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 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. 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 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