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- 2014 (3) (entfernen)
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The results of analytical measurements performed with solid-sampling techniques are affected by the distribution of the analytes within the matrix. The effect becomes significant in case of determination of trace elements in small subsamples. In this framework we propose a measurement model based on Instrumental Neutron Activation Analysis to determine the relative variability of the amount of an analyte among subsamples of a material. The measurement uncertainty is evaluated and includes the counting statistics, the full-energy gamma peak efficiency and the spatial gradient of the neutron flux at the irradiation position. The data we obtained in a neutron activation experiment and showing the relative variability of As, Au, Ir, Sb and W among subsamples of a highly pure Rh foil are also presented.
After some months of operation, a number of PV modules develop a discolouration defect called 'snail trails', or 'snail traces', which appear as irregular dark stripes across the cells. Whereas these traces were soon identified as discoloured silver contacts along the cell edges or at micro cracks, the chemical and mechanistic reasons for this phenomenon have not yet been resolved in detail. In this work we show that silver nanoparticles accumulating within the encapsulation foil cause the brownish discolouration, and that certain additives of encapsulation and back sheet foils trigger the formation of these nanoparticles.
Aiming for a round-robin test, a new method for the direct determination of fluorine in niobium oxide has been developed. It is based on the use of high-resolution molecular absorption spectra of calcium mono-fluoride (CaF) generated in the graphite tube, combined with the slurry sampling technique. The absorption measurement was performed at the 606.44 nm CaF rotational line. By using graphite tubes with zirconium carbide (ZrC) modified platform, the molecular absorption sensitivity of CaF has been improved by a factor of 20, and no additional chemical modifier was necessary. Generally, non-spectral interferences were observed in the presence of HCl, H2SO4, and H3PO4. For HCl, additional spectral interference occurred due to an overlap of the absorption spectra of CaF and CaCl. However, due to the absence of these mentioned substances in the current material, such interferences do not exist for this application. The characteristic mass found for the CaF 606.44 nm line was 0.1 ng; the limit of detection was 5 mg fluorine per kg solid sample (3σ criterion). The results obtained by the method were within the range of certified values. Comparing to the classical method such as the pyrohydrolysis-photometric method, the developed new method showed clear advantages regarding sensitivity and specificity. The time requirement for one sample analysis was strongly shortened from several hours to only some minutes.