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Last update: SUCHAN (12.04.2005)
Tomáš Grygar, Institute of Inorganic Chemistry AS CR Overview of methods used to identification of bulky and powdered solids and quantitative analysis of their mixtures without their chemical pre-treatment or dissolution. The overview includes non-destructive methods (X-ray powder diffraction, X-ray fluorescence analysis, infrared, visible, and ultraviolet spectroscopy, optical light and electron microscopy), methods requiring local destruction of samples (Raman spectroscopy and laser ablation), methods based on monitoring selective dissolution (chemical dissolution and voltammetry) and thermal decomposition (TG/DTA), and some further special methods. Extent: 2 hours weekly (1 hour lecture, 1 hour seminar). Seminars will include tasks such as abstracts of monographs and individual literature surveys. It is finished by an exam. It is designed for pregraduate students and doctoral students, mainly for those interested in analytical chemistry and geochemistry. |
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Last update: doc. RNDr. Karel Nesměrák, Ph.D. (09.05.2012)
• vybrané časopisecké publikace na téma přednášky • T. Grygar, F. Marken, U. Schröder, F. Scholz: Electrochemical analysis of solids. A review. Coll Czech Chem Commun 67 (2002) 63-107. • I. Němcová et al.: Spektrometrické analytické metody II. Praha, Karolinum 1998. |
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Last update: RNDr. Tomáš Matys Grygar, Ph.D. (16.11.2011)
Nejméně jeden referát z vybrané vědecké (časopisecké) publikace relevantní k tématu Diskuse v průběhu přednášek po referátech ostatních Diskuse na téma implementace přednášených metod do odborné práce studenta Zkouška probíhá formou testu, který shrnuje podstatné části odpřednášeného učiva |
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Last update: SUCHAN (12.04.2005)
1. Introduction The limits of traditional destructive analytical methods. The importance of direct identification of phase (mineralogical) and molecular composition of solids. Microanalysis - analysis with high spatial resolution. Differences in results based on characterization of atoms, functional groups, and crystals.
2. Traditional methods Optical microscopy. Identification of chemically and mineralogically pure species according to their basic physical properties.
3. Electron and X-ray fluorescence analysis Electron scanning (SEM) and transmission microscopy (TEM, HRTEM), electron and X-ray fluorescence element analysis. Surface imaging using various detectors. Size of the analyzed area or volume.
4. X-ray powder diffraction Prerequisites of acquisition of useful signal: Size of coherent length, structural disorder, sample size and nature. Conventional diffractometers, X-ray microdiffraction, and high-temperature measurements. Interpretation: identification using databases of known compounds, a quantitative analysis of mixtures, and estimating particle size.
5. Spectral methods Modes of measurement of solids: transmission and reflectance arrangement. Electron (UV-Vis-nr IR) and vibrational (IR) spectroscopy. Possibility of quantitative analysis of solids using diffuse reflectance spectroscopy. Infrared microspectroscopy: how to get useful signal.
6. Methods with excitation by laser and particle beam Locally destructive micromethods: Raman spestroscopy, methods based laser and particle ablation.
7. Kinetic methods Analysis of the course of thermal decomposition (TG/DTA/EGA). Methods based on monitoring the course of chemical dissolution (selective extraction systems). Voltammetry of microparticles.
8. Examples of application Speciation of transition metals in heterogeneous catalysts. Identification of active groups and phases in very poorly ordered matrices. Imaging - 2D representation of analytical signal. Remote sensing of Earth surface, portable instruments used in geological localities, scanning spectral microanalysis. Analysis of unconsolidated (soft) sediments. Definition and utilization of proxy parameters as a basis for climatic and environmental interpretations. Materials research of art works. Combination of traditional and high-tech analytical methods required by sample complexity. Problem of application of analytical methods in general practise.
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