615-0803/01 – Organic Analysis (OA)
Gurantor department | Department of Analytic Chemistry Processes | Credits | 6 |
Subject guarantor | doc. RNDr. Ervín Kozubek, CSc. | Subject version guarantor | doc. RNDr. Ervín Kozubek, CSc. |
Study level | undergraduate or graduate | Requirement | Compulsory |
Year | 2 | Semester | winter |
| | Study language | Czech |
Year of introduction | 2004/2005 | Year of cancellation | 2013/2014 |
Intended for the faculties | FMT | Intended for study types | Follow-up Master |
Subject aims expressed by acquired skills and competences
To take up with instrumental methods in organic analysis. The main attention is paid to the separation and spectral methods and their use in the analysis of organic substances.
Teaching methods
Lectures
Experimental work in labs
Project work
Summary
The subject is an extension of the subject in Inorganic Analysis and describe the structure of organic compounds, both in terms of theoretical, and practical (deepening of spectral and separation methods of instrumental structural analysis). In limited range it also deals with classic organic analysis of functional groups and their reactions.
Compulsory literature:
1] Praus, P., Dombek V., Klika Z. Základy analytické chemie VŠB-TUO, Ostrava,
2001, 110 s.
[2] Stránský, Z. a kol. Analýza organických sloučenin UP, Olomouc,1981. 235 s.
[3] Holzbecher, Z., Churáček J.a kol. Analytická chemie SNTL, Praha 1987, 664
s.
[4] Zýka, J. a kol. Analytická příručka 1. a 2. díl, SNTL, Praha např. 1973 a
1988.
[5] Kalous, V. a kol. Metody chemického výzkumu SNTL Alfa, Praha 1987. 431s.
[6] Böhm, S., Smrčková-Voltrová S. Strukturní analýza organických látek
Skripta, VŠCHT Praha, Praha, 1995.
Recommended literature:
[1] Churáček, J. a kol. Analytická separace látek SNTL, Praha, 1990, 384 s.
[2] Kalous, V. Jak moderní chemie zkoumá strukturu molekul SNTL, Praha, 1983, 152 s.
Additional study materials
Way of continuous check of knowledge in the course of semester
E-learning
Other requirements
There are no additional requirements for students.
Prerequisities
Co-requisities
Subject has no co-requisities.
Subject syllabus:
1st Sample preparation for analysis and preliminary testing. Sample preparation for trace analysis: liquid extraction, sorbent extraction, headspace-gas extraction
analysis, extract purification, properties (physical state, color, odor, solubility,
groupings).
2nd Electron spectroscopy (UV, VIS) luminescence spectroscopy.
Molecular orbitals, chromophore, LCAO theory, ligand field theory, charge
transfer complexes, selection rules, auxochrom, influence the position and intensity molecular bands. UV-VIS spectroscopy. Radiation sources, monochromators, types cells, detectors, practical applications in the UV and VIS region. Luminescence spectrometry. Fluorescence, phosphorescence, practical use.
3rd Infrared spectroscopy. Rotational and vibrational spectra of small rotation
molecules, harmonic and anharmonic oscillator, wave number, selection rules, types of vibration. calculate the lengths of links, classical infrared spectrometer, preparation samples of gases, liquids and solids measurement, spectrum analysis, interpretation fundamental frequency spectroscopy of organic molecules. FTIR instrument, spectroscopy, qualitative and quantitative evaluation of the determined elements. Near infrared (NIR).
4th Raman spectroscopy. Polarization of molecules induced and permanent,
Rayleigh scattering, Stokes and anti-Stokes line. Instrumentation: Laser
sources, monochromators, detectors, applications (e.g. biology). Nuclear
magnetic resonance spectroscopy. Nuclear spin, magnetic moment,
Larmor frequency, the Boltzmann distribution, spin-lattice relaxation, relaxation
spin-spin, chemical shift (due to the aromatic core, insulated double and triple
ties), the first spectrum order, constant interaction.
5th Nuclear magnetic resonance spectroscopy (continued). NMR spectrum
higher orders, simplifying the spectra (sliding agents, deuterizace,
decoupling), the influence of chemical exchange in NMR spectra. Instrumentation and evaluation of spectra, spectra of selected organic compounds. 13C-NMR spectroscopy, pulse methods, Fourier transform, the accumulation of data, examples spectra.
6th Mass spectrometry. Molecular ion and fragmentation, the basic
fragmentation mechanisms, the fragmentation of some organic compounds. Methods ionization (EI, CHI, MALDI, APIs, etc. FAB)
7th Mass spectrometry (continued). Methods of separation and detection of ions
(Single and double fokuzace, flight analyzer), examples of fragmentation
ions to determine the molecular weight determination of elemental formulas, and examples Interpretation of mass spectra.
8th The combination of spectral methods. Identification of substances by UV-Vis spectra, MS IR, NMR and elemental analysis, practical examples.
9th Electrochemical methods in organic analysis. Electrolysis, the mass transfer
electrolysis, diffusion and capacitive current Ilkovič equation. Polarography:
Polarographic curves halfvawe potential interferences and their elimination,
pulse methods, practical applications. Voltammetry, stripping voltammetry,
coulometry.
10th Gas chromatography. Carrier gases, sample injection, filling the columns,
detectors (including GC-MS), pyrolysis chromatography, derivatization of organic
substances. Separation of aliphatic and aromatic hydrocarbons, alcohols, phenols, carboxylic acids, esters and amino acids, carbonyl compounds, amines and amides. Examples of applications in environmental analysis (PAHs, PCBs, selected pesticides, dioxins, volatile halogenated substances, phenols, etc.).
11th Liquid chromatography. The choice of mobile and stationary phases, dose
sample, columns, detectors, ion chromatography and gel. Separation
aromatic hydrocarbons, esters, carboxylic acids and amino acids, amines and
amides, examples of use in environmental analysis (PAHs, selected
pesticides, phenols, etc.).
12th Electromigration methods. Capillary zone electrophoresis, gel
electrophoresis, capillary isotachophoresis, isoelectric focusing. Description
basic theoretical principles and instrumentation. Using the separation
karboxylovýh acids, phenols, amines and amino acids, peptides and proteins,
humic substances, DNA fragments, chiral separations.
13th The combination of spectral separation methods and GC-MS, LC-MS, LC-NMR, LC / GC-FTIR, LC-UV/VIS LC-AAS, GC-AES. The combination of both techniques (molecular separator) ionization methods, detection of ions.
14th Elemental analysis. Sample decomposition and oxidation-reduction destruction. Evidence and identification of C, H, N, O, S, halogens, other elements. Evidence of functional groups and identification of organic compounds. Determination of organic substances based on reactions of functional groups. Determination of physical constants. Melting point and mixed melting point, boiling point and distillation curve, density, refractive index, optical rotation, calorific value, surface tension, etc.
Conditions for subject completion
Occurrence in study plans
Occurrence in special blocks
Assessment of instruction