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Previous studies of the hyphenation of gas chromatographic separation and spectrophotometric detection in the ultraviolet wavelength range between 168 and 330 nm showed a high potential for applications where the analysis of complex samples is required. Within this paper the development of a state-of-the-art detection system for compounds in the vapour phase is described, offering an improved behaviour compared to previous systems: Dependent on the requirements of established detection systems hyphenated with gas chromatography, the main components of the system have to be designed for optimum performance and reliability of the spectrophotometric detector: A deuterium lamp as a broadband light source has been selected for improved stability in the measurements. A new-type absorption cell based on fiber-optics has been developed considering the dynamic necessary to compete with existing techniques. In addition, the influence of the volume of the cell on the chromatogram needs to be analyzed. Tests for determining the performance of the absorption cell in terms of chemical and thermal influences have been carried out. A new spectrophotometer with adequate spectral resolution in the wavelength range, offering improved stability and dynamic for an efficient use in this application was developed. Furthermore, the influence of each component on the performance, reliability and stability of the sensor system will be discussed. An overview and outlook over the potential applications in the environmental, scientific and medical field will be given.
In thin-layer chromatography, fiber-bundle arrays have been introduced for spectral absorption measurements in the UV-region. Using all-silica fiber bundles, the exciting light will be detected after re-emission on the plate with a fiberoptic spectrometer. In addition, fluorescence light can be detected which will be masked by the re-emitted light. Therefore, it is helpful to separate the absorption and fluorescence on the TLC-plate. A modified three-array assembly has been developed: using one array for detection, the two others are used for excitation with broadband band deuterium-light and with UV-LEDs adjusted to the substances under test. As an example, the quantification of glucosamine in nutritional supplements or spinach leaf extract will be described. Using simply heating of the amino-plate for derivation, the reaction product of Glucosamine can be detected sensitively either by light absorption or by fluorescence, using the new fiber-optic assembly. In addition, the properties of the new 3-row fiber-optic array and the commercially available UV-LEDs will be shown, in the interesting wavelength region for excitation of fluorescence, from 260 nm to 360 nm. The squint angle having an influence on coupling efficiency and spatial resolution will be measured with the inverse farfield method. Some properties of UV-LEDs for analytical applications will be described and discussed, too.
Non-esterified plant oils gain ecological and economical importance, particularly in the EU where it is intended to increase the share of renewable energies. Plant oils do not require any chemical treatment so do not cause secondary pollution. The importance of plant oil will increase in Germany for mobile and stationary applications. The generation co-generation of heat and power is subsidized by the German “Erneuerbares Energiegesetz” and the “Kraft-Wärme-Kopplungsgesetz” when renewable fuels are used such as plant oils..
Plant oils have a much higher viscosity than conventional gas oil. It is mandatory to decrease the oil viscosity by heating prior to injection to assure proper injection and to avoid engine damage due to coke formation in the combustion chamber and at the injection nozzle. The German quality standard of Weihenstephan (RK-Qualitätsstandard 05/2000) for rape seed oil should be followed for use as diesel fuel. The chemical composition of plant oils is appreciably different in comparison to diesel fuels derived from mineral oils suggesting also different emission behavior.
The identification and quantification of compounds in the gas phase becomes of increasing interest in the context of environmental protection, as well as in the analytical field. In this respect, the high extinction coefficients of vapours and gases in the ultraviolet wavelength region allow a very sensitive measurement system. In addition, the increased performance of the components necessary for setting up a measurement system, such as fibres, light sources and detectors has been improved. In particular the light sources and detectors offer improved stability, and the deep UV performance and solarisation resistance of fused silica fibres allow have been significantly optimized in the past years. Therefore a compact and reliable detection system with high measuring accuracy is developed. Within this paper possible applications of the system under development and recent results will be discussed.
Soot particles emitted from a light duty (LD) Volkswagen diesel engine running at different operating points (speed and torque levels) are analyzed for mean size determination using a laser‐based three Wavelength Extinction Method (3‐WEM). For this reason, collected soot samples are suspended using an appropriate sample preparation technique with optimized conditions of sonication as it revealed its effect on the soot mean particle size measured by 3‐WEM.
An online Scanning Mobility Particle Analyzer (SMPS) is also used to measure soot emission at identical engine operating points. Size values obtained from SMPS are lower than those of suspended soot samples obtained from 3‐WEM. The size discrepancies are mainly related to the required sample preparation procedure employed for 3‐WEM measurements. The engine operating points affect, differently, the size measurements obtained from SMPS and 3‐WEM.
Sedimentation Field‐Flow Fractionation (SdFFF) is used for density determination of soot samples based on size measurements of fractions collected at peak maxima of fractograms using the off‐line hyphenation with 3‐WEM. It is assumed that a size dependent separation of soot particles occurred with a uniform particle density over the whole size distribution. An average density value is used for the conversion of soot fractograms to size distributions. Discrepancies are also found with size distribution profiles obtained from SMPS for the same engine operating points, due to the sample preparation procedure employed for SdFFF measurements.
The identification and quantification of compounds in the gas phase becomes of increasing interest in the context of environmental protection, as well as in the analytical field. In this respect, the high extinction coefficients of vapours and gases in the ultraviolet wavelength region allow a very sensitive measurement system. In addition, the increased performance of the components necessary for setting up a measurement system, such as fibres, light sources and detectors has been improved. In particular the light sources and detectors offer improved stability, and the deep UV performance and solarisation resistance of fused silica fibres allow have been significantly optimized in the past years. Therefore a compact and reliable detection system with high measuring accuracy is developed. Within this paper possible applications of the system under development and recent results will be discussed.