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Determination of polar, low-molecular-weight microcontaminants in aqueous samples using micro liquid chromatography interfaced with gc detection and eluent-jet mass spectrometry


Research objectives and content
Concern about environmental problems, i.e. the ubiquitous presence of toxic micro-contaminants, has led to the rapid development of adequate analytical procedures. Many methods are available today to determine organic micro pollutants at the levels required by the European Union. However, much less attention has been paid to the (bio)degradation products of the parent compounds, and the present knowledge about these almost invariably polar, low-molecular-weight compounds, and their analysis is sadly inadequate. These compounds are especially interesting, because (i) trace enrichment using conventional approaches still is rather difficult due to early breakthrough and interferences caused by, e.g. humic substances, (ii) detection is often problematic because of poor UV-absorbance or fluorescence characteristics. Attention will therefore be directed at (i) novel trace-enrichment procedures using suitably modified sorbents and/or a dual-precolumn set-up, (ii) micro-LC separation conditions compatible with the modes of detection to be developed, and (iii) detection either by modified GC detectors such as the thermionic or nitrogen phosphorus detector (NPD), the (pulsed) flame photometric (FPD) detector, or (tandem) mass spectrometry (MS). In the latter case, a novel eluent-jet interface will be tested. The total analytical system will be based on at-line/on-line combinations of the SPE procedure and the LC-cum-detection modules. The practicality will be demonstrated by analysing real-life problems; one of these will be the suspected presence of acrylamide in many Swedish water courses. Other analytes of interest will be pesticides and their transformation products.
Training content (objective, benefit and expected impact)
During the 36-month-period, several new analytical techniques will be used by the candidate. Regarding sample enrichment, a dual-precolumn set-up will be tested for the removal of interfering compounds on the first, and selective enrichment of the polar analytes of interest on the second precolumn. Regarding interfacing techniques the candidate will be trained in the laboratory of dr. Ch.E. Kientz at TNO (Prins Maurits Laboratory, Rijswijk. The Netherlands). Miniaturisation will be studied at LC Packings (Amsterdam, The Netherlands). The present knowledge of the candidate with regard to GC detectors and MS detection for LC is insufficient and will be improved by her attending relevant courses. Working with the proposed techniques and the new theoretical aspects will enlarge the candidate's theoretical view. Introduction into the use of the various coupled-column and hyphenated techniques will be combined with an adequate theoretical training. In addition, the practical relevance of the novel techniques and procedures will, in all cases, be demonstrated by analysing real-life samples.
Links with industry / industrial relevance (22)
See description of the host institute.


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