Syllabus
Introduction: interaction of radiation and analysed compounds and classification of methods according to type of interaction. Utilization of information obtained by spectrometric methods for the qualitative, quantitative and structure analysis. Basic instrumentation (radiation sources, dispersion systems, detectors) and possible reasons for measurement errors.
Spectral analysis in X-ray range: Principles. Radiation emission (electron microanalysis), absorption, fluorescence, difraction. Experimental set- up in individual methods. Applications - elemental analysis; characterization of powdered samples (drugs).
Atomic emission spectral analysis in ultraviolet/visible range of radiation: Principles. Experimental - flame photometry, spectrography, methods with inductively coupled plasma (ICP), ICP- mass spectrometry. Applications - multielemental analysis, possibilities of analysis of biological samples.
Atomic absorption spectrometry in ultraviolet/visible range of radiation: Principles. Experimental - flame and electrotermic atomization, hydride technique; primary radiation sources. Application - trace quantitative metal analysis; biological samples.
Molecular absorption spectrometry in ultraviolet/visible range of radiation: Principles. Experimental - colorimetry, fotometry, spectrophotometry. Extraction spectrophotometry, kinetic methods of analysis, flow-through methods. Application - determinations using spectrophotometric reactions in analyte solutions; study of chemical (acid-base, complexation) equilibria.
Molecular absorption spectrometry in infrared range of radiation (vibration and rotation spectroscopy): Principles. Experimental - dispersion measurement, Fourier-transform spectrometers. Transmission and reflection measurement, measurement according to sample state. Application - compounds identification, structure determination, quantitative analysis.
Raman spectroscopy: Principles (non-elastic scattering of radiation, changes of vibration and rotation energy of molecules). Experimental - dispersion measurement, FT-Raman spectrometers. Applications, combination with infrared spectroscopy.
Nuclear magnetic resonance, electron spin (paramagnetic) resonance spectroscopy: Principles (systems with magnetic moments, effect of magnetic field). Experimental, application - structural analysis; medicine.
Mass spectrometry: Principle (ionic fragments with different mass and charge). Experimental. Application - identification of chemical compounds. The combination with separation methods (GC-MS, HPLC-MS).
Refractometry, interferometry: Principles (refractive index, molar refraction). Experimental in both methods. Application - identification of compounds, purity control, quantitative analysis.
Polarimetry, spectropolarimetry. Principles (polarization of light, optical activity of compounds, specific rotation). Experimental. Application - characterisation of compounds (drugs), quantitative analysis.
Nefelometry, turbidimetry: Principles (elastic scattering in turbid samples). Experimental. Application - quantitative analysis of aerosols, suspensions, body fluids.
Annotation
A basic overview in spectrometric methods used for chemical analyses. Principles of methods, interactions between the analyzed compounds and the electromagnetic radiation, instrumentation, typical measurement procedure and evaluation of results are explained in these lectures including listed examples of analytical applications.