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Lecturer(s)
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Šimůnek Petr, doc. Ing. Ph.D.
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Svobodová Markéta, Ing. Ph.D.
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Course content
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Deeper look at spin-spin coupling: The analysis of the first-order multiplets. The manifestation of higher-order effects (virtual couplings, simplifications of the multiplets, AB systems) and their interpretation. The magnetic non-equivalence of the nuclei. Basic editation of carbon spectra: APT pulse sequence, advantages, drawbacks, interpretation. DEPT pulse sequence, advantages, drawbacks, interpretation. The application of the editation techniques for the solving of the structural problems. 2D NMR spectroscopy: Basic description of 2D spectrum. Basic correlation techniques. Homonuclear correlations: COSY, TOCSY, INADEQUATE. Heteronuclear correlations through single bond: HMQC, HSQC. Long-range heteronuclear correlations: HMBC. Hybrid 2D techniques: HSQC-DEPT, HMQC-TOCSY. The solution of the structural problems using 2D approach. Selective-excitation techniques: 1D COSY, 1D TOCSY Relaxation, through-space interaction, NOE: Nuclear Overhauser Effect, its origin, manifestations. Gated and inverse-gated decoupling. Relaxation after the application of radiofrequent pulse, its mechanisms, relaxation times, quadrupolar nuclei. The application of NOE for solution of structural problems, 1D and 2D NOESY. Mid-size molecules, 1D and 2D ROESY. Solution of structural problems using techniques with dipolar interaction. Dynamic NMR spectroscopy: Spectroscopic time-scales, molecular motion, chemical exchange. The effect of dynamic processes on spectral parameters. NMR spectroscopy of other selected nuclei (19F, 11B, 15N, 2H, 17O, 31P): chemical shifts, spin-spin couplings. Experimental approaches to the measurement of the selected heteronuclei. The solution of the spectral problems including heteronuclei. Basic work with TopSpin software.
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Learning activities and teaching methods
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unspecified, Monologic (reading, lecture, briefing), Dialogic (discussion, interview, brainstorming), Work with text (with textbook, with book), Methods of individual activities
- Contact teaching
- 52 hours per semester
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Learning outcomes
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The aim of the subject is to provide the students with deeper knowledge on NMR spectroscopy. It gives them an ability to use the advanced techniques offered by modern NMR spectroscopy for the solution of more complex structural problems. The main emphasis is to learn the students the skill to interpret the spectra single handedly and to suggest the convenient approach for solving various structural problems.
The ability to work single-handedly, precision, critical evaluation, conscientiousness.
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Prerequisites
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Basic knowledge on NMR spectroscopy and structural organic chemistry and stereochemistry.
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Assessment methods and criteria
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Oral examination, Written examination
The successful graduation from the subject means to pass the final exam. The exam consists of both written and oral part. The written part incorporates the solution of various types of structural problems. For its successful manage it is necessary to retrieve at least 60% of the possible points. The oral part incorporates e.g. the theoretical fundamentals of the methods presented during the whole course. The student is allowed to enter the oral part only after the successful manage of the written part. The final assessment is based on both the parts of the exam.
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Recommended literature
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Breitmaier E. Structure Elucidation by NMR in Organic Chemistry. Chichester, 1993. ISBN 0-471-93381-3.
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Duddeck H., Dietrich W., Tóth G. Structure Elucidation by Modern NMR, A Workbook. Darmstadt, 1998. ISBN 3-7985-1111-X.
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Jacobsen N.E. NMR Spectroscopy Explained. New Jersey, 2007. ISBN 978-0-471-73096-5.
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Jandera P. Atomová a molekulová spektroskopie se zaměřením na stopovou analýzu kontaminantů. Díl B ? Molekulová spektroskopie v organické analýze.. Pardubice, 2011. ISBN 978-80-7395-392-8.
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Silverstein R.M., Bassler G. C., Morill T. C. Spectrometric Identification of Organic Compounds.. New York, 1991. ISBN 0-471-54193-1.
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Simpson J. H. Organic Structure Determination using 2D NMR Spectroscopy. Amsterdam, 2008. ISBN 978-0-12-088522-0.
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Šimůnek P., Váňa J. Sbírka řešených příkladů z organické strukturní analýzy.. Pardubice, 2021. ISBN 978-80-7560-384-5.
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