A technique to alter the morphology of the inner surface of fused silica capillaries has been developed. The internal surface area is enlarged by means of nano-wires of silica, which are grown from the capillary walls. The growth is initiated by the decomposition of the etchant precursor 2-chloro-1,1,2–trifluoroethylmethyl ether at elevated temperature and pressure. It is suggested that the formation of the nano-wires is a process where hydrogen fluoride is continuously consumed and re-liberated. The amorphous bulk silica wall is dissolved, vaporized and finally condensed, yielding a directional re-formation of silica into nano-wire structures. The unidirectional growth of the nano-wires seems to follow the well-known vapor-liquid-solid (VLS) mechanism since characteristic attributes of the VLS mechanism can be observed in the modified capillaries, such as spherical particles terminating each nano-wire. An alternative procedure was developed based on non-isothermal etching which enabled nano-wire outgrowth in fused silica capillaries with internal diameters exceeding 5 µm. The etched and modified capillaries are expected to be suitable for fluidic applications where a higher surface-to-volume ratio is beneficial, such as open tubular liquid chromatography as well as solid-phase micro-reactors and catalysis including enzymatic reactions. The last part of the thesis describes new techniques developed for matrix-assisted laser desorption/ionization (MALDI) mass spectrometry. A set of novel matrices based on polymers/oligomers of benzodioxins and thiophenes has been introduced. Using this approach, which has been given the name Polymer-Assisted Laser Desorption/Ionization (PALDI), the low m/z-range of the mass spectrum, from 180 to 1.000 Da, could be used without the abundant chemical noise which normally disturbs such MALDI-MS spectra. Some of the PALDI matrices also showed excellent behavior in the analysis of low molecular weight polymers. A methodology based on non-linear regression of cumulative frequency distributions in polymers has been developed to compare and evaluate different matrix/polymer/cation agent sample combinations for MALDI and PALDl-MS analyses of low molecular weight polymers.
| Identifer | oai:union.ndltd.org:UPSALLA1/oai:DiVA.org:kth-79 |
| Date | January 2004 |
| Creators | Woldegiorgis, Andreas |
| Publisher | KTH, Kemi, Stockholm : Kemi |
| Source Sets | DiVA Archive at Upsalla University |
| Language | English |
| Detected Language | English |
| Type | Doctoral thesis, comprehensive summary, info:eu-repo/semantics/doctoralThesis, text |
| Format | application/pdf |
| Rights | info:eu-repo/semantics/openAccess |
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