Contemporary Methods of Analysis and Establishing Chemical Compound Structure

1. apply the acquired knowledge during the course and apply them in decision making and problem solving in the analysis of real samples
2. argue the advantages, disadvantages and limitations of each sample preparation method
3. apply sampling methods to real samples and prepare the real samples for analysis, analyze them, interpret and evaluate the obtained analysis results
4. analyze and interpret spectra of known organic compounds by spectroscopic methods UV / VID, FTIR, fluorescence, 1H and 13C NMR, and mass spectrometry
5. analyze, determine and confirm the structures of unknown compounds based on data obtained by spectroscopic methods
6. explain the factors affecting spectral parameters in UV / VIS, FTIR, 1H and 13C NMR spectra

PowerPoint presentations

Solving practical problems like interpretation of the obtained spectra (UV / VIS, IR, NMR, MS spectra)

visit to the Croatian Standards Institute

making and presenting seminar work on a given topic

practical exercises in the lab

1. Definition of the sample. Sampling errors and sampling uncertainty. Sampling planning. Sampling procedures (air, water, soil, sediment, biological samples). Laboratory exercises: Preparation of water samples for chromatographic analysis: Determination of the usefulness of the solid phase preparation column (SPE) using liquid chromatography of high performance.
2. Preparation of samples for analysis. Importance and the basic principle of sample preparation in the analysis. The objective of sample preparation. Optimization of the sample preparation process. Laboratory exercises: Preparation of water samples for chromatographic analysis: Determination of the usefulness of the solid phase preparation column (SPE) using liquid chromatography of high performance. Comparison of extraction methods for the determination of polyphenolic compounds in food samples: extraction by scattering the sample nut through a solid phase, solvent extraction by ultrasound and microwaves.
3. Review the method of sample preparation. Extraction as the oldest sample preparation method. Analytes in solid samples. Analytes in liquid samples. Analyzes in the Gaseous Phase. Other methods of sample preparation. Real Samples: Problems and Access. Special applications. Laboratory exercises: Comparison of extraction methods for the determination of polyphenolic compounds in food samples: extraction by scattering the sample nut through a solid phase, solvent extraction by ultrasound and microwaves.
4. Techniques and methods of chemical analysis according to the type of samples: analysis of inorganic and organic compounds. Classical methods. Instrumental methods (spectrometry, electroanalytic methods, separation and other techniques). Qualitative analysis (identification and detection) and quantitative analysis. Laboratory exercise: Comparison of HPLC and HPTLC analytical methods: HPLC-DAD determination of sulfonamide antibiotics in wastewater - identification and detection.
5. Standard methods in environmental analytics. Calibration procedures. Macroanalysis of compounds. Trace analysis and ultratrace analysis. Laboratory exercise: Determination of inorganic compounds in inorganic matrix using classical and instrumental methods. Determine a rough error (Q-test).
6. Insurance of measurement data quality: errors in environmental analysis, validation of methods, uncertainty measurement, chemometrics in analytics. Laboratory exercise: Validation of chromatographic determination of pesticides in soil.
7. First partial test
8. Ultraviolet-visible spectroscopy (UV/VIS): electronic transitions, basic photophysical processes, light absorption (Lambert-Beer's law), chromophores, examples of UV/VIS spectra. Fluorescence spectroscopy, examples of emission spectra. Practice problems: Recording and interpretation of qualitative and quantitative absorption and emission spectra of selected molecules.
9. Infrared spectroscopy with I Transformation (FTIR): vibration of covalent bonds in molecules (stretching and bending), area of functional groups and fingerprint area, examples of IR spectra. Practice problems: Recording and interpretation of IR spectra of selected molecules
10. Nuclear magnetic resonance spectroscopy (1H i 13C NMR): physical principles, spectral parameters of NMR (chemical shift, spin-spin coupling constant J, relative signal intensity, peak width), factors influencing chemical shift, Nuclear Overhauser effect (NOE) Practice problems: Interpretation of 1H and 13C NMR spectra of selected molecules and confirmation of their structure.
11. 1H NMR spectroscopy: spin-spin couplings (1H-1H), multiplets (n+1 rule), coupling schemes Practice problems: spin-spin coupling and multiplet interpretations in 1H NMR spectra
12. 13C NMR spectroscopy: spin cutting techniques; untreated and rasped spectra, APT, DEPT Two-dimensional (2D) NMR spectroscopy: homonuclear 1H-1H (COSY, NOESY) and heteronuclear 1H-13C (HSQC, HMQC) correlations Practice problems: 13C NMR spectra interpretation; application of 2D NMR spectroscopy in molecular structure confirmation
13. Mass spectrometry (MS): ionization methods, high resolution mass spectrometers, basic processes of fragmentation of organic compounds. Practice problems: Recording and interpretation of MS spectra of selected molecules.
14. Presentation of seminar papers by students
15. Second partial test