A robust method of analysis that uses multichannel array detector technology is presented for high-precision, accurate measurement of Pt, Pd and Rh in catalytic converters. Catalytic converter samples, National Institute of Standards and Technology (NIST) reference standards, and a fresh converter sample are dissolved and analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES). Complete dissolution of sample sizes up to 2 g of NIST reference standards is achieved with the use of high-pressure, high-temperature carius tubes. Carius tube dissolution of a modern catalytic converter sample is found to be incomplete because of the presence of higher concentrations of Ce, Ni, and Zr. For this sample, the addition of FeCl<sub>3</sub> increases the dissolving power of the carius tube for base metals and noble metals, particularly Rh. Although interference problems are encountered in samples bearing high concentrations of Fe, use of a high-resolution ICP-AES system alleviated these problems. Precise quantitation of Pt, Pd, and Rh is accomplished by using the method of standard additions, with high accuracy and a precision of 1–2% RSD (relative standard deviation). This analysis also confirmed the values determined by NIST by using isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) for standard reference materials (SRMs) 2556 and 2557.
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