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Advanced environmental contaminant analytics: extraction, SPME method, and trouble shooting in chromatography

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Time: May 3 - 12, 2006

Place: University of Kuopio, Kuopio (Maps and connections)

Tietoteknia (the building number 13 on the map)

Medistudia (the building number 3 on the map)

Canthia (the building number 1 on the map)

Bioteknia (the building number 14 on the map)

Melania (the building number 6 on the map)

Snellmania (the building number 5 on the map)

National Public Health Institute (KTL), Neulaniementie 4, Kuopio

Credits: 3.0 credit points

Language: English (and/or Finnish)

Organizer: The course is organized jointly by the Graduate school in Environmental Health and Environmental Risk Assessment Centre (ERAC).

Course leader: Anne Korpi, PhD, Dept. of Environmental Sciences, University of Kuopio

Course description:

The course will cover several aspects of the analysis of environmental contaminants in air and water matrixes.

The topics include liquid-chromatography (LC-MS), gas chromatography (GC-MS), practical solutions in chromatographic problems, typical sources of errors in chromatographic analysis, choice of columns, detectors, preparation and use of standards. Another focus lies in the extraction processes, especially Accelerated solvent extraction (ASE) and its comparison to supercritical fluid extraction (SFE), sonication, and solid phase extraction (SPE) in addition to the handling of the extracts (such as drying, cleaning, fractioning) prior to the analysis. Finally, the third aspect of the course deals with solid phase microextraction (SPME). This method utilizes a small segment of fused silica fibre coated with an appropriate material and mounted on syringe-like device for extraction of analytes from various matrices and introduction to a chromatographic system. No solvents are used in the process. Analyte extraction and pre- concentration are combined in a single step.

Lecturers:

Asst. Prof. Jacek Koziel, Iowa State University, Air Quality Engineering and Livestock Odor, Agricultural & Biosystems Engineering Dept., National Swine Research & Information Center, Ames, USA

Prof. Marja-Liisa Riekkola, University of Helsinki, Laboratory of Analytical Chemistry

Docent Jaana Koistinen, National Public Health Institute, Kuopio

PhD Panu Rantakokko, National Public Health Institute, Kuopio

Examination:

The first exam will be arranged on 2nd June, 2006 and the last exam 30th June, 2006.

  • Friday 2nd June, 2006 (8-12 a.m.). Place: University of Kuopio, Snellmania building, Room SL. Please, register for the exam by 26th May, 2006.
  • Friday 30th June, 2006 (9-13 a.m.). Place: Room SL. Please, register for the exam by 21st June, 2006.


Further information: Sari.Makkonen(at)uku.fi, Tel. +358-17-163188


Time schedule:


DateLecture
May, 3
Medistudia, MR10
9.15-12.00Section I: Chromatography Prof. Riekkola
  • Theoretical aspects
  • GC and HPLC, band broadening, optimisation of instrumental parameters affecting separations (columns; stationary phase, film thickness, diameter etc. in GC, and stationary phase, particle size, porosity etc. in LC)
  • LC-MS, ionization techniques and mass analysers
  • Choice of columns and detectors
  • Quantitative analysis
  • Problem solving
13.15-14.00Section I
Canthia, MC2
14.15-16.00E1: Choice of a GC column
May 4
Medistudia, MS1
9.15-12.00Section I
14.15-15.00Section I
15.00-16.00E1: Choice of a GC column
May 8
Tietoteknia, 1038
9.15-12.00Section II: SPME Prof. Koziel
  • Introduction to SPME
  • Theoretical principles of SPME and quantitation
  • Method development
  • Selected aspects of GC analysis for SPME
  • SPME applications especially in environmental analysis (water and air samplings)
  • Future directions
13.15-14.00Section II
Snellmania, Sn 3020/3027
14.15-17.00E2/Group 1: GC-MS
May 9
Snellmania, Sn 3020/3027
8.15-11.00E2/Group 2: GC-MS
Tietoteknia, 1038
12.15-13.00Ordior Product group manager Teuvo Joki from Ordior Ltd will give a presentation on products relevant to this course topic.
13.15-15.00Section II
May 10
Tietoteknia, 1038
9.15-11.00Section II
Snellmania, Sn 3020/3027
12.00-15.00E2/Group 3: GC-MS
Bioteknia 2, Room B2440
15.15-16.00Prof. Koziel's general lecture The Research Seminars of Dept of Environmental Sciences: Prof. Koziel will give a general lecture on their research at the Iowa State University. The title of the lecture is " Finding stinky 'needles' in the chemical 'haystack' of livestock odor: towards solving livestock odor problems with SPME and multidimensional GC-MS-O"
May 11
Melania, S31
9.15-10.00E2/all
10.15-12.00Section III: Extraction and handling of extracts Dr Rantakokko and Docent Koistinen
  • Introduction to extraction methods (Soxhlet, SPE, sonication)
  • Cleanup and other handling procedures in conventional environmental analysis (PCDD/PCDFs, PCBs)
  • Principles of ASE - theory and instrumentation
  • ASE applications in environmental analysis (PCDD/PCDFs, PCBs)
  • Comparison of Soxhlet and ASE
  • Principles of SFE - theory and instrumentation
  • SFE applications in environmental analysis (PCDD/PCDFs, PCBs)
13.15-14.00Section III
KTL
14.15-15.00E3/Group 1: LC-MS
May 12
KTL
9.15-10.00E3/Group 2: LC-MS
10.15-11.00E3/Group 3: LC-MS
Snellmania, S27
12.15-13.00Section III
13.15-14.00Summary of the course, Feedback


Exercises:

E1: Choice of a GC column. 3 h. (Marja-Liisa Riekkola)

Theoretical exercises with artificial sample mixtures including environmentally important compounds with different physicochemical properties.

E2: GC-MS. Demonstration. 3 h + summary lecture 1 h. (Marko Hyttinen, Jacek Koziel, Juhani Tarhanen)

SPME sample collection and analysis: a) Headspace extractions of benzene, toluene, xylene and ethylbenzene (BTEX) from water. b) Air sampling and analysis of laboratory/ classroom air.

E3: LC-MS, Extraction, clean-up & fractionating. Demonstration. 1 h. (Tuomo Korhonen, Panu Rantakokko)

LC-MS: Schematic and concrete presentation of LC-MS-MS instrument with electrospray interface. Sample pretreatment, HPLC-solvents, system equilibration, compound separation, ionization, fragment ions and chromatograms.

ASE: Sample pretreatment, fat extraction with ASE, determination of fat content, fat removal on sulphuric acid silica with ASE, further cleanup and fractionation of PCBs and PCDD/Fs with tandem aluminum oxide and carbon columns. If time allows, GC-MS analysis of PCBs and PCDD/Fs.

Kurssimateriaali:





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