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An algorithm is presented that has successfully been utilized in practice for several years. It improves data analysis in chromatography. The program runs in an extremely reliable way and evaluates chromatographic raw data with an acceptable error. The algorithm requires a minimum of preliminaries and integrates even unsmoothed noisy data correctly.
Shapes and structures of vortex breakdown phenomena in rotating fluids are visualized. We investigate the flow in a cylindrical container and in a cone between two spherical surfaces. The primary swirling flow is induced by the rotating upper disk in the cylindrical case and by the lower boundary in the spherical case. The upper surface can be fixed with a no slip condition or can be a stress-free surface. Depending on these boundary conditions and on the Reynolds number novel structures of recirculation zones are realized. Experiments are done to visualize the topological structure of the flow and to determine their existence range as function of the geometry and rotation rate. A comparison between the experimental and theoretical approach shows a good agreement in respect to the topological structures of the flows.
Rotating flow systems are often used to study stability phenomena and structure developments. The closed spherical gap problem is generalized into an open flow system by superimposing a mass flux in meridional direction. The basic solutions at low Reynolds numbers are described by analytical methods. The nonlinear supercritical solutions are simulated numerically and realized in experiments. Novel steady and time-dependent modes of flows are obtained. The extensive results concern the stability behaviour, non-uniqueness of supercritical solutions, symmetry behaviour and transitions between steady and time-dependent solutions. The experimental investigations concern the visualization of the various instabilities and the quatitative description of the flow structures including the laminar-turbulent transition. A comparison between theoretical and experimental results shows good agreement within the limit of rotational symmetric solutions from the theory.
In this paper a high-performance thin-layer chromatography (HPTLC) scanner is presented in which a special fibre arrangement is used as HPTLC plate scanning interface. Measurements are taken with a set of 50 fibres at a distance of 400 to 500 μm above the HPTLC plate. Spatial resolutions on the HPTLC plate of better than 160 μm are possible. It takes less than 2 min to scan 450 spectra simultaneously in a range of 198 to 610 nm. The basic improvement of the item is the use of highly transparent glass fibres which provide excellent transmission at 200 nm and the use of a special fibre arrangement for plate illumination and detection.
High performance thin layer chromatography (HPTLC) is a frequently used separation technique which works well for quantification of caffeine and quinine in beverages. Competing separation techniques, e.g. high-performance liquid chromatography (HPLC) or gas chromatography (GC), are not suitable for sugar-containing samples, because these methods need special pretreatment by the analyst. In HPTLC, however, it is possible to separate ‘dirty’ samples without time-consuming pretreatment, because disposable HPTLC plates are used. A convenient method for quantification of caffeine and quinine in beverages, without sample pretreatment, is presented below. The basic theory of in-situ quantification in HPTLC by use of remitted light is introduced and discussed. Several linearization models are discussed.
A home-made diode-array scanner has been used for quantification; this, for the first time, enables simultaneous measurements at different wavelengths. The new scanner also enables fluorescence evaluation without further equipment. Simultaneous recording at different wavelengths improves the accuracy and reliability of HPTLC analysis. These aspects result in substantial improvement of in-situ quantitative densitometric analysis and enable quantification of compounds in beverages.
A new diode-array scanner in combination with a computer-controlled application system meets all the demands of modern HPTLC measurement. Automatic application, simultaneous measurements at different wavelengths, and different linearization models enable appropriate evaluation of all analytical questions. The theory of error propagation recommends quantification at reflectance values smaller than 0.8; this can be verified only by use of diode-array scanning. The same theory also recommends quantification by use of peak height data, because the theory predicts best precision only for peak height evaluation. Diode-array scanning with reflectance monitoring enables appropriate validation in TLC and HPTLC analysis. All these aspects result in substantial improvement of in-situ quantitative densitometric analysis, and simultaneous recording at different wavelengths opens the way for chemometric evaluation, e.g. peak purity monitoring, which improves the accuracy and reliability of HPTLC analysis.
A systematic toxicological analysis procedure using high-performance thin layer chromatography in combination with fibre optical scanning densitometry for identification of drugs in biological samples is presented. Two examples illustrate the practicability of the technique. First, the identification of a multiple intake of analgesics: codeine, propyphenazone, tramadol, flupirtine and lidocaine, and second, the detection of the sedative diphenhydramine. In both cases, authentic urine specimens were used. The identifications were carried out by an automatic measurement and computer-based comparison of in situ UV spectra with data from a compiled library of reference spectra using the cross-correlation function. The technique allowed a parallel recording of chromatograms and in situ UV spectra in the range of 197–612 nm. Unlike the conventional densitometry, a dependency of UV spectra by concentration of substance in a range of 250–1000 ng/spot was not observed.
Ozon-Querempfindlichkeit bei der Immissionsmessung von schwebstaubakkumuliertem Benzo[a]pyren
(2002)
Für die Beschreibung der Belastung der Luft mit polycyclischen aromatischen Kohlenwasserstoffen (PAK) wird vorwiegend die Konzentration eines Vertreters, das auf Schwebstaub akkumulierte Benzo[a]pyren (BaP), analysiert. Hierbei stellt Benzo[a]pyren die Leit komponen te für die Stoffklasse der PAK dar. Auf europäischer Ebene ist vorgesehen, für diesen Luftinhaltsstoff einen Grenzwert als Jahresmittelwert festzulegen. Deshalb wird bei bei der Normungsbehörde CEN zurzeit eine Europäische Norm für diesen Stoff erarbeitet. Aus der Literatur ist bekannt, dass für Benzo[a]pyren eine Querempfindlichkeit gegen Ozon und NO2 besteht. Im Zuge der Neuentwicklung eines Probenahmekopfs (PNK) für PAK-Immissionsmessungen, der durch den Einsatz eines Ozon- Scrubbers eine ozonfreie Immissionsmessung der Benzo[a]pyren-Konzentration ermög licht, wurde in dieser Arbeit die prinzipielle Einsetzbarkeit dieses Probe nahmekopfs geprüft. Zu diesem Zweck wurden Voruntersuchungen und Feldversuche durchgeführt, mit dem Ziel, Kenntnisse über die Ozon-Querempfindlichkeit zu erhalten. Um die Ozon-Querempfindlichkeit bei der Benzo[a]pyren-Bestimmung zu studieren, wurde Ozon in den Ansaugbereich der Probenahme dosiert. Als Ergebnis der Untersuchungen kann festgehalten werden, dass für die Benzo[a]pyren-Immissionsmessung eine deutliche Ozon-Querempfindlichkeit besteht, die unter Einsatz des neuen Ozon- Scrubbers vermieden werden kann.
The aim of this study was to develop a biomechanically validated finite element model to predict the biomechanical behaviour of the human lumbar spine in compression.
For validation of the finite element model, an in vitro study was performed: Twelve human lumbar cadaveric spinal segments (six segments L2/3 and six segments L4/5) were loaded in axial compression using 600 N in the intact state and following surgical treatment using two different internal stabilisation devices. Range of motion was measured and used to calculate stiffness.
A finite element model of a human spinal segment L3/4 was loaded with the same force in intact and surgically altered state, corresponding to the situation of biomechanical in vitro study.
The results of the cadaver biomechanical and finite element analysis were compared. As they were close together, the finite element model was used to predict: (1) load-sharing within human lumbar spine in compression, (2) load-sharing within osteoporotic human lumbar spine in compression and (3) the stabilising potential of the different spinal implants with respect to bone mineral density.
A finite element model as described here may be used to predict the biomechanical behaviour of the spine. Moreover, the influence of different spinal stabilisation systems may be predicted.
The use of a TLC scanner can be regarded as a key step in high performance thin layer chromatography (HPTLC). Densitometric measurements transform the substance distribution on a TLC plate into digital computer data. Systems that allow quantitative measurements have been available for many years for either fluorescence or ultraviolet absorption measurements, while lately the reflection analysis mode for both types is the most common application. New scanning approaches are designed to aid the analyst who has common demands for TLC-densitometry without using special data, such as scanned images. Two examples that have been developed lately in the laboratories of the authors are described in this paper. These approaches were developed on the basis of current needs for analysts who employ TLC as a tool in research, as well as in routine analysis. One approach is aimed to support analysts in economically disadvantaged areas, where cost intensive apparatus is unsuitable but trace analysis by simple means is required. The other system, allows the spectral determination of chromatographic spots on TLC plates covering the ultraviolet and visible range, thus, revealing highly desired information for the analyst.