Abstract
A method for determining traces of fluoride in tantalum metal powder using pyrolytic separation and alizarin complexone extraction spectrophotometry has been established.A half gram of sample is mixed with 1 g of uranium oxide (U3O8) by grinding, and the mixture is transferred into a porcelain boat. Pyrolysis is carried out under a stream of moist nitrogen (for 10 minutes) followed by moist oxygen (for 5 minutes) in a fused silica combustion tube (about 1100°C).The volatilized fluoride is absorbed in 20ml of dilute sodium hydroxide solution. This solution is taken into a separatory funnel, and added with 20ml of combined lanthanum-alizarin complexone reagent solution.Extraction is made with 10ml of 5vol% N, N-diethylaniline in iso-amyl alcohol by shaking for 3 minutes, and the two layers are allowed to separate by standing. After the drainage of the aqueous layer, the organic layer is washed with 50ml of acetate buffer solution. The absorbance of the organic layer is measured at 580 mμ using a reagent blank as a reference.
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