C7950 Speciation analysis

Faculty of Science
Autumn 2009
Extent and Intensity
2/0/0. 2 credit(s) (plus extra credits for completion). Type of Completion: zk (examination).
Teacher(s)
prof. RNDr. Viktor Kanický, DrSc. (lecturer)
prof. RNDr. Josef Komárek, DrSc. (lecturer)
prof. RNDr. Přemysl Lubal, Ph.D. (lecturer)
Guaranteed by
prof. RNDr. Viktor Kanický, DrSc.
Department of Chemistry – Chemistry Section – Faculty of Science
Timetable
Mon 11:00–12:50 AK1
Prerequisites
Knowledge of analytical chemistry on the level of basic courses Analytical chemistry I (C3100) and Analytical Chemistry II (C4050)
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
While finishing this course the student of chemistry master study programme will be able to understand the following analytical methods, to explain their principles and to get knowledge about their practical application.Speciation analysis is method of identification and determination of various chemical forms of certain elements in solution and solid samples or determination of its topological location there. The species can be considered as elements in oxidation state, organometalic compounds and complexes bound in various phases of the system (e.g. in soils), with bioligands (peptides, polysaccharides) and biological systems of organized structure (organelles, biomembranes, cells). Toxic and favour action of elements depends on biological, physical and chemical properties of the compounds species having the information about bioavailability of relevant metals and metaloids. Chemical, biological and toxicological properties of elements occurring as the species have impact into various field of daily life: risk assessment in environment; ecotoxicology; food industry; health and hygiene in work process; clinical chemistry and medicine; industrial analysis. Speciation analysis for determination of chemical forms of elements in solution and extracts obtained from solid samples are mostly realized by tandem techniques based on combination of on-line joining of high-efficient separation technique followed by specific element detection. Elemental speciation in solution can be also measured using electrochemical techniques, biosensors and radioanalytical methods. Topological speciation is based on application of probe measuring the interaction of focused photon or ion beam with matter. Based on acquired knowledge the student of chemistry master study programme will be able to apply an appropriate analytical technique and method for solution of particular speciation task.
Syllabus
  • 1. Introduction into subject. Sampling, treatment and storage of environmental, clinical and food samples. The work with samples for speciation analysis of biological materials. Techniques of sample preparation for the study of elemental speciation. Sample preparation for element fractionation in environmental samples, sediments, soils, aerosols, etc. 2. Separation techniques in speciation analysis. Chromatography: liquid chromatografy with reversed phases, ion-pairing chromatography, ion chromatography, size-exclusion (gel) chromatography, gas chromatography, capillary zone electrophoresis and gel electrophoresis. 3. Detection techniques I. Selective techniques of atomic optical spectrometry: atomic absorption spectrometry (AAS), atomic emission spectrometry with inductively coupled plasma (ICP-OES), OES in microwave plasma, atomic fluorescence spectroscopy (AFS). 4. Detection techniques II. Selective techniques of mass spectrometry: mass spectrometry with inductively coupled plasma (ICP-MS), plasma spectrometry with time-of-flight analyzer (TOF-MS), high-resolution ICP-MS, ESI- MS. 5. Techniques of speciation using other principles than atomic optical and mass spectroscopy: electrochemical methods of speciation, biosensors for metal ion monitoring, radioanalytical methods, perspectives of instrument development. 6. Elemental speciation I: Al, , Au, Cd, Cr, Co, Cu, Fe, Hg, Mn, Mo, Ni, Pb, Pt, Rh. 7. Elemental speciation II: As, Sb, Se, Si, Sn, Tl, V, Zn, actinoids, S, halogens. Volatile organometalic compounds of biogenic origin, metal ion complexes with humic acids, metal ion complexes with proteins. 8. Speciation elemental modelling. Theoretical base for modelling of chemical processes in solution. Application of thermodynamic and kinetic data for modelling. Thermodynamic databases. 9. Experimental methods for determination of equilibrium concentrations of species. Numerical methods for calculation of equilibrium concentrations of species and their application for species calculation under non-equilibrium and equilibrium experimental conditions. 10. Speciation modelling of elements in environment, food, clinical chemistry and medicine. Software demonstration for calculation. 11. Calibration in speciation analysis, semiquantitative speciation, (certificated) reference materials. Species bioavailability, environmental risk assessment, legislative. 12. Direct speciation in solid samples: absorption spectroscopy of fine structure in roentgen region, electron spectroscopy. Chosen topological speciation techniques: electron microprobe (EPXMA), roentgen spectrometry of secondary emission with total reflection (TRXRF), optical and mass spectrometry with glow discharge (GD-OES, GD-MS), laser ablation (LA) with ICP-MS a ICP-OES, spectroscopy of laser induced microplasma (LIPS, LIBS).
Literature
  • Handbook of elemental speciation : techniques and methodology. Edited by Rita Cornelis. Chichester: Wiley, 2003, xii, 657. ISBN 0471492140. info
  • Handbook of elemental speciation II. Species in the Environment, Food, Medicine and Occupational Health techniques and methodology. Edited by Rita Cornelis. West Sussex, England : Wiley, 2005.
  • Modelling in aquatic chemistry. Edited by Bert Allard - Ingmar Grenthe - Ignasi Puigdomenech. Paris: OECD - Organization for economic co-operation and development, 1997, liii, 724. ISBN 92-64-15569-4. info
  • STUMM, Werner and James J. MORGAN. Aquatic chemistry : chemical equilibria and rates in natural waters. New York: John Wiley & Sons, 1995, xvi, 1022. ISBN 0-471-51184-6-. info
  • PITTER, Pavel. Hydrochemie [Pitter, 1999]. 3. přeprac. vyd. Praha: Vydavatelství VŠCHT, 1999, 568 s. ISBN 80-03-00525-62. info
  • SZPUNAR, Joanna and Ryszard ŁOBIŃSKI. Hyphenated techniques in speciation analysis. Cambridge: Royal Society of Chemistry, 2003, xvi, 220. ISBN 0854045457. info
Teaching methods
lectures
Assessment methods
lecture, written test
Language of instruction
Czech
Further Comments
Study Materials
The course is taught annually.
The course is also listed under the following terms Autumn 2007 - for the purpose of the accreditation, Autumn 2010 - only for the accreditation, Autumn 2005, Autumn 2006, Autumn 2007, Autumn 2008, Autumn 2010, Autumn 2011, Autumn 2011 - acreditation, Autumn 2012, Autumn 2013, Autumn 2014, Autumn 2015, Autumn 2016, Autumn 2018, Autumn 2019, Autumn 2020, autumn 2021, Autumn 2022, Autumn 2023, Autumn 2024.
  • Enrolment Statistics (Autumn 2009, recent)
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