Instrumental Methods of Analysis

This course is part of the programme
Bachelor's programme in Environment (first cycle)

Objectives and competences

To give basic knowledge on instrumental methods of chemical analysis and train students to perform practical work on real samples to get acquainted with instrumentation and equipment which is needed in monitoring of environmental pollution and in investigating current environmental processes.

Prerequisites

Required knowledge of general chemistry, physics and selected topics of mathematics (in particular of functions, derivatives) and statistics.

Content

  • Sampling and sample preparation: handling, treatment and storage of samples prior to analysis, methods of purification and pre-concentration.

  • Measurement uncertainties, error propagation, standards, reference materials

  • Spectroscopic methods:
    • Absorption spectrometry (UV-Vis, NIR and IR spectrometry, AAS, ET-AAS)
    • Emission spectrometry (fluorescence, luminiscence, XRF)
    • Mass spectrometry

  • Electrochemical methods:
    • Ion selective and reference electrodes (glass, fluoride, metal ions, H2, calomel and Ag/AgCl electrodes …)
    • Voltametric methods (polarography)

  • Separation methods:
    • Liquid chromatography (HPLC, HPLC-MS, ion chromatography)
    • Gas chromatography (GC, GC-MS)
    • Electrophoresis

  • Radioanalytical methods: spectrometry α, β, γ; scintillation methods; radioisotopes and radiodating, neutron activation analysis

  • Bioanalytical methods: radioimmunological tests biosensors.
    • Continuous and automated methods
    • Automatic sampling
    • Flow injection analysis

  • Continuous and semi-continuous methods for determination of atmospheric pollutants

  • Instrumentation for field measurements

  • LABORATORY PRACTICE
    • Sampling and determination of physico-chemical parameters of soil and water,
    • spectrophotometric determination of chromate by DPC method,
    • Determination of metals in soil by AAS in ET-AAS
    • Determination of lead by ion-selective electrode
    • Determination of anions in water by ion chromatography,
    • Determination of neonicotinoids by HPLC
    • Determination of trihalomethanes by gas chromatography with ECD and MS detection
    • Measurements of Rn-222 by scintillation cells and alpha spectrometry,
    • Determination of toxicity of organophosphorous pesticides by biosensors and flow injection analysis
    • Semi-continuous measurements of NO2 concentration in atmosphere

Intended learning outcomes

Knowledge and understanding:
• Proficiency in professional sampling and sample treatment prior to analysis
• Capability of treatment and evaluation of the results of analysis
• Understanding and capability of performing basic chemical processes in an analytical laboratory
• Capability of peforming measurements on basic analytical instruments (photometers, spectrometers, chromatographs, ion-selective electrodes)

Readings

• OORT, Pouline M. van, WHITE, Iain R., AHMED, Waqar, JOHNSON, Craig, BANNARD-SMITH, Jonathan, FELTON, Timothy, BOS, Lieuwe D., GOODACRE, Royston, DARK, Paul, FOWLER, Stephen J. Detection and quantification of exhaled volatile organic compounds in mechanically ventilated patients : comparison of two sampling methods. Analyst, ISSN 1364-5528, 2021, vol. 146, no. 1, str. 222-231, ilustr. https://doi.org/10.1039/C9AN01134J, E-version
• BEALE, David J., JONES, Oliver A. H., KARPE, Avinash V., OH, Ding Y., WHITE, Iain R., KOUREMENOS, Konstantinos A., PALOMBO, Enzo A. Breathomics and its application for disease diagnosis : a review of analytical techniques and approaches. V: CUMERAS, Raquel (ur.). Volatile organic compound analysis in biomedical diagnosis applications. Oakville; Waretown: Apple Academic Press. cop. 2018, str. 159-194, ilustr.
• SONDERFELD, Hannah, WHITE, Iain R., GOODAL, Iain C. A., HOPKINS, James R., LEWIS, Alastair C., KOPPMANN, Ralf, MONKS, P. S. What effect does VOC sampling time have on derived OH reactivity?. Atmospheric chemistry and physics, ISSN 1680-7316, May 2016, vol. 16, iss. 10, str. 6303-6318, ilustr. https://doi.org/10.5194/acp-16-6303-2016. E-version
• CORDELL, Rebecca L., WHITE, Iain R., MONKS, Paul S. Validation of an assay for the determination of levoglucosan and associated monosaccharide anhydrides for the quantification of wood smoke in atmospheric aerosol. Analytical and bioanalytical chemistry, ISSN 1618-2642, 2014, vol. 406, no. 22, str. 5283-5292, ilustr. https://doi.org/10.1007/s00216-014-7962-x. E-version
• BARBER, Shane, BLAKE, Robert S., WHITE, Iain R., MONKS, P. S., REICH, Fraser, MULLOCK, Steve, ELLIS, Andrew Michael. Increased sensitivity in proton transfer reaction mass spectrometry by incorporation of a radio frequency ion funnel. Analytical chemistry, ISSN 0003-2700. [Print ed.], 2012, vol. 84, no. 12, str. 5387-5391, ilustr. https://doi.org/10.1021/ac300894t. E-version
• PRADHAN, M., LINDLEY, R. E., GRILLI, R., WHITE, Iain R., MARTIN, Damien, ORR-EWING, A. J. Trace detection of C2H2C2H2 in ambient air using continuous wave cavity ring-down spectroscopy combined with sample pre-concentration. Applied physics. B, Lasers and optics, ISSN 0946-2171. Tiskana izd., 2008, vol. 90, iss. 1, str. 1-9, ilustr. https://doi.org/10.1007/s00340-007-2833-1. E-version

Assessment

Test in laboratory practice (50 %), written exam (25 %), oral exam (25 %).

Lecturer's references

Assistant Professor of Chemistry at the University of Nova Gorica

  • OORT, Pouline M. van, WHITE, Iain R., AHMED, Waqar, JOHNSON, Craig, BANNARD-SMITH, Jonathan, FELTON, Timothy, BOS, Lieuwe D., GOODACRE, Royston, DARK, Paul, FOWLER, Stephen J. Detection and quantification of exhaled volatile organic compounds in mechanically ventilated patients : comparison of two sampling methods. Analyst, ISSN 1364-5528. [Online ed.], 2021, vol. 146, no. 1, str. 222-231, ilustr. https://doi.org/10.1039/C9AN01134J, doi: 10.1039/C9AN01134J.

  • BEALE, David J., JONES, Oliver A. H., KARPE, Avinash V., OH, Ding Y., WHITE, Iain R., KOUREMENOS, Konstantinos A., PALOMBO, Enzo A. Breathomics and its application for disease diagnosis : a review of analytical techniques and approaches. V: CUMERAS, Raquel (ur.). Volatile organic compound analysis in biomedical diagnosis applications. Oakville; Waretown: Apple Academic Press. cop. 2018, str. 159-194, ilustr.

  • SONDERFELD, Hannah, WHITE, Iain R., GOODAL, Iain C. A., HOPKINS, James R., LEWIS, Alastair C., KOPPMANN, Ralf, MONKS, P. S. What effect does VOC sampling time have on derived OH reactivity?. Atmospheric chemistry and physics, ISSN 1680-7316, May 2016, vol. 16, iss. 10, str. 6303-6318, ilustr., doi: 10.5194/acp-16-6303-2016.

  • CORDELL, Rebecca L., WHITE, Iain R., MONKS, Paul S. Validation of an assay for the determination of levoglucosan and associated monosaccharide anhydrides for the quantification of wood smoke in atmospheric aerosol. Analytical and bioanalytical chemistry, ISSN 1618-2642, 2014, vol. 406, no. 22, str. 5283-5292, ilustr., doi: 10.1007/s00216-014-7962-x.

  • BARBER, Shane, BLAKE, Robert S., WHITE, Iain R., MONKS, P. S., REICH, Fraser, MULLOCK, Steve, ELLIS, Andrew Michael. Increased sensitivity in proton transfer reaction mass spectrometry by incorporation of a radio frequency ion funnel. Analytical chemistry, ISSN 0003-2700. [Print ed.], 2012, vol. 84, no. 12, str. 5387-5391, ilustr., doi: 10.1021/ac300894t. [COBISS.SI-ID 5420283],

  • PRADHAN, M., LINDLEY, R. E., GRILLI, R., WHITE, Iain R., MARTIN, Damien, ORR-EWING, A. J. Trace detection of C2H2C2H2 in ambient air using continuous wave cavity ring-down spectroscopy combined with sample pre-concentration. Applied physics. B, Lasers and optics, ISSN 0946-2171. Tiskana izd., 2008, vol. 90, iss. 1, str. 1-9, ilustr., doi: 10.1007/s00340-007-2833-1.