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Eingeladener Vortrag
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For ten years µ-XRF (micro-focus X-ray fluorescence) analysis has been performed with SEM/EDS (scanning electron microscope with an energy dispersive X-ray detector) so that non-destructive analysis of elements at trace level concentrations below 100 µg g-1 becomes possible. This can be considered as a valuable completion of the classical electron probe microanalysis by EDS, an analytical method 'suffering' from rather poor limits of detection in the range of one to two orders of magnitude higher than those of µ-XRF. Based on a representative actual application, namely analysis of RoHS relevant elements at trace concentration levels, the performance of the rather new analytical method with respect to its limits of detection is systematically evaluated. CRMs (certified reference materials) specially prepared to support the quantitative XRF analysis of RoHS relevant elements were employed. On the other side, based on calculations of µ-XRF spectra according to a recently developed physical model the optimization of the analytical performance is also successfully undertaken.
In this study the microscopic homogeneity of the newly developed plastic reference materials BAM H001-BAM H010 was investigated. The materials consist of an acrylonitryle-butadien-styrene terpolymer, doped with different amounts of the elements Br, Cd, Cr, Hg and Pb. For the quantitative determination of the degree of homogeneity, a procedure proposed by Kempenaers et al. (Fresenius J. Anal. Chem., 2001, 369, 733-737) was used. On every sample an extensive number of different points were analyzed and standard deviation for every element mentioned above was used to calculate a minimal sampling mass that is necessary to reach a certain level of uncertainty caused by inhomogeneity (mmin,5%). The experiments were taken out with synchrotron µ-XRF (SR µ-XRF) at BESSYII in Berlin and by laser ablation inductively coupled plasma mass spectroscopy (LA-ICP-MS). The calculated values for mmin,5% of both techniques showed comparable results for all elements. It could be shown that the materials are suitable for calibration of micro analytic techniques if at least 64 µg are used.
A new setup for fast spatially resolved measurements of elemental trace amounts under total reflection conditions using a new colour X-ray camera is described. Samples prepared on conventional total reflection X-ray fluorescence (TXRF) reflectors were measured at BESSY II synchrotron. A spatial resolution of 50 × 50 µm² was obtained, while the required time for the investigation of a 10 × 10 mm² sample is 30 seconds. The set-up is up to 350 times faster than conventional X-ray fluorescence systems for elemental traces. The major components of the X-ray camera are polycapillary optics and a pn-CCD chip with an active area of 13 × 13 mm². This area is divided into 264 × 264 pixels of 48 × 48 µm². A full X-ray spectrum with a resolution of 152 eV @ 5.9 keV and a chip temperature of 246 K is recorded for each pixel. The chip has a read-out rate of 400 Hz.