Fast GC-analysis of selected organic compounds at trace levels with the novel RAPID-MS/MS-technology

The main topic of the present thesis was the development of rapid analytical procedures for the environmental analysis of a steel producing company, to speed up the sample throughput for the daily routine work. Additionally, high precision of analysis results was requested. This brought a certain effort concerning the validation of the results which was supported by the analysis of certified reference materials. Special interest was laid on the optimization of the trace analysis of dioxins and furans (PCDD/DF). An expansion of the established methods with powerful techniques like single ion storage and tandem-mass spectrometry resulted in an obvious improvement of the limits of quantitation and the reliability of analysis. Further advances could be achieved with the simplification of the clean-up procedure by the application of a new sampling technique which reduced the demand on sample preparation time as well. Analysis were also carried out with brominated Dioxins and Furans (PBrDD/DF). The next item focused on the analysis of polycyclic aromatic hydrocarbons (PAH) with the implementation of five new representatives with a highly carcinogenic potential. In this case, the coupling of three detectors resulted in a robust and precise HPLC-method with a highly qualitative and quantitative analytical reliability. Furthermore, the aim was to promote the routine analysis of alkylated aromatics (BTEX) and halogenated volatile organic (VOC) compounds. By the use of gas chromatography coupled with mass spectrometric detection a common analytical technique for both classes of substances could be found with an enhancement of sensitivity due to application of the single ion storage technique. The existing method for the determination of polychlorinated biphenyls (PCB) was improved by replacing the electron capture detector with mass spectrometry. Due to an optimization of the single ion storage and tandem mass spectrometry parameters the requested demands on low detection limits together with precise results were achieved. Nearly all of the methods mentioned above could be accelerated by the use of a new column called Rapid-MS. In most cases a reduction of analysis time by a factor of 5 to 10 was possible, but a loss of resolution has to be considered. (author)