Determination of Oxygen in Zirconium Metal by Vacuum Fusion Method and Bromination-Carbon Reduction Method

Abstract

Determination of oxygen in zirconium metal were studied by the vacuum fusion method and the bromination-carbon reduction method. In the vacuum fusion method, the iron-tin bath technique usually applied for the analysis of gases in titanium metal was used. In this case the molten iron bath in a graphite crucible is the reaction medium. The sample reacts with the molten iron bath containing tin to form a stable carbide of zirconium. At a furnace temp. of 1850°, complete reduction of the oxides is effected within 30 minutes. The evolved gases are extracted and analyzed. In the bromination-carbon reduction method, the sample is mixed with carbon and treated with bromine at 925°, using argon as carrier gas. The oxygen in the sample is converted into carbon monoxide, which is then oxidized to carbon dioxide with hot copper oxide. The carbon dioxide is absorbed into a weighing bulb containing sodium hydroxide.The results with various samples of materials with these methods show a good agreement. In the vacuum fusion method, oxygen in zirconium metal could be determined with accuracy of ±0.01%.