PřF:C7060 Trace Analysis - Course Information

C7060 Trace Analysis

Extent and Intensity

2/0/0. 2 credit(s) (plus extra credits for completion). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
In-person direct teaching

Teacher(s)

prof. RNDr. Josef Komárek, DrSc. (lecturer)
doc. RNDr. Pavel Coufalík, Ph.D. (lecturer)

Guaranteed by

prof. RNDr. Josef Komárek, DrSc.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science

Timetable

Wed 8:00–9:50 C14/207

Prerequisites

Knowledge of Analytical chemistry on the level of fundamental courses.

Course Enrolment Limitations

The course is also offered to the students of the fields other than those the course is directly associated with.

fields of study / plans the course is directly associated with

• Analytical Chemistry (programme PřF, N-CH)

Course objectives

The main objective of the course is to obtain an overview and deeper knowledge in the field of trace analysis from clean laboratory, treatment of samples and flow analysis to preconcentration of trace elements. At the end of the course, students should be able to: - understand the problems of trace analysis - choose system of work in laboratory for trace analysis - characterize parameters important for environment of clean laboratory - compare capacities for methods for preconcentration of trace elements and separation of matrix - assess the advantages of flow analysis.

Learning outcomes

The student is able to: - utilize knowledge of requirements for environment of clean laboratory at work in this laboratory - use methods for preconcentration of trace elements by ultratrace analysis - assess the advantages of flow analysis.

Syllabus

• 1. Specific problems in work with a small amount of sample. Microanalysis, ultramicroanalysis, conversion from macroscale to microscale, sample homogeneity, microprobe. Microgravimetry, precipitation, filtration, drying, annealing, microelectrogravimetry. Microtitration, volumetric flasks, micropipettes, microburettes, titration vessels. Potentiometric, conductometric and amperometric microtitration. Microphotometry, flow microcells. Micrometry, sedimetry, Microanalytical balances, microbalances. Electromagnetic balances, microbalances with a quartz resonator. 2. The importance of trace analysis for practice. Trace content, particles in the atmosphere and laboratory, space cleaning. Laboratory for trace analysis, requirements for it, its equipment and operation. Other options for reducing air contamination. Chemical vessels, material, contamination and losses, cleaning, sample preparation material. 3. Reagents, methods of purification and preparation of reagents of the required purity, their storage, preparation of pure water, marking of the quality of reagents. Trace analysis problems and their effect on the result. Sampling, homogeneity of the material. Trace analysis of metals and alloys. 4. Sample stability and storage. Contamination and losses of analyte during the analytical procedure. Decompositions of inorganic samples. Autoclaves with Teflon and quartz vessels. Decomposition in the gas phase, in the liquid phase with acid distillation inside the autoclave, heterogeneous decomposition. Decomposition of biological materials. Decomposition on a wet road by mineral acids, relation to carbon content, decompositions under normal and high pressure. UV-photolysis. Autoclaves. 5. Normal and high pressure microwave decomposition systems. Low-temperature wet decomposition (Fenton's reagent). High-temperature dry combustion (ashing), classic and microwave muffle furnace, decomposition in the presence of oxygen at normal pressure and in a closed system. Apion mineralizer. Low temperature combustion, high frequency plasma. Sample drying, traditional, IR radiation and microwave energy. Enrichment techniques in trace analysis. Separation of the microcomponent from the macrocomponent and vice versa. Distillation methods, distillation of trace elements from solutions, solid and liquid samples, matrix evaporation from solutions, solid and liquid samples. Selective dissolution of trace elements and matrix. Dokimastic separation. 6. Liquid phase preconcentration. Liquid-liquid extraction, batch, continuous, reverse, extraction of chelates and ion associates, extraction of trace elements and matrix. Three-phase and homogeneous extraction. Liquid phase, single drop, hollow fiber microextraction and dispersive microextraction. Cloud point extraction, separation of metal nanoparticles. 7. Solid phase preconcentration. Solid phase extraction (SPE), procedure, sorbents, ion exchangers, chelating sorbents, ionex celluloses, polyurethane foam, activated carbon. SPE disks, nanoparticle metal oxides, biomass of microscopic filamentous fungi. Solid phase microextraction, performance, use of fiber and stir bar. SPE using carbon nanotubes and magnetic nanoparticles. 8. Flow analysis, segmented flow, FIA. Dispersion, dosing units, construction of FIA systems. Measurement of pH, ISE, dilution of samples, mineralization of samples. Preconcentration on sorbents and FIA systems. Liquid extraction in FIA, segmentor, phase separator. Precipitation systems, membrane separation. SIA. 9. Freezing and zonal melting. Precipitation, precipitation from a homogeneous environment, precipitation of matrix elements, precipitation of trace elements, collectors, carrier precipitation. Carrier precipitation and subsequent flotation, flotation cell, collectors. Ion flotation. 10. Electrochemical deposition on solid electrodes, static and flow arrangement. Coupling of electrodeposition with ET-AAS, electrodes, deposit processing, stationary arrangement with probes, flow off-line and on-line arrangement. In-situ electrodeposition of the analyte, design, dosing capillary. Deposition of trace elements on mercury electrode, spontaneous electrochemical deposition, anodic dissolution. 11. Trace analysis of organic compounds. Derivatization procedures, reactors, applications, carbon skeleton technique. "Head space" analysis, "purge and trap" technique. Gas chromatography-mass spectrometry. Infrared reflection spectroscopy, ATR, with a micromirror. Long Distance Analysis, DIAL. 12. Blank test and its meaning, log-normal distribution, limit of detection. Methods of analysis of surfaces and thin layers. Scanning electron microscopy, electron spectroscopy, scanning Auger electron microscopy, X-ray fluorescence, particle-induced X-ray emission, secondary ion mass spectrometry. Glow discharge spectrometry, laser ablation, LA-ICP-OES.

Literature

recommended literature
• Trace metal analysis and speciation. Edited by I. S. Krull. Amsterdam: Elsevier, 1991, 302 s. ISBN 0-444-88209-X. info
• MIZUIKE, Atsushi. Metody koncentrirovanija mikroelementov v neoorganičeskom analize. Moskva: Chimija, 1986, 151 s. info
• BEYERMANN, Klaus. Organic Trace Analysis. Chichester: Ellis Horwood Limited, 1984, 365 s. ISBN 0-85312-638-0. info
• Dulski T.R.: Trace elemental analysis of metals. Methods and Techniques. 1999.
• Coufalík P.: Stopová analýza kovů, 2019.

Teaching methods

Education is performed as lectures with PowerPoint presentation. Understanding of solution of trace analysis problems, preconcentration methods, flow analysis, data evaluation and the use in practical analysis is emphasized.

Assessment methods

Final assessment (at the end of semester) is by oral examination in the attendance or distance form. The exam consists in six questions, which require description and explanation of asked topic.

Language of instruction

Czech

Further Comments

Study Materials
The course can also be completed outside the examination period.
The course is taught annually.

• Enrolment Statistics (recent)
  
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