Flow-injection analysis of the platinum-group metals

Doctoral Thesis

1995

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University of Cape Town

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Abstract
To date the principle methods for the determination of the platinum-group metals (PGMs) use an "off-line" assay with flame-atomic absorption spectrometry and visible spectrometry. Both suffer numerous interferences and involve time-consuming and arduous laboratory separation methods prior to analysis. An "on-line" method for the rapid assay of the PGMs is indeed a lacking component in the analysts' repertoire of methods. This study describes the development of spectrophotometric methods for the determination of the PGMs using flow-injection analysis (FIA). The principle of exploiting the remarkably specific and selective reaction of stannous halides with the PGMs to yield a series of intensely coloured complexes in acidic solutions forms the basis of these methods. The reaction is subject to relatively few interferences from other transition metals. A high speed scanning spectrophotometer is employed to obtain second order data. The successful manipulation of the data enables the determination of PGMs as single components and also simultaneously in mixtures. Attention is focused on the establishment of principles for successful multi-component analysis of PGMs. The development of a software program for multi-wavelength data manipulation was mandatory and is described. Criteria for successful selection of analytical wavelengths are discussed. The usefulness of multi-dimensional graphical data representation is demonstrated in a stop-flow study of the palladium reaction with tin (II) chloride. Qualitative information is provided regarding the nature of complexes and their interactions. Correlation of spectrophotometric data with complex solution colour changes is made. The requirements for future progress in multi-component FIA determinations as well as the direction for future research conclude the study.
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