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Determinação dos elementos do grupo da platina após fusão coletora com sulfeto de nível

by de Souza, Alexandre Paulo

Abstract (Summary)
The nickel sulfide fire assay was used to separate and to concentrate the platinum group elements (PGE) and gold (Au) from geological matrices, seeking their analytic determination. The fire assay was accomplished by fusing 10 g of sodium carbonate, 20 g of sodium tetraborate, 1 g of nickel, 0,75 g of sulfur and 10 to 20 g of sample, thoroughly mixed. After cooling, a button of nickel sulfide containing the PGE and Au is obtained. Two analytic techniques were used in the determination of PGE and Au: instrumental neutron activation analysis (INAA) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). The analyses by INAA were made in the residues obtained after the dissolution of the button in concentrated HCI. The determinations by LA-ICP-MS were ma_e directly in the buttons of NiS, after polish. The instrument was calibrated with NiS buttons prepared using quartz doped with PGE and Au standard solution. The two methodologies were appraised through the analysis of seven intemational reference samples, with PGE concentration between 2,4 ng g"l (Os) and 731 ng gol (Pt). The results obtained by INAA tended to be lower than the recommended values, for the analyzed samples. This tendency was attributed to losses of PGE during the dissolution of the NiS buttons. The results obtained by LA-ICP-MS, are in good or excellent agreement with the recommended values, indicating that the extraction of PGE and Au, during the fire assay is quantitative. The detection limits (3s), for all PGE and Au, were in the range ofO,01 ng gol (Ir) to 20 ng g-l (Pd) for INAA and between 0,2 ng gol (Ir) and 2,5 ng gol (Pt) for the LA-ICP-MS technique. The comparison of the two analytic techniques, favors the LA-ICP-MS: the NiS buttons are analyzed directly, the analytic times are significantly smaller, the absence of procedures with can cause losses and/or occasional contamination after the formation of the button, and the instruments tend to become more accessible to the users
This document abstract is also available in Portuguese.
Bibliographical Information:

Advisor:Jacinta Enzweiler; Jacinta Enzweiler [Orientador]; Hardy Jost; Alfonso Schrank

School:Universidade Estadual de Campinas

School Location:Brazil

Source Type:Master's Thesis

Keywords:geoquimica analitica grupo da platina ouro

ISBN:

Date of Publication:01/26/1999

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