Graduate Thesis Or Dissertation
 

The analytical application of the galvanic dissolution of niobium and tantalum : the determination of nitrogen

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  • Nitrogen is a contaminant of niobium and tantalum adversely affecting the workability of the metal. With recent interest in the refractory metals, one problem the chemical analyst must solve is the accurate determination of nitrogen in niobium and tantalum at very low levels. The usual method of assaying for nitrogen in metals uses a modification of the Kjeldahl fixation with subsequent distillation of the ammonia. The dissolution of niobium and tantalum was studied to elucidate a method in which a quantitative recovery of nitrogen could be attained in an economical period of time. Galvanic coupling of the sample with a more noble metal was found to increase the dissolution rates several fold. Methods using rhodium and osmium salts with tantalum and rhodium and platinum salts with niobium were developed using in situ coupling for more efficient contact. The proposed methods were checked against "standard" procedures, and against a recent method using iodate and hydrofluoric acid to promote dissolution.
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