Course code:
221A2
Course name:
Structural Instrumental Methods

Academic year:

2023/2024.

Attendance requirements:

201A2 + 202A2

ECTS:

9

Study level:

basic academic studies

Study programs:

Chemistry: 3. year, winter semester, compulsory course

Environmental Chemistry: 3. year, winter semester, compulsory course

Teacher:

Vele V. TeЙeviц, Ph.D.
full professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Assistants:

Gordana B. Krstiц, Ph.D.
assistant professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Stefan G. Ivanoviц

Katarina Z. Simiц

Hours of instruction:

Weekly: four hours of lectures + five hours of exercises (4+5+0)

Goals:

The goal of the course Structural Instrumental Methods is to introduce students to the basic instrumental techniques ‒ spectrometric and chromatographic ‒ used in chemistry. The course includes the basic theory of the interaction of electromagnetic radiation with matter, the absorption of electromagnetic radiation in various parts of the spectrum (Ultraviolet–visible spectroscopy, Infrared spectroscopy, 1H and 13C NMR spectroscopy), basic theory of mass spectrometry and chromatography (liquid and gas), measurement of spectra and chromatograms and their interpretation (by using tables) with a special focus on qualitative (structural determinations) and quantitative analysis. Students will become familiar with the equipment available at the Faculty of Chemistry (NMR, FT IR, UV/Vis, MS, GC). Students will also participate in sample preparation, spectra recording and their interpretation.

Outcome:

After they have successfully completed the course, students will be able to determine the structures of simple organic compounds by using spectroscopic methods. Furthermore, students will acquire the knowledge of the basic principles of instrument operation (NMR, IR, UV/Vis, MS, GC and HPLC).

Teaching methods:

Lectures, experimental and theoretical exercises.

Extracurricular activities:

Coursebooks:

  1. Слободан Милосављевић: Структурне инструменталне методе
  2. Веле Тешевић: Основе масене спектрометрије органских једињења
  3. Љубодраг Вујисић, Гордана Крстић, Ивана Софренић, Бобан Анђелковић, Веле Тешевић: Одређивање структуре молекула спектроскопским методама: Збирка спектара
  4. Clerck Pretsch and Simon Seibl: Tables of Spectral Data for Structure Determination of Organic Compounds

Additional material:

  Course activities and grading method

Lectures:

0 points (4 hours a week)

Syllabus:

  1. Ultraviolet/visible spectroscopy (UV/Vis). Energy and electron transfer, chromophores, dependence of λmax on the type of chromophore, the use of tables of spectral data to predict λmax for dienes and enones.
  2. Infrared spectroscopy (IR). Types of vibrations. Characteristic absorptions of some functional groups.
  3. The dependence of absorption intensity and νmax on structural factors.
  4. Nuclear magnetic resonance spectroscopy (NMR). Basic principles.
  5. Chemical shift (δ) in 1H NMR spectra. The coupling constant (J) and the integral.
  6. The multiplicity of signals (first-order spectra and higher-order spectra).
  7. Fundamentals of 13C NMR spectroscopy.
  8. Chemical shift (δ) in 13C NMR spectra.
  9. Qualitative and quantitative NMR analysis of organic compounds.
  10. Fundamentals of mass spectrometry (MS) and its application.
  11. Gas chromatography, basic principles of separation.
  12. Columns and detectors for gas chromatography.
  13. Liquid chromatography, basic principles of separation.
  14. Columns and detectors for liquid chromatography.
  15. Combined methods: Chromatography/mass spectrometry (GC/MS, LC/MS).

Exercises:

10 points (5 hours a week)

Syllabus:

  1. Using tables of spectral data to predict λmax for dienes and enones.
  2. Determining the structure of organic compounds based on the IR spectra by using tables of spectral data.
  3. Determining the structure of organic compounds based on IR, 1H NMR and UV/Vis spectra by using tables of spectral data.
  4. Determining the structure of organic compounds based on 1H NMR, 13C NMR, UV/Vis and IR spectra by using tables of spectral data.
  5. Determining the structure of organic compounds based on mass spectra by using tables of spectral data.
  6. Determining the structure of organic compounds based on 1H NMR, 13C NMR, UV/Vis, IR and MS spectra by using tables of spectral data.
  7. Students get some basic information about the equipment available at the Faculty of Chemistry (NMR, FT IR, UV/Vis, GC, LC, MS, GC/MS, LC/MS); sample preparation, recording spectra and their interpretation.

Colloquia:

30 points

Remarks:

  • Progress test I: UV and IR spectroscopy (10 points) in the first week of November.
  • Progress test II: 1H and 13C NMR spectroscopy (10 points) in the first week of December.
  • Progress test III: MS and chromatographic methods (10 points) in the second week of January.
  • An additional class session for the progress test in the third week of January.

Written exam:

20 points

Oral exam:

40 points