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Direct precise determination of Pd, Pt and Rh in spent automobile catalysts solution by high-resolution continuum source graphite furnace atomic absorption spectrometry
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.2 ) Pub Date : 2020-03-01 , DOI: 10.1016/j.sab.2020.105784
Vasilina V. Eskina , Olga A. Dalnova , Daria G. Filatova , Vasilisa B. Baranovskaya , Yuri A. Karpov

Abstract This work investigates the analytical possibilities of high-resolution continuum source graphite furnace atomic absorption spectrometry (HR CS GFAAS) for the determination of Pd, Pt and Rh (PGMs) in spent automobile catalysts without chemical separation. A novel approach for the microwave dissolution with the mixture of HCl and H2O2 (4:1) was developed for the further HR CS GFAAS. It was found that within 20 min at the temperature 210 °C of the PGMs quantitatively and simultaneously transferred to solution. It did not show any matrix interferences in determining Pd and Rh, when using HR CS GFAAS for determining the PGMs. When determining Pt, the matrix effect can be expressly minimized by diluting the sample or applying a corrective model. Limits of quantification (μg l−1) by HR CS GFAAS achieved were 1 (Pd), 2 (Pt), and 0.5 (Rh). Correlation coefficients were 0.9973 (Pd), 0.9995 (Pt), and 0.9983 (Rh). The relative standards deviation for PGM determination by the developed procedure was not higher than 5% in the concentration range 0.0005–0.5% weight. Moreover, validation of the developed multielement method demonstrated its robustness. The trueness of experimental results was assured by comparison with the atomic emission spectrometry with inductively coupled plasma method.

中文翻译:

高分辨率连续源石墨炉原子吸收光谱法直接精确测定废汽车催化剂溶液中的Pd、Pt和Rh

摘要 本工作研究了高分辨率连续源石墨炉原子吸收光谱法 (HR CS GFAAS) 用于测定废汽车催化剂中 Pd、Pt 和 Rh (PGM) 的分析可能性,无需化学分离。为进一步的 HR CS GFAAS 开发了一种使用 HCl 和 H2O2 (4:1) 的混合物进行微波溶解的新方法。结果发现,在 210°C 的温度下,PGM 在 20 分钟内定量并同时转移到溶液中。当使用 HR CS GFAAS 测定 PGM 时,它在测定 Pd 和 Rh 时没有显示任何基质干扰。在确定 Pt 时,可以通过稀释样品或应用校正模型来明确地最小化基质效应。HR CS GFAAS 的定量限 (μg l-1) 为 1 (Pd)、2 (Pt) 和 0.5 (Rh)。相关系数为 0.9973 (Pd)、0.9995 (Pt) 和 0.9983 (Rh)。在 0.0005-0.5% 重量的浓度范围内,通过开发的程序测定 PGM 的相对标准偏差不高于 5%。此外,开发的多元素方法的验证证明了其稳健性。通过与电感耦合等离子体法原子发射光谱法的对比,保证了实验结果的真实性。
更新日期:2020-03-01
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