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Zusammenfassung:
Being the most important part in the energy supply chain, crude oil is one of the most important resources for our technology-driven society. Although strong efforts are undertaken to gain energy out of renewable resources, it is certain that crude oil will be needed at least for the next couple of decades as feedstock for transportation fuels, as raw material for the chemical industry and for a number of other different applications. The respective products need to be produced constantly in an environmentally friendly and economical way, even though feedstocks are continuously changing. Analytical chemistry is of particular importance here, as a detailed analysis can help understanding numerous adverse effects during production. The comprehensive analysis of crude oil, however, is a problematic task. Over the last years it has been shown that no single analytical technique exists that allows a complete description of a crude oil. However, ultra-high resolving Fourier transform mass spectrometry (FTMS) has developed into the method of choice to gain information on a molecular level. One major problem is the complexity of the sample which leads to suppression effects during ionization and overall sensitivity issues. Crude oil is thus “sabotaging” its own analysis.
Aim of this work was the development of methods that allow a simplification of the sample and thus help analyte detection by reducing discrimination and suppression effects. This has been achieved by hyphenating FTMS to separation techniques such as ion mobility spectrometry (FAIMS) and ligand exchange chromatography (LEC). A new source block for 1- and 2-photon ionization with FAIMS-FTMS was developed that allows also the studying of non-polar analytes. Details of the structural composition of individual components in very complex crude oil samples were investigated by detecting structural motifs in different isomeric compounds.
A group-selective analysis of sulfur containing compounds was offered through the development of a LEC separation method on a Pd-based stationary phase. The application of this method solves one of the most glaring problems in petroleum research: The quantitative analysis of individual compounds within a complex crude oil sample. This had not been possible before due to unresolved response issues. This problem was addressed by selective detection with uniform response using ICP-MS/MS. The combination of class selective separation and qualitative analysis of sulfur containing compounds by LEC-FTMS with quantitative analysis by LEC-ICP-MS/MS allowed the quantitative analysis of different sulfur containing compounds in crude oil for the first time.
