SYLABUS: Introduction to the subject Instrumental analysis vs. chemical analysis. Qualitative analysis and identification of substances. Methods of quantitative analysis (m. of calibration curve, standard sample and standard addition(s). Electroanalysis Potentiometry: Electrode potential, indication and reference electrodes. Glass electrode and other pH-sensing electrodes, pH measurement. Direct potentiometry with on-selective electrodes (ISEs): F-, NO3-, Ca2+-, and K+-ISE. Potentiometric indication in traditional titrations. Choice of electrodes, examples of applications. Polarography, voltammetry, and related techniques: Polarization and depolarization, faradaic vs. non-faradaic currents. Classical (Heyrovsky) polarography and dropping mercury electrode (DME). Voltammetry with linear and modulated-potential techniques: LSV (DC), DPV and SWV. Working electrodes, applications. Amperometry and biosensors. Coulometry and Faraday's law. Conductometry and conductivity in solutions. Spectral analysis Electromagnetic irradiation and its classification. The formation of spectra and their types. Spectrophotometry (SpF) in UV/Vis-region: absorption spectra, transmittance vs. absorbance. Lambert-Beer law and its analysis. Instrumentation and use. Luminescence spectrometry and fluorimetry. Atomic emission spectrometry (AES): Classical spectrography: emision spectra and their analysis. Flame photometry. Modern variants of AES: ICP-OES and LIBS. Atomic Absorption Spectrometry (AAS): Variants FL-AAS, ET-AAS, HG-AAS, and CV-AAS. Equipment for AAS: scheme (fig.) and its description. AAS in analytical practice (examples). Infrared spectrometry (IR-S): Classical (dispersive) IR, Basic principles of FTIR, interpretation of IR-spectra and applications to identify various substances. Mass Spectrometry (MS): Principles, scheme, and description of MS equipment: ways of ionizations, ion fragmentation, molecular ion. Apparatus for MS and its scheme. interpretation of MS-spectra. Non-spectral (optical) techniques: Polarimetry. Nephelometry and turbidimetry. Analytical separations Basic definitions and classifications. Principles of separation: two-phases separations (adsorption and extraction), ion exchange, inclusion (permeation) effect, bioaffinity. Planar chromatography: Paper- (PC) and thin-layer chromatography (TLC): Principles of separation, experimental equipment for both PC and TLC. Working procedures, physical and chemical detection of TLC-spots. Examples of use. Gas Chromatography (GC): Separation in gas/solid and gas/liquid phase systems. Chromatograms, their description and evaluations. Instrumentation: GC apparatus in scheme with description of the individual parts. Types of columns, detectors (TCD, FID, ECD and MS). Typical applications. Liquid chromatography (LC or HPLC): Separation in liquid/solid, liquid/liquid, and reverse phase systems. HPLC: mobile or stationary phases. Device for HPLC: scheme and its description. Pumps, columns, and detectors: (UV/Vis, FL, RF, EC, LC-MS coupling). Analytical applications Electromigration techniques: Separation of charged particles in the electric field. Classic (zone) electrophoresis in planar arrangement (ZE), capillary and gel electrophoresis (CE and GE), isotachophoresis (ITP). Use of ZE, CE , GE, and ITP. Extraction and other pre-concentration techniques: Distribution equilibria in a system of different phases. Liquid-to-liquid extraction, Soxhlet apparatus (and its function). Extraction of a solid with a liquid. Extraction with gases. Extraction with solid sorbents. Supercritical fluid extraction. Principles and analytical use (with examples).
|