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首页> 外文OA文献 >High precision and spatial analysis of platinum, palladium, and rhodium in catalytic converters by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry
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High precision and spatial analysis of platinum, palladium, and rhodium in catalytic converters by inductively coupled plasma atomic emission spectroscopy and inductively coupled plasma mass spectrometry

机译：电感耦合等离子体原子发射光谱法和电感耦合等离子体质谱法对催化转化器中的铂，钯和铑进行高精度和空间分析

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摘要

The accuracy and precision of catalytic converter analysis using conventional analytical methodology such as fire assay, x-ray fluorescence, atomic absorption and ICP-AES are typically in the range of ±7-10% RSD. Due to the high cost of noble metals, methods of analysis with increased accuracy and precision are desired to evaluate the loading of noble metals onto converter bricks. The investigations described in this work have resulted in a better understanding of many of the inherent problems and have contributed new approaches for sample dissolution and analysis using array detector based Inductively Coupled Plasma Atomic Emission Spectroscopy (ICP-AES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). These methods are shown to be accurate and precise for the analysis of Pt, Pd, and Rh in catalytic converters. Catalytic converters are difficult to dissolve by conventional acid methodology. While carius, tubes have previously been employed to dissolve small weights of sample, complete dissolution of increased amounts of sample, as needed for high precision ICP-AES analysis, has been hindered by the insufficient oxidation potential of the acids in the carius tube. In this work, the addition of ferric chloride is shown to increase the dissolving power of the carius tube method and specifically targets Pt, Pd and Rh for dissolution. Simultaneous collection of analyte wavelengths and simultaneous background correction, as performed with multichannel array detector ICP-AES instrumentation, have enhanced sensitivity and precision in catalytic converter analysis when compared to single channel instrumentation. The studies described within this dissertation demonstrate that flicker noise has been effectively eliminated through the use of multichannel array based ICP-AES instrumentation. With proper line selection and the use of the high-resolution system, Pt, Pd and Rh in catalytic converters can be analyzed with precision of 1-1.5%. ICP-AES accuracy has been confirmed through isotope dilution ICP-MS employing new methodology to avoid Zr isobaric interferences.
机译：使用常规分析方法（例如，火焰分析，X射线荧光，原子吸收和ICP-AES）进行催化转化器分析的准确性和精度通常在±7-10％RSD范围内。由于贵金属的高成本，需要一种具有更高准确性和精度的分析方法来评估贵金属在转炉砖上的负载。这项工作中描述的研究已经使人们对许多内在问题有了更好的了解，并为使用基于阵列检测器的电感耦合等离子体原子发射光谱法（ICP-AES）和电感耦合等离子体质谱法（ ICP-MS）。这些方法对于催化转化器中的Pt，Pd和Rh的分析显示出精确的结果。催化转化器难以通过常规酸方法溶解。尽管在龋齿管中以前曾使用过管来溶解小重量的样品，但由于龋齿管中酸的氧化电位不足，妨碍了高精度ICP-AES分析所需的增加量的样品完全溶解。在这项工作中，氯化铁的添加显示出增加了卡里乌斯管法的溶解能力，并且特别针对溶解的目标是Pt，Pd和Rh。与单通道仪器相比，同时使用多通道阵列检测器ICP-AES仪器进行分析物波长的同时收集和同时进行背景校正，在催化转化器分析中具有更高的灵敏度和精度。本文所描述的研究表明，通过使用基于多通道阵列的ICP-AES仪器，闪烁噪声已得到有效消除。通过正确的选线和高分辨率系统的使用，催化转化器中的Pt，Pd和Rh可以以1-1.5％的精度进行分析。通过采用新方法避免Zr同量异位干扰的同位素稀释ICP-MS，已确认ICP-AES的准确性。

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