oa South African Journal of Chemistry - Alternative dissolution methods for analysis of niobium containing samples : research article

Volume 63, Issue 1
  • ISSN : 0379-4350



Inductively coupled plasma optical emission spectrometry was applied for the qualitative and quantitative analyses of the different high purity Nb containing samples such as Nb metal, NbO and NbF. Microwave-assisted digestion of the Nb compounds with concentrated HSO in PTFE vessels produced Nb recoveries of 99.90 ± 0.08 % for Nb metal, 98.8 ± 0.7 % for NbO and 100.7±0.4% for NbF. Fusion of NbO with LiBO flux and the subsequent dissolution of the melt with concentrated HSO resulted in the precipitation of HBO under these conditions. Methanol was added to the reaction mixture to convert the boric acid into the volatile methyl ester in an effort to remove the excess HBO. This procedure yielded a recovery of 103±2% for the pure NbO sample.

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