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Samples of the permineralized tree fern Psaronius sp. from the Lower Permian Rotliegend of Chemnitz were examined to find out their chemical composition and structural behavior. The inhomogenic distribution of elementary constituents of oxides, sulfates and carbonates within the silica-matrix consisting of ?-quartz and chalcedony were formerly detected by analytical X-ray microscopy. Most of the compounds could be revealed by Raman spectroscopy. Calcite and barite developed in small fissures. Iron of different oxidation level is the prevailing pigment in the agate preserved adventitious roots. Coalified cellulose whose structure mainly corresponds to anthracite reflects the anatomical detail of the former organic tissues.
Permineralized samples of the tree fern Psaronius sp. belong to the spectacular discoveries of the Lower Permian Rotliegend Petrified forest of Chemnitz, one of the most famous palaeontological sites in the world. The cellular tissues of the 280 million years old fossil fern show a delicate three-dimensional preservation by permineralization. Moreover, anatomical detail can be distinguished very well because of the black coloured former cell walls. By means of Raman spectroscopy this fossilised tissue of the adventitious roots is revealed to be carbon which structure seems to correspond to anthracite. The aim of this work is the experimental confirmation of the carbon structure by means of thermogravimetry and Raman spectroscopy on coal samples of different rank, especially anthracite samples from different times and localities.
Coal maturation involves the sequence peatlignitecoalanthracite-microcrystalline graphite by incresasing the density and specific energy. The loss of in situ moisture (typically up to 200 °C) and volatile organic matter (up to 600 °C) has been acquired by thermogravimetry. The increasing carbon content, density resp. structure results in Raman spectra with typical band shape of the D- and G-peaks. We used these methods to characterise and compare the separated coal samples to the dispersed carbon inclusions in permineralized Psaronius.
Samples of different three-dimensionally preserved fossil plants (Medullosa sp., Dadoxylon sp., Calamodendron striatum, Psaronius sp.) from the Lower Permian petrified forest of Chemnitz were examined with regard to their chemical composition and structural order. Raman spectroscopy and cathodoluminescence microscopy are shown to be powerful tools for such investigations.
Silicified wood from ChemnitzHilbersdorf generally shows yellow cathodoluminescence (CL) of the cell walls and only weak yellow-brownish CL of the cell lumina. By time-resolved cathodoluminescence spectroscopy, a secondary mineralisation of hydrothermal origin was recognized. The latter is shown by short-lived blue CL at the cell walls extinguishing the yellow signal. Therefore, after the primary silicification step a secondary mineralisation step initiated by hydrothermal processes, seems to have taken place at probably slightly higher temperatures. The resulting silica matrix consists of phanerocrystalline and microcrystalline a-quartz as well as microcrystalline moganite, both partially associated with iron oxides.
Dadoxylon sp. is a prominent example for parallel permineralisation by a-quartz and fluorspar, which is outstanding for the Chemnitz Petrified Forest. CL on this samples shows parallel silicification and fluoritisation, followed by infiltration of iron oxides.
Permineralised samples show very low percentage of original organic remains. The seed fern Medullosa, for example, shows dispersed carbon, which is mainly restricted to the centres of the typical star-shaped vascular bundles. Raman spectroscopy revealed that these carbonaceous particles are of an anthracite structure. For experimental confirmation coal samples of different rank, especially anthracite from different geological times and localities, were studied by means of Raman spectroscopy. The remaining pith of the vascular bundles is white-coloured and consists of a-quartz and moganite, whereas surrounding tracheides exhibit white and reddish coloured parts. The reddish parts, mainly found in the rays, additionally contain a-Fe2O3 and Fe3O4 among the SiO2 polymorphs of a-quartz and moganite. Sometimes iron oxides could have dominated permineralisation processes as the peak intensities of distinct parts of the samples suggest.
The improved Monte-Carlo (MC) method for standard-less analysis in laser induced breakdown spectroscopy (LIBS) is presented. Concentrations in MC LIBS are found by fitting model-generated synthetic spectra to experimental spectra. The current version of MC LIBS is based on the graphic processing unit (GPU) computation and reduces the analysis time down to several seconds per spectrum/sample. The previous version of MC LIBS which was based on the central processing unit (CPU) computation requested unacceptably long analysis times of 10's minutes per spectrum/sample. The reduction of the computational time is achieved through the massively parallel computing on the GPU which embeds thousands of co-processors. It is shown that the number of iterations on the GPU exceeds that on the CPU by a factor > 1000 for the 5-dimentional parameter space and yet requires > 10-fold shorter computational time. The improved GPU-MC LIBS outperforms the CPU-MS LIBS in terms of accuracy, precision, and analysis time. The performance is tested on LIBS-spectra obtained from pelletized powders of metal oxides consisting of CaO, Fe2O3, MgO, and TiO2 that simulated by-products of steel industry, steel slags. It is demonstrated that GPU-based MC LIBS is capable of rapid multi-element analysis with relative error between 1 and 10's percent that is sufficient for industrial applications (e.g. steel slag analysis). The results of the improved GPU-based MC LIBS are positively compared to that of the CPU-based MC LIBS as well as to the results of the standard calibration-free (CF) LIBS based on the Boltzmann plot method.
Tomography of a laser-induced plasma in air is performed by inverse Radon transform of angle-resolved plasma images. Plasmas were induced by single laser pulses (SP), double pulses (DP) in collinear geometry, and by a combination of single laser pulses with pulsed arc discharges (SP-AD). Images of plasmas on metallurgical steel slags were taken at delay times suitable for calibration-free laser-induced breakdown spectroscopy (CFLIBS). Delays ranged from few microseconds for SP and DP up to tens of microseconds for SP-AD excitation. The white-light and the spectrally resolved emissivity ε(x,y,z) was reconstructed for the three plasma excitation schemes. The electron number density Ne(x,y,z) and plasma temperature Te(x,y,z) were determined from Mg and Mn emission lines in reconstructed spectra employing the Saha-Boltzmann plot method. The SP plasma revealed strongly inhomogeneous emissivity and plasma temperature. Re-excitation of plasma by a second laser pulse (DP) and by an arc discharge (SP-AD) homogenized the plasma and reduced the spatial variation of ε and Te. The homogenization of a plasma is a promising approach to increase the accuracy of calibration-free LIBS analysis of complex materials.