SubjectsSubjects(version: 875)
Course, academic year 2020/2021
  
Methods of analysis of solids - MC230P30
Title: Metody analýzy pevných látek
Czech title: Metody analýzy pevných látek
Guaranteed by: Department of Analytical Chemistry (31-230)
Faculty: Faculty of Science
Actual: from 2012
Semester: winter
E-Credits: 2
Examination process: winter s.:
Hours per week, examination: winter s.:2/0 Ex [hours/week]
Capacity: unlimited
Min. number of students: unlimited
State of the course: not taught
Language: Czech
Guarantor: RNDr. Tomáš Matys Grygar, Ph.D.
Opinion survey results   Examination dates   Schedule   
Annotation -
Last update: SUCHAN (12.04.2005)
Methods of analysis of solids
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.
Literature - Czech
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.

Requirements to the exam - Czech
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

Syllabus -
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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