銅-ジルコニウム合金中の介在酸化ジルコニウムの定量

概要

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A methanolic bromine method for determination of zirconium oxide inclusion in Cu-Zr alloy have been presented. In order to decide the optimum condition for extracting the inclusion, the effects of decomposition temperature, concentration of bromine, etc. on the solubility (recovery) of zirconium oxide have been studied by the use of pure zirconium oxide and internally oxidized Cu-Zr alloy. The zirconium oxide inclusion have been isolated completely as the residue from the matrix by this method. The recommended procedure is as follows : 25g of Cu-Zr alloy is decomposed with methanolic bromine (200 ml methano1+10 ml of bromine) in a decomposition flask at 6065°C for 3 hrs. The solution is filtered by suction through Membrane filter (UCF, mittel). The residue is washed with methanol, ignited in a platinum crucible, and dissolved with 6 ml of 60% HClO4, 3 ml of conc. HNO3 and 3 ml of 46% HF. The solution is evaporated to fumes of HClO4 and made up to 100 ml with 5ml of conc. HNO3 and water. An aliquot containing 525μg of zirconium is taken into a 50ml volumetric flask, and 25ml of conc. HNO3, 2.5 ml of 10% urea solution and 10.0 ml of 0.05% Arsenazo-III solution are added. It is made up to 50ml with water and the absorbance at 665 mμ is measured against water. The amount of zirconium is determined from its calibration curve.
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