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Atomic Spectroscopy Methods - MC230P13
Title: Metody atomové spektrometrie
Czech title: Metody atomové spektrometrie
Guaranteed by: Department of Analytical Chemistry (31-230)
Faculty: Faculty of Science
Actual: from 2017
Semester: winter
E-Credits: 2
Examination process: winter s.:
Hours per week, examination: winter s.:2/0, Ex [HT]
Capacity: unlimited
Min. number of students: unlimited
4EU+: no
Virtual mobility / capacity: no
State of the course: taught
Language: Czech
Note: enabled for web enrollment
Guarantor: RNDr. Václav Červený, Ph.D.
Teacher(s): RNDr. Václav Červený, Ph.D.
RNDr. Jakub Hraníček, Ph.D.
RNDr. Jan Kratzer, Ph.D.
RNDr. Eliška Nováková, Ph.D.
Annotation -
Last update: RNDr. Václav Červený, Ph.D. (08.01.2018)
The most frequently used methods of atomic spectrometry are compared in this course: atomic absorption spectrometry (AAS), atomic fluorescence spectrometry (AFS), inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS). Instrumentation, sampling methods, metrological and methodological problems, interferents influences, and analytical applications are discussed in each method. Furthermore, attention is paid to derivatizing the analyte (conversion to the volatile compound) and elemental speciation analysis including the increased demands of such assays. Typical detection limits, sensitivity, and concentration ranges are mutually compared between all atomic spectrometry methods.
Literature -
Last update: doc. RNDr. Karel Nesměrák, Ph.D. (28.10.2019)

1. Welz B. and Sperling M.: Atomic Absorption Spectrometry (3rd edn.), Wiley - VCH, Weinheim 1999.

2. Welz, B., Becker-Ross, H., Florek, S., Heitmann, U.: High-resolution continuum source AAS: the better way to do atomic absorption spectrometry, Wiley-VCH, Weinheim, 2005

3. Haswell S.J.: Atomic Absorption Spectrometry. Theory, Design and Applications, Elsevier, Amsterdam 1994.

4. Moore G.L.: Introduction to Inductively Coupled Plasma Atomic Emission Spectrometry, Elsevier, Amsterdam 1993.

5. Dědina J., Tsalev D.L.: Hydride Generation Atomic Absorption Spectrometry, Wiley, Chichester 1995.

6. Sanz-Medel A.: Flow Analysis with Atomic Spectrometric Detectors, Elsevier, Amsterdam 1999.

7. Černohorský T., Červený V., Dočekal B., Komárek J., Kratzer J., Spěváčková V., Sysalová J.: Atomová absorpční spektrometrie. Kurz AAS I. Spektroskopická společnost Jana Marka Marci a Vysoká škola chemicko-technologická v Praze (2015) ISBN 978-80-905704-6-7.
Requirements to the exam -
Last update: doc. RNDr. Karel Nesměrák, Ph.D. (28.10.2019)

The exam is oral. They try any of the lecturers of anything that has been recited
Syllabus -
Last update: RNDr. Václav Červený, Ph.D. (08.01.2018)

1. Introduction and listing of methods of atomic spectrometry: Principle and patterns of atomic spectrum. Emission and absorption spectra. Doppler and Lorentz broadering of the analytical line. Boltzman's relationship. Atomic absorption, fluorescence and emission methods. The most used methods.
2. Common components of instruments: sources of electromagnetic radiation; dispersing elements; detectors.
3. Preparation of samples for trace elemental analysis using atomic spectrometric methods as detectors. Working with solid samples, solid sampling technique, advantages and limitations (sample homogeneity, matrix effects, calibration curves). Mineralization of samples (instrumentation).
4. Atomic emission spectrometry with plasma excitation sources: method principle, plasma definition, plasma formation, physical properties of plasma; plasma excitation sources (DC coupled plasma, microwave-induced plasma, inductively coupled plasma, design, differences, benefits, usability)
5. ICP-MS: principle of joining both methods - instrumentation (interface design and function, plasma sampling area, plasma head, rotary and diffusion pumps, radio frequency generator, quadrupole mass analyzer, signal processing, system control); resolution, sensitivity, examples of spectras of some compounds; isotopic composition; isotope dilution method; mass interference.
6. Atomic absorption spectrometry: AAS principle, instrumentation: radiation sources (Xe-lamp, hollow cathode lamps, superlamps, non-electrodes, tunable dye laser, deuterium lamp); dispersive elements and auxiliary optics; atomization (principle, F-AAS, ETA-AAS, QF-AAS); radiation detection and non-specific background absorption compensation (photomultiplier vs. CCD, HR-CS-AAS correction, Zeeman correction, Smithe-Hieftje, D2 lamp - principles).

7. Atomic fluorescence spectrometry: Principle, fluorescence yield, AFS experimental arrangement, instrumentation, determinations, flame atomizers (DF, FIGS), advantages, special requirements, constraints and applications.
8. Generation of volatile compounds and application in atomic spectrometry methods: (methods, reactions, optimal release conditions - gas / liquid separators, transport of volatile compounds; atomization of volatile compounds (QTA, GF, DBD and other plasma); interferences in the determination of hydride forming elements (liquid phase or gaseous phase; cold vapor technique for mercury determination; applications to various samples in AAS, AFS, ICP-AES and ICP-MS).
9. Comparison of sensitivities and achievable limits of detection of individual methods of atomic spectrometry and comparison with other instrumental analytical methods including economic aspects. Development of individual methods. Numbers of applications of individual methods in publications and comparison with other instrumental methods.
10. Using the atomic spectrometers as highly selective detectors for separation techniques (interfaces, analyte conversion efficiency, post- (HPLC) vs. pre- (cryotrapping) column derivatization). Speciation analysis, extraction of analytes without loss of speciation information. Specifics of speciation analysis. Use of Reference Materials.
 
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