C6300 Inductively Coupled Plasma Atomic Emission/Mass Spectrometry (ICP-AES, ICP-MS)

Faculty of Science
Spring 2013
Extent and Intensity
1/0/0. 1 credit(s) (fasci plus compl plus > 4). Recommended Type of Completion: zk (examination). Other types of completion: k (colloquium).
Teacher(s)
prof. RNDr. Viktor Kanický, DrSc. (lecturer)
Guaranteed by
prof. RNDr. Viktor Kanický, DrSc.
Department of Chemistry – Chemistry Section – Faculty of Science
Supplier department: Department of Chemistry – Chemistry Section – Faculty of Science
Timetable
Tue 13:00–13:50 C14/207
Prerequisites
Previous passing the subjet Atomic spectrometry C7031 is benefit but not condition
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
Course objectives
At the end of the course the student of chemistry master study programme will acquire knowledge about principles, instrumentation, analytical features and practical application of ICP-AES and ICP-MS. Student will be acquainted with processes in plasma that are important for spectrochemical analysis, sample introduction techniques, optimization of analytical procesures. For this the following tems will be explained and elucidated: High-frequency generators, plasma torches, ionization and excitation mechanisms, spatial distributions of emission, background equivalent concentration, lateral and axial ICPs. Sample introduction techniques, nebulization, generation of volatile hydrides, introduction of solids, electrothermal vaporization, spark ablation, arc evaporation, laser ablation. Emission spectrometers, monochromators, polychromators, echelle spectrometers with CTD detectors, application to analysis of materials, trends of development of plasma spectrometry; ICP mass spectrometry, ICP-MS instrumentation, spectral and non-spectral interferences in ICP-MS. Having passed this course, the student is able (after practical training) to develop and optimize analytical method ICP-AES/MS for a particular type of a sample, perform routine analysis as well as research.
Syllabus
  • 1. Role and significance of plasma spectrometry in analytical chemistry; principle and physical features of inductively coupled plasma source (ICP); ICP as a source for atomic emission spectrometry (AES), atomization medium for atomic fluorescence spectrometry (AFS) and ion source for mass spectrometry (MS); plasma torches, ICP generators; overview of sample introduction into an ICP; instrumentation for ICP optical emission spectrometry and mass spectrometry. 2. Temperatures and thermodynamic equilibrium in ICP (partial, local), excitation and ionization mechanisms, ICP-AES, atomic and molecular spectra in ICP, spectral line intensity, norm temperature,"hard" a "soft" spectral lines; analytical signal and background, background equivalent concentration, standard deviation of signal and background, limit of detection, limit of quantification; analytical features of ICP-AES, analytical feqatures of ICP-MS. 3. Axial, radial and lateral emission intensity distribution in ICP discharge, emissivity, ICP regions and zones; multiplicative (matrix) interferences, effects of easily ionizable elements (EIE), matrix interferences of acids; influence of generator frequency, power input, gas flow rates, observation height, and sample uptake (pump feed rate) on intensity, detection limits, and matrix effects spatial distribution in ICP; elimination of matrix interferences by selection of robust plasma conditions, compensation of matrix interferences by means of internal standardization; lateral and axial observation of ICP - benefits and limitations; non spectral interferences in ICP mass spectrometry. 4. Origin and classification of spectral interferences, selectivity; spectrometer, dispersion, resolution and resolving power, influence of resolving power on signal-to-background ratio and on magnitude of spectral interferences; influence of spectral interferences and their corrections on precision and accuracy of measurement, true limit of detection; algorithms of spectral interference corrections; influence of ICP operating conditions on magnitude of spectral interferences, spectral atlases; spectral interferences in ICP-MS; classification and elimination of spectral interferences in ICP-MS. 5. Noise and its sources in ICP-AES, shot noise, flicker noise, background noise, signal noise; precision of measurement, influence of signal integration time on precision of measurement, influence of signal magnitude on precision of measurement; repeatability (short-term, long-term), intermediate repeatability, reproducibility; instrumental drift, drift sources and their elimination; compensation of drift by means of internal reference methods. 6. Calibration in ICP-AES, linearity of calibration, calibration model, influence of number and distribution of calibration samples, confidence bands, calibration at solution analysis, preparation of calibration solutions, standard addition method. 7. Introduction of solutions into ICP, pneumatic nebulizers (concentric, cross flow, Babington-type, vee-groove nebulizer, grid nebulizer, fritted disc nebulizer); ultrasonic nebulizer, direct injection nebulizer, thermospray, hydraulic high-pressure nebulizer; generating, modification and transport of aerosol into ICP, nebulizer characteristics, wet and dry aerosol, electrothermal vaporization into ICP. 8. Solid sample introduction into ICP; powder and compact samples, electrically conducting and non-conducting samples, slurry nebulization, electrothermal vaporization; direct solid sample introduction (DSID - direct sample insertion device, SET - sample elevator technique); electroabrasion, electroerosion, ablation by electric spark/arc; laser ablation. 9. Introduction of gaseous samples, generating of volatile hydrides, other volatile compounds; on-line coupling of ICP with separation techniques; speciation analysis with ICP-MS and separation techniques. 10. Methodology of measuring with ICP-AES, solution preparation, determination of optimum measurement conditions, measurement with low and high signal-to-background ratios, background correction, correction of spectral interferences, checking of correction factors, error of sum of contents, normalization of contents to their sum (sum correction). 11. Plasma diagnostics, magnesium atomic and ionic lines intensity ratio as a criterion of plasma robustness, checking of nebulization, checking of energy transfer into plasma, checking of optical system, methodology of measurement, regulation diagram, analysis of check sample, current problems with ICP measurement. 12. Preparation of samples and sample decomposition for ICP spectrometry in solution analysis, decomposition methods based on fusion and acid digestion or dissolution, error sources at decomposition; preparation of samples for direct solid analysis; limitations of sample preparation techniques for ICP-MS. 13. Overview of ICP-AES and ICP-MS applications in analysis of technological materials, raw materials, in geological sciences, in environmental analysis, foodstuff, biological and clinical materials. 14. Sources of uncertainties and calculation of uncertainties at the determination by ICP-AES, evaluation of analytical results. 15. Present state and future prospects of plasma spectrometry; development of instrumentation, new excitation sources, miniaturization.
Literature
  • KANICKÝ, Viktor, Vítězslav OTRUBA, Lumír SOMMER and Jiří TOMAN. Optická emisní spektrometrie v indukčně vázaném plazmatu a vysokoteplotních plamenech (Optical emission spectrometry in inductiveky coupled plasma and high temperature flames). 1. st. Praha: Academia, 1992, 152 pp. Pokroky chemie 24. ISBN 80-200-0215-4. info
  • TAYLOR, Howard E. Inductively coupled plasma-mass spectrometry : practices and techniques. San Diego: Academic Press, 2001, xi, 294. ISBN 0126838658. info
  • Inductively coupled plasmas in analytical atomic spectrometry. Edited by Akbar Montaser - D. W. Golightly. 2nd ed. Hoboken, N.J.: Wiley-VCH, 1992, xxii, 1017. ISBN 1560815140. info
  • Inductively coupled plasma mass spectrometry handbook. Edited by Simon M. Nelms. 1st pub. Oxford: Blackwell Publishing, 2005, xv, 485. ISBN 1405109165. info
Teaching methods
lectures
Assessment methods
oral examination
Language of instruction
Czech
Further Comments
Study Materials
The course is taught annually.
The course is also listed under the following terms Spring 2008 - for the purpose of the accreditation, Spring 2011 - only for the accreditation, Spring 2000, Spring 2001, Spring 2002, Spring 2003, Spring 2004, Spring 2005, Spring 2006, Spring 2007, Spring 2008, Spring 2009, Spring 2010, Spring 2011, Spring 2012, spring 2012 - acreditation, Spring 2014, Spring 2015, Spring 2016, Spring 2017, spring 2018, Spring 2019, Spring 2020, Spring 2021, Spring 2022, Spring 2023, Spring 2024, Spring 2025.
  • Enrolment Statistics (Spring 2013, recent)
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