C9055 Analysis of geological materials by X-ray fluorescence spectrometry

Faculty of Science
Spring 2023
Extent and Intensity
1/0/0. 1 credit(s) (plus extra credits for completion). Type of Completion: zk (examination).
Teacher(s)
Mgr. Aleš Hrdlička, Ph.D. (lecturer)
Guaranteed by
doc. Mgr. Karel Novotný, Ph.D.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science
Prerequisites
Basic knowledge of analytical chemistry is recommended but not required.
Course Enrolment Limitations
The course is offered to students of any study field.
Course objectives
The subject is aimed to introduce fundamentals of X-ray fluorescence theory and applications in quantitative elemental analysis of mainly but not solely geological samples.
Learning outcomes
Students will understand principles of X-ray generation, use of X-ray in analytical chemistry and geology, pros and cons of X-ray fluorescence analysis, schemes of energy and wavelength dispersive X-ray spectrometers; will be able to solve some problems of matrix effects and spectral interferences; will be able to work and analyze selected geological nad metallic materials with ElvaTech X-ray fluorescence spectrometer and analyze selected geological and metallic materials.
Syllabus
  • Theoretical lectures 1) nature of electromagnetic radiation and its kinds, wave, photon and its energy, energy levels of electrons in atoms and transitions, continuous spectrum, Bremsstrahlung, discrete spectrum, physical principles of X-ray, Auger electrons, continuous X-ray and characteristic lines, Moseley law, X-ray nomenclature both traditional (Siegbahn notation) and modern (IUPAC systematic notation), methods of X-ray generation, principles of X-ray sources 2) dispersion and monochromatization, collimation, crystals, Soller plates, detection (scintillation, proportional, semiconductor…detectors), X-ray spectrometers energy and wavelength dispersive, advantages and disadvantages, advanced combined instrumentation: principles and use of electron microprobe X-ray microanalysis (EMPXA), X-ray microscope, particle-induced X-ray emission (PIXE), X-ray diffraction (XRD), total reflection X-ray fluorescence (TXRF). Area of use of X-ray analytical instrumentation, laboratory and portable instruments, comparison of its analytical capabilities with inductively coupled plasma optical emission or mass spectrometry (ICP-OES or MS), atomic absorption spectrometry (AAS) 3) Light elements, limitations in bulk and spatially resolved analysis, limit of detection and quantification, calibration in XRF: principle, fundamental parameters, calibration standards, matrix of calibration coefficients, matrix matched calibration, matrix effects, inter-element effects, crystallographic effects, influence of the sample shape, surface and state, powder, pressed, irregular samples, sample inhomogeneity, sample preparation, examples of geological samples, presentation and comparison of results Practical training 1) XRF laboratory spectrometer ElvaTech, its construction and components, safety regulations, area of use, control software, use of internal calibration for demonstrative analysis of compact XRF calibration standards: copper alloys (discs), iron alloys (shavings) 2) External calibration, comparison of calibration using pressed pellets and powder of synthetic limestone, analysis of limestone samples, presentation and comparison of results 3) Calibration using fused pellets and NIST glass, analysis of silicate and oxide samples (obsidian, ceramics), rock samples with complex matrices, selection of representative spots, comparison of results from different calibration standards
Literature
  • Handbook of practical X-ray fluorescence analysis. Edited by Burkhard Beckhoff - Birgit Kanngiesser - Norbert Langhoff - Reiner Wed. Berlin: Springer, 2006, xxiv, 863. ISBN 3540286039. info
  • BERTIN, Eugene P. Introduction to X-ray spectrometric analysis. New York: Springer Science+Business Media, 1978, xiv, 485. ISBN 9780306310911. info
Teaching methods
2-3 theoretical lectures, 7 h total; 3 sessions of practical training, 7 h total
Assessment methods
A student must -actively participate in all laboratory tasks -have accepted protocols from all laboratory tasks. Evaluation: 1/2 of the mark - quality of protocols and laboratory work 1/2 of the mark - oral theoretical exam
Language of instruction
Czech
Further Comments
The course is taught annually.
The course is also listed under the following terms Spring 2020, Spring 2021, Spring 2022, Spring 2024, Spring 2025.
  • Enrolment Statistics (Spring 2023, recent)
  • Permalink: https://is.muni.cz/course/sci/spring2023/C9055