of subject: Techniques for Experimentation in Chemistry
Code: 10150
Type: Optional
Level: Postgraduate
Year: 1
Semester: 1
Timetable:
See general course programme
Timetabled within module MCTQ6: Tools for the Diffusion and
Teaching of Chemistry
Language: Spanish, Catalan
Teaching staff
Subject leader
Name: Dr Gemma Turnes Palomino
Name: Dr Josefa Donoso Pardo
Name: Dr Gabriel Martorell Crespí
Name: Dr Magdalena Capó Cañellas
Name: Dr Bartolomé Simonet
Contact: g.turnes@uib.es
Contact: josefa.donoso@uib.es
Contact: biel.martorell@uib.es
Contact: magdalena.capo@uib.es
Contact: bartolome.simonet@uib.es
Pre-requisites:
Number of ECTS credits: 5
Contact hours: 41
Independent study hours: 86
Key terms:
Spectroscopic techniques: UV visible, fluorescence, infrared FTIR, nuclear magnetic resonance
(NMR). Mass spectrometry (MS). Gas and liquid chromatography techniques (GC and LC).
Electrophoretic techniques (CE and CEC).
General subject aims
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Introduce students to the main progress in separation and spectroscopic characterisation
in chemistry.
Approach the main separation techniques as indispensable aspects in a chemist’s work,
both in the commercial and research fields.
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Train students in the basic criteria to be able to choose and use correctly separation and
structural characterisation techniques, placing special emphasis on new separation
methods (chromatography and electrophoresis).
Subject skills and objectives
Specific:
 Be aware of the theoretical and practical principles behind UV visible, fluorescence, IR
NMR and MS spectroscopic techniques.
 Be aware of the theoretical and practical principles behind GC and HPLC
chromatographic techniques.
 Be able to use UV visible, fluorescence, IR NMR and MS spectroscopic techniques and
apply them to the resolution of the molecular structure of organic and inorganic
chemical compounds.
 Be able to use UV visible, fluorescence, IR NMR and MS spectroscopic techniques and
apply them to the resolution of analytical problems and problems with material
composition.
 Be able to use separation, chromatographic and electrophoretic techniques to determine
minority elements in complex matrices.
 Be able to use correctly separation techniques combined with spectroscopic detection
systems.
General:
 Be able to apply knowledge to practice.
 Be able to analyse information and synthesise concepts.
 Be able to communicate with others and work as part of team.
 Be able to work individually and plan and manage time.
Content
Introduction to spectroscopy. Interaction between matter and electromagnetic
Section radiation. Magnitude of energy of movements, electron transits and molecular spin
I
states: localisation in electromagnetic spectrum.
Section UV visible spectroscopy. Molecular spectroscopy of UV visible absorption. Intensity
II
and form of absorption bands. Applications. Characteristics of molecular emission
spectroscopy. Molecular fluorescence. Applications.
Practical content: Obtaining UV visible and fluorescence absorption spectra.
Decomposition of spectroscopic bands. Determining receptor-ligand union constants.
Section Infrared molecular absorption spectroscopy. Basics in IR spectroscopy. IR
III
spectrometer. IR techniques. Applications of IR spectroscopy.
Practical content: Learn to use IR spectrometer. Obtain and interpret solid and liquid
sample spectra.
Section NMR spectroscopy. Introduction. Instrumentation. NMR basics. Interpretation of
IV
one-dimensional spectra. NOE effect. Introduction to main multidimensional
techniques: 2D and 3D NMR. Application of multidimensional techniques to
structural elucidation of macromolecules: proteins and nucleic acids.
Practical content. a) 1D NMR: characterisation of different medicines. b) 2D NMR:
structural elucidation of an immunosuppressant polypeptide: cyclosporine. c)
Structural elucidation of a metalloproteinase inhibiting enzyme.
Section Mass spectrometry (MS). Introduction. Instrumentation. Recording mass spectra.
V
Mass spectra generation mechanisms. Main fragmentations of organic compounds.
Interpreting mass spectra. Ionisation methods: chemical electrospray ionisation (ESI),
fast atom bombardment (FAB), other methods. Types of analysers. Main applications
of MS.
Practical content. a) Identification by GC/MS of volatile compounds in liquid
emitted by the skunk. b) Analysis of 201 pesticides by GC/MS in fruits and
vegetables. c) Determining drugs in urine by GC/MS. d) Determining substances
responsible for “bad taste” in beer.
Section Progress in chromatographic systems. Evolution of chromatographic systems. HighVI
speed gaseous chromatography. Liquid micro and nano-chromatography.
Development in monolithic capillary columns. Development of molecular impression
and chiral separation polymers. Progress in sample introduction systems: integrated
systems.
Progress in electrophoretic systems. Evolution of electrophoretic methods.
Electrochromatographic systems. Development of electrophoretic microchips.
Integrated -TAS.
Hybrid systems. Coupling electrophoretic and chromatographic systems to MS.
Atmospheric pressure interphases based on chip technology.
Practical content. a) Direct analysis of antibiotics (tetracyclines) in urine samples by
LC-UV-Vis. b) Determination of pesticides (chlorophenolic compounds) in water
samples by solid phase micro-extraction coupled with GC-FID. c) Determination of
DNA genetic sequencing by means of PCR amplification and electrophoretic analysis.
Methodology and student work plan
1. Learning methods: Attendance at theory classes (16 hours)
Class work
Group size: intermediate
Lectures include PowerPoint presentations. All material will be made available to
students.
2. Learning methods: Study/preparation for theory classes (16 hours)
Independent study
Use of e-learning: Information on the web, e-mail
Group size: individual
3. Learning methods: Attendance at and work in practical classes (20 hours)
Supervised class work
Group size: intermediate
Laboratory work in the laboratories belonging to the Department of Chemistry
(chromatographic techniques, UV visible spectroscopy) and/or in those of the UIB scientific and
Technical Services (NMR, IR, MS). These will be individual where space allows.
4. Learning methods: Study/preparation for and report on practical classes (35 hours)
Independent and/or small group study
Use of e-learning: Information on the web, e-mail
Group size: individual and/or small group
5. Learning methods: Individual tutorials (5 hours)
Physical and /or via e-mail
Use of e-learning: Information on the web, e-mail
Group size: individual
Tutorials will be personalised and allow a better coordination and guidance of students.
The tutor will check on student progress and be able to resolve any problems.
6. Learning methods: Coursework and report on supposed practical work for final assessment
(35 hours)
Physical and /or via e-mail
Use of e-learning: Information on the web, e-mail
Group size: individual
Learning agreement and assessment criteria and instruments
Assessment criteria:
Students must attend at least 85% of theory sessions and 95% of practical session to pass the
course.
The final mark will be gained from:
 Report on activities from practical classes (50%)
 Report on supposed practical work for final assessment (50%)
Is assessment organised by means of a learning agreement? No
Bibliography, resources and appendices
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Métodos Espectroscópicos en Química Orgánica. Manferd Hesse. Herbert Meier.
Bernd Zeeh. Editorial Sintesis.1997. ISBN: 87738-522-X
Spectrophotometry and spectrofluorimetry. A practical approach. Editorial: IRL
press. Oxford. 1987
Structural Methods in Inorganic Chemistry. E.A.V. Ebsworth, D.W.H. Rankin, S.
Cradock. Blackwell Scientific Publications, 1991.
Técnicas de separación en Química Analítica. R. Cela, R. A. Lorenzo and M. C.
Casais. Síntesis, Madrid, 2002
Cromatografía y electroforesis en columna . M. V. Dabrio. Springer-Verlag Iberica,
Barcelona, 2000
Interpretation of Mass Spectra.Fred W. McLafferty. Frantisek Turecek. University
Science Books. 1993. ISBN: 0-935702-25-3
Basic One- and Two-Dimensional NMR Spectroscoy Horst Friebolin. VCH. 1993
ISBN 3-527-29059-1
NMR of Proteins and Nucleic Acids. Kurt Wüthrich. John Wiley & Sons, Inc. 1986
ISBN 0-47182893-9
UV-VIS spectroscopy and its applications. H.H. Perkampus. Springer-Verlag. Berlin
1992
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