Reflection spectroscopy in microstructured light scattering materials

Summary A theoretical model is derived that describes the influence of lateral light diffusion in a scattering medium on the absorptivity of an absorber spot on top of the substrate. The model uses the lateral resolved reflectivity under point irradiation that has been analyzed experimentally with a scanning-micro-laser-reflectometer. The model allows quantification of the absorptivity by one single equation that contains only the mean radial diffusion length of light and the spot area. Experiment and theory are applied to typical substrates for thin layer chromatography (alumina, silica, cellulose). The diffusion lengths in these substrates are given and the absorptivities of the spots are calculated as a function of the spot area.     

Memory effects in gas chromatographic detection with a microwave-induced plasma

Capillary gas chromatography coupled to microwave-inducedplasma detection furnishes sensitivity adequate for trace analysis when the signal is monitored at a carbon emission line. Work performed with one of these systems at high electronic gain for the carbon signal has revealed solvent band widths in excess of four minutes; these impeded quantification of peaks eluting after the solvent. This report discusses two phenomena which could be related to the unexpected intensity of this solvent response: photomultiplier tube saturation and carbon deposits in the quartz plasma discharge tube.     

Dense Monolayers of Monodisperse Opaque Spheres: Transmission and diffraction in the fraunhofer domain

The transmission and diffraction of radiation through dense monolayers of monodisperse opaque spheres were studied for the Fraunhofer domain. Theoretical considerations, numerical calculations and experiments on ultrasonic transmission and on laser light transmission and diffraction yielded corresponding results. Complementary studies included the cases of sterically non-interacting particles (by numerical simulation) and of small particle size parameters (by ultrasonic extinction). Transmission was found to be, in general, a non-linear function of the monolayer density. Secondary effects on the transmission can be attributed to the effect of the monolayer structure (characterized by the pair correlation function) on the angular distribution of diffracted intensity. The results were found to be in accordance with experimental results on extinction in three-dimensional systems.     

Ferrocene derivatives XXVIII. The metallation of phenylazoferrocene and the synthesis of phenylazocyclopentadienyl derivatives of other metals

Phenylazoferrocene undergoes nickelation and palladation exclusively on the phenyl group. Lithium phenylazocyclopentadienide has been converted into derivatives of Mo, Mn, Fe, Ru and Rh.     

Analysis of barbiturates in human serum and urine by high-performance capillary electrophoresis-micellar electrokinetic capillary chromatography with on-column multi-wavelength detection

The analysis of barbiturates in human serum (or plasma) and urine by high-performance capillary electrophoresis-electrokinetic capillary chromatography with on-column fast-scanning multi-wavelength detection is discussed. The use of a buffer of ca. pH 8 and containing sodium dodecyl sulphate provides a medium suitable for fast and high-resolution separations of barbiturates. Seven barbiturates are characterized by their retention and absorption spectra between 195 and 320 nm. Comparison of these computer-stored data with those of unknown samples is shown to allow the identification of barbiturates in samples of patients undergoing pharmacotherapy and in toxicological urine and serum specimens. Three-dimensional electropherograms provide reliable information on the requirement and suitability of sample pretreatment procedures. With urine, extraction of barbiturates prior to analysis is necessary. With human serum several barbiturates, including phenobarbital, are shown to elute in an interference-free window in front of uric acid and the proteins, allowing these substances to be determined by direct sample injection. The need for multi-wavelength detection over a relatively wide wavelength range as a means of peak confirmation in electrokinetic capillary analyses is demonstrated and limitations of this technique for compounds with similar retention behaviour and absorption spectra are discussed.