Course code:
221B2
Course name:
Structural Instrumental Methods

Academic year:

2023/2024.

Attendance requirements:

201B2 + 202B2

ECTS:

6

Study level:

basic academic studies

Study program:

Biochemistry: 3. year, winter semester, compulsory course

Teacher:

Ljubodrag V. Vujisiц, Ph.D.
associate professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Assistants:

Ivana V. Sofreniц, Ph.D.
assistant with PhD, Faculty of Chemistry, Studentski trg 12-16, Beograd

Katarina Z. Simiц

Stefan G. Ivanoviц

Hours of instruction:

Weekly: four hours of lectures + three hours of exercises (4+3+0)

Goals:

The goal of this course is to introduce students to the basic instrumental techniques - spectrometric and chromatographic - which are used in chemistry nowadays. 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), the basic theory of mass spectrometry and chromatography (liquid and gas), the measurements 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, FTIR, UV/Vis, MS, GC) and they will participate in sample preparation, spectra recording and their interpretation.

Outcome:

After successfully completing this course, students will be able to determine the structures of simple organic compounds by using spectroscopic methods. Furthermore, students will be familiar with the fundamental working principles of some instruments (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, using tables of spectral data to predict λmax for dienes and enones.
  2. Infrared spectroscopy (IR). The 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. The chemical shift (δ) in 1H NMR spectra. The coupling constant (J) and the integral.
  6. Signal multiplicity (first-order spectra and higher-order spectra).
  7. Fundamentals of 13C NMR spectroscopy.
  8. The 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, the basic principles of separation.
  12. Columns and detectors for gas chromatography.
  13. Liquid chromatography, the basic principles of separation.
  14. Columns and detectors for liquid chromatography.
  15. Combined methods: Chromatography/mass spectrometry (GC/MS, LC/MS).

Exercises:

10 points (3 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 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, FTIR, UV/Vis, GC, LC, MS, GC/MS, LC/MS); sample preparation, recording spectra and their interpretation.

Colloquia:

30 points

Remarks:

  • Progress test 1: UV and IR spectroscopy (10 points)
  • Progress test 2: 1H and 13C NMR spectroscopy (10 points)
  • Progress test 3: MS and chromatographic methods (10 points) 

Written exam:

20 points

Oral exam:

40 points