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Determination of Platinum, Palladium, and Rhodium in Automotive Catalysts Using High-Energy Secondary Target X-ray Fluorescence Spectrometry

机译:高能次级靶X射线荧光光谱法测定汽车催化剂中的铂,钯和铑

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A fast and direct determination procedure for preciousmetals 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 0.5percent, while the precision of the whole method was approx1percent. 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 95percent 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.
机译:使用新型高能极化光束XRF,开发了一种快速,直接测定废汽车催化剂中贵金属的方法。优化了直接在地面材料上工作的样品制备方法。使用蜡作为粘合剂将材料压成小丸;没有添加内标。此应用的标准是可用的废旧汽车催化剂,该催化剂已由ICP-OES进行了分析,以验证其浓度,该方法与未知样品的制备方法相同。研究的浓度范围从Pt接近0到大约2700 ppm,Rh到500 ppm和Pd到7500 ppm。 XRF测量的可重复性似乎优于0.5%,而整个方法的精度约为1%。 XRF方法的准确性已通过完善的(但非常耗时)ICP-OES方法进行了验证。结果发现一个很好的一致性(使用95%置信区间时没有差异)。当对CsI次要靶标和Zr次要靶标使用500 s的辐照时间时,发现Pt,Pd和Rh的检出限优于5 ppm。

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