C9053 Determination of elements in geological materials by the ICP-OES method

Faculty of Science
Spring 2022
Extent and Intensity
1/0/0. 1 credit(s) (plus extra credits for completion). Type of Completion: zk (examination).
Teacher(s)
doc. Mgr. Karel Novotný, 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
Course Enrolment Limitations
The course is offered to students of any study field.
Course objectives
The aim of the course "Determination of elements in geological materials by the ICP-OES method" is to build on the basic lecture on ICP spectrometry and make students familiar with the practical use of this method especially in connection with the analysis of geological samples. In the first part, the course will focus mainly on sampling and sample preparation, the inclusion of this technique among other methods of spectral analysis and the basic principles and possibilities of ICP OES spectrometry will be repeated. In the following part, the problem will be explained on practical examples and the demonstration of solving of various tasks directly in the laboratory on the instrument will follow (thus complementing the laboratory course "Analysis of geological samples by ICP-OES").
Learning outcomes
Upon completion of this course, students will be able to independently design a method for analysis of a specific geological sample using ICP OES spectrometry. Knowledge of basic principles and parameters of the method will allow him to critically evaluate the possibilities of determination with the estimation of detection limits, limits of determination and problems of spectral and non-spectral interferences. In practice, he should then be able, after basic training, to prepare a method on any ICP OES spectrometer for determination selected elements in a particular geological sample.
Syllabus
  • 1. Collection, treatment and storage of geological samples focused on the determination of elemental composition by ICP-OES method. Preservation of samples, prevention of hydrolysis and leakage of volatile components. Determination of physical properties - conductivity, pH, density, granularity. Problems of grinding, homogenization and sorting by particle size. Basic types of minerals and rocks, soil analysis and hydrogeology analysis.
  • 2. Different types of sample decomposition. Preparation of extracts and total decomposition. Decomposition in acid mixtures, microwave decomposition and autoclave decomposition. Dry decomposition and melting with selected fluxes. Utilization of automatic fluxer and melting with lithium metaborate. Decomposition of silicates. The problem of samples with complex matrix, separation and preconcentration. Differences in approach when determining the majority, minority and trace elements. Special requirements for specimen preparation.
  • 3. History of ICP-OES method and other analytical techniques used in geology for determination of elemental composition. Arc and spark spectrography and spectrometry. Methods for determination of average composition - flame AAS, ETV AAS, atomic emission spectrometry with microwave coupled plasma. Comparison of parameters with ICP OES. X-ray spectrometry and local analysis methods - electron microscope and LIBS laser-induced plasma spectroscopy. Mass spectrometry and determination of isotopes.
  • 4. Basic principles of ICP-OES spectrometry, instruments with various configurations, selection of radial and axial observation. Sample introduction into plasma - solution analysis (aqueous solutions and analysis of organic solvents), electrothermal vaporation ETV. Analysis of solid samples - ETV and Laser ablation.
  • 5. Generation of volatile hydrides. Sample preparation and use of various procedures and instrumentation. Commercial devices for hydride generation and their applications. Generation of other volatile compounds. Combination of ICP-OES spectrometry with separation techniques. Problems of analysis of samples with small volumes, combination with FIA analysis.
  • 6. Creation of the method in ICP OES spectrometry. Selection of appropriate emission lines and basic orientation in the database of element emission lines. Adjustment of plasma gas flow and power to plasma, Mermet test and optimization of measurement parameters. The problem of spectral and non-spectral interference. Background correction settings.
  • 7. Introduction to the iCAP 6500 Duo (Thermo) ICP-OES spectrometer - optical configuration and instrument components. Instrument capabilities, wavelength range and spectral resolution in different parts of the spectrum.
  • 8. Nebulization of solutions - concentric and cross-flow nebulizer, glass and Teflon spray chamber. iTeva and Qtegra software, advantages and disadvantages of both control software.
  • 9. Procedures in qualitative and quantitative analyses of the sample. Fast qualitative and semiquantitative analysis. Measurement in Fullframe mode, advantages and disadvantages, application possibilities. Quantitative analysis - method of the calibration curve and standard addition method. Verification of stability and matrix effects. Use of reference element. Selection and adjustment of appropriate reference element concentration and line. Signal evaluation and recalculation to the reference signal. Problems of interelement interference. Determination of rare earth elements and possibilities of using interference factors.
  • 10. Preparation of method for large samples series. Use of autosampler and dilution unit. Suitable dishes and preparation of necessary solutions (dilution and rinsing solutions). Preparation of standards and instrument calibration. Incorporation of control standards into the analyzed sequence, recalibration, control charts. Checking the autosampler and control unit for proper operation, cleaning and maintenance.
  • 11. Method validation and evaluation of results. Statistical analysis and interpretation of measured data. GLP principles accredited methods and accredited laboratory. Advanced chemometric methods. Trend tracking, case studies, reporting.
  • 12. Example of analysis of a particular geological material from sampling and treatment, selection of suitable lines and spectrometer settings to calibration and evaluation of results. Discussion of individual alternatives - wet decomposition vs. melting, solution analysis hydride generation, classical calibration vs. use of the reference signal. Evaluation of major elements, minor elements and trace elements. Evaluation of method parameters - limits of detection, range of linearity, the accuracy of the determination. Use of different procedures for evaluation and presentation of results.
  • 13. Typical problems in the practical use of ICP OES spectrometer and their solutions. Regular maintenance and service of the device. Deterioration of instrument parameters over time, causes and possible solutions. Problems of clogging of the transport route of the sample - cleaning of nebulizer and spray chamber. Optical components cleaning, plasma torch replacement.
Teaching methods
lecture, demonstration on ICP OES spectrometer
Assessment methods
written or oral examination
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 2023, Spring 2024, Spring 2025.
  • Enrolment Statistics (Spring 2022, recent)
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