Spectroscopic Methods in Chemical Analysis 310-ERS-MSA
Konwersatorium (KON) Rok akademicki 2023/24

Course credit is awarded based on a written final test. The passing requirement is to achieve a minimum of 51% of the total points.

One retake test is allowed.The final grade is assigned in accordance with the University of Białystok (UwB) Study Regulations. A student's activity and completion of additional tasks may influence the final grade.

Unexcused absence from more than three classes will result in a failure to receive credit for the course. In the case of an excused absence, the student must arrange an individual form of catching up on the material with the instructor.

It is possible to introduce flexible forms of course credit, agreed upon between the instructor and the student, following the principles of universal design for learning. Such conditions must be established at the beginning of the semester.

1. Types of spectroscopic methods (UV-VIS, MS, IR, ¹H and ¹³C NMR), their physical basis and examples of application. Information obtained from spectra. Conversion of wavelength to frequency and wavenumber.

2. Mass spectrometry: ionization methods; types of ions (molecular, base, fragment, isotopic ions), ion fragmentation pathways; distinguishing simple compounds based on the intensity of fragment ions; MS spectra of compounds containing a halogen atom; influence of the ionization method (energy) on the MS spectrum shape.

3. UV-VIS spectroscopy: basic concepts (chromophore, auxochrome, bathochromic shift, hypsochromic shift, hyperchromic effect, hypochromic effect); absorption laws; determination of the molar absorption coefficient and specific absorption coefficient.

4. Infrared spectroscopy (IR): harmonic oscillator; Hooke's law – approximate determination of absorption bands based on the masses of vibrating atoms; types of vibrations observed in IR spectroscopy; sample preparation methods; characteristic absorption bands of functional groups; identification of bonds and functional groups in IR spectra; hydrogen bonding in IR.

5. NMR spectroscopy: nuclear spin; magnetic moment of the nucleus and its interaction with a magnetic field (Boltzmann distribution, number of allowed spin orientations); conditions necessary for recording an NMR spectrum (nuclear property, Bo field, electromagnetic pulse); sample preparation (standards and solvents). Converting ppm values to Hz at a known operating frequency of the instrument. Basic terms: chemical equivalence; homotopic, enantiotopic, and diastereotopic protons (groups of protons); chemical shift δ, multiplicity, spin-spin coupling constant J, signal intensity, n+1 rule, Pascal's triangle, shielding effect, deshielding effect. Data read from ¹H and ¹³C NMR spectra and their significance for identifying the chemical structure of the studied compound. Characteristic ranges of chemical shift values for signals in ¹H and ¹³C NMR spectra of organic compounds. Predicting the pattern of a first-order ¹H NMR spectrum based on a known compound structure (determining the number of signals, their intensity, multiplicity, and position on the scale). Anisotropic effect – ¹H NMR spectra of benzene, ethene, and ethyne.

6.¹³C NMR spectra recorded using the DEPT technique (90 and 135) – determining the number of hydrogen atoms bonded to a carbon atom.

7. Determining the topicity of protons (diastereotopic, enantiotopic, homotopic).

8. Determining the values of chemical shifts δ [ppm] for signals in the ¹H NMR spectrum: singlet (s), doublet (d), triplet (t), quartet (q), doublet of doublets (dd), and multiplet (m).

9. Determining the value of the coupling constant J [Hz] for signals in the ¹H NMR spectrum: doublet (d), triplet (t), quartet (q), and doublet of doublets (dd).

10. Interpretation of IR, ¹H NMR, ¹³C NMR spectra of simple organic compounds (saturated and unsaturated hydrocarbons, aromatic compounds, aldehydes, ketones, etc.). Working with IR and NMR Correlation Tables.

a) Interpretation of signals in ¹H and ¹³C NMR spectra;

b) Interpretation of bands in IR spectra;

c) Assignment of signals in ¹H and ¹³C NMR spectra of a known organic compound to the corresponding hydrogen and carbon atoms.

d) Preparation of IR, ¹H, and ¹³C NMR text interpretation according to a given template.

11. Distinguishing geometric isomers (cis/trans) based on proton spectra.

12. Predicting the influence of shielding and deshielding substituents in an aromatic ring.

13. Drawing diagrams illustrating the shape of ¹H NMR signals depending on the values of coupling constants.

Teaching methods: instruction, problem-based learning, group work, discussion, brainstorming, consultations.

The classes are primarily based on solving spectroscopy problems of varying difficulty (basic level), aimed at preparing students for the independent interpretation of spectral data.

Class structure:

1. Introduction: A presentation of key concepts by the instructor.

2. Practical part: Students solve problems by working individually or in small groups. The instructor actively participates in this part by providing guidance and discussing the results.