| 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. |
