M.Tech. / The Inductively Coupled Plasma Mass Spectrometry (ICP-MS) technique showed very high uncertainties associated with the determination of the concentrations of minor elements in the Platinum Group Metal (PGM) smelting plant samples. This project reports on the work done for the identification of, and subsequent minimisation of the sources of uncertainties associated with the measurements of minor elements in the PGM Furnace Matte material by ICP-MS. To perform these studies, Elan 6000, Shimadzu ICPM-8500 and Finnigan Element 2 ICP-M spectrometers were employed. Synthetic Furnace Matte samples (SFMSs) were prepared and used to ascertain the uncertainties associated with the alleged sources at Mintek and Leo-Tech laboratories. The Element 2 spectrometer dominated the other two ICP-M spectrometers in terms of the accuracy for the determination of the concentrations of minor elements in SFMSs. The evidence of spectral interferences from the significant deviations in the measurement results between the isotopes of the same element was observed in the quantification of Zn, Se, Te and Sn in SFMS by the quadrupole Elan 6000 and the Shimadzu spectrometers. It also transpired that the accuracy of the quantitative determination of minor elements in the Furnace Matte (FM) matrix by ICP-MS was hampered by the matrix elements with the severity depending on the specific analyte and the make and model of the ICP-M spectrometer. The Anglo platinum FM material that was analysed in the second round robin was used as a Certified Reference Material (CRM) in the analysis of the Lonmin FM sample. It was revealed that the laboratory standard operating procedures for the preparation, dilution and subsequent analysis of the sample are potential sources of uncertainty in measurement results. The two-fold dilution of the sample for the lessening of the matrix effects was not effective. The use of multi-walled nanotubes for the alleviation of the matrix effects by removal was also not successful. Nevertheless standard addition method (SAM), combined with internal standardisation can be used as an effective calibration method in ICP-MS to achieve less matrix interfered results over the combination of the common external standardisation and internal standardisation methods.
| Identifer | oai:union.ndltd.org:netd.ac.za/oai:union.ndltd.org:uj/uj:8239 |
| Date | 31 March 2009 |
| Creators | Goso, Xolisa Camagu |
| Source Sets | South African National ETD Portal |
| Detected Language | English |
| Type | Thesis |
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