Determination of tungsten in niobium–tantalum, vanadium and molybdenum bearing geological samples using derivative spectrophotometry and ICP-AES

Abstract

Two different procedures, one using derivative spectrophotometry and another using inductively coupled plasma atomic emission spectrometry (ICP-AES) have been developed for the determination of tungsten in niobate–tantalates, tin slag samples, ores, concentrates and vanadium and molybdenum bearing geological materials. In the first method involving derivative spectrophotometry, 0.05–0.5 g of the sample is fused with sodium hydroxide, the tungsten is extracted by leaching the melt with distilled water and estimated as thiocyanate using a second derivative spectrophotometric method in the presence of interferents, i.e. Nb, Mo and V, without separating them. Mixtures of tungsten with V, Nb and Mo are used for standardizing the various parameters like zero-crossing wavelength, wavelength range, etc. Tolerance limits for V, Nb and Mo have also been evaluated. In the second method involving ICP-AES, 0.05–0.5 g of sample is fused with KHSO 4 to a clear melt and dissolved in ammonium oxalate solution. Ammonium hydroxide precipitation is then carried out to separate Nb and Ta as hydroxides and the filtrate is boiled with nitric acid to destroy the oxalates before aspiration into the plasma for measurement of tungsten values by ICP-AES using the 207.911 nm emission line. Both methods have been applied to niobate–tantalate and tin slag samples and the results obtained are reported in this paper. The values obtained by both methods are in good agreement with each other. The proposed methods have also been applied to the determination of tungsten in two Canadian Certified Reference Standards (CT-1 and MP-2) and the values obtained are in good agreement with the certified values and the R.S.D.% in case of the ICP-AES method varied from 1–2% at >1000 μg g −1 level to 9.4% at the 20 μg g −1 level whereas the R.S.D.% in case of the derivative method varied from 1 to 7.8%.