A fast and direct determination procedure for precious metals in spent automotive catalyst was developed using the novel high-energy polarized-beam XRF. A sample preparation method working directly on the ground material was optimized. The material was pressed as a pellet using wax as a binder; no internal standard was added. The standards for this application were available spent automotive catalyst, previously analyzed by ICP-OES to verify their concentration, prepared in the same way as the unknown samples. The investigated concentration ranged from nearly 0 to approximately 2700 ppm for Pt, to 500 ppm for Rh, and to 7500 ppm for Pd. The repeatability of the XRF measurement appeared to be better than 0.5%, while the precision of the whole method was approximately 1%. The accuracy of the XRF method was verified with the well-established (but very time-consuming) ICP-OES method; a good agreement (no difference when using the 95% confidence interval) was found for the results. When using an irradiation time of 500 s for the CsI secondary target and the Zr secondary target, the detection limits for Pt, Pd, and Rh were found to be better than 5 ppm.

A new commercial energy dispersive X-ray fluorescence spectrometer (EDXRF), applying a three-dimensional geometry and high-energy excitation, was optimized for the quantitative analysis of aerosols deposited on filters. The preliminary results are presented here. First-order calibration curves were obtained for 20 elements deposited on the filters. The accuracy of the applied method and of the obtained calibration curves was checked by the measurement of a standard reference material from NIST. The precision of the analysis for the majority of the analytes was better than 10%. Due to the obtained low detection limits, it is possible to determine the analytes usually present at very low concentrations in ambient air, such as, e.g., Cd, Sb, Cr, and V. It is also possible to decrease significantly the time of analysis or the time of the sampling.