Spectrophotometric determination of niobium in rocks

After acid decomposition and evaporation to volatilize silica, samples containing 0.5 6 μg Nb are fused with pyrosulfate and dissolved in hydrochloric acid tartaric acid. Niobium is separated by thiocyanate extraction with amyl alcohol and back-extracting from the organic solvent with dilute hydrofluoric acid. Niobium is reacted with 4-(2-pyridylazo)-resorcinol to obtain a colored species. Analytical error, estimated from replicate analyses of eight U.S. Geological Survey standard rocks, ranges from 2.9 to 6.4 percent at the 1 27 μg/g Nb level.