高純度안티몬 中의 不純物 (鐵 및 銅)의 8-Hydroxy-quinoline에 依한 吸光光度定量法

Spectrophotometric Determination of Impurities such as Iron and Copper in High Purity of Antimony with 8-Hydroxy-quinoline

8-Hydroxy-Quinoline(Qxine)에 依한 高純度 Antimony中 不純物(鐵 및 銅)의 吸光光度 定量法을 檢討하였다. 試料의 黃酸溶液에 안티몬을 Masking하기 위하여 必要한 酒石酸의 影響을 調査한 結果, 0.5M-酒石酸溶液 10ml로서 600mg 까지의 안티몬을 Masking할 수 있었다. pH 範圍는 鐵은 5.0-5.7, 銅은 3.5-4.0이었다. 鐵은 580$m{\mu}$ 에서 吸光度를 測定하면 되나, 銅은 15%苛性소오다溶液으로 逆抽出하고, 남은 鐵을 580$m{\mu}$, 410$m{\mu}$ 에서 測定하여 補正할 必要가 있다. 500mg 안티몬에 對하여 鐵은 150${\mu}g$(0.005~0.03%)까지, 銅은 100${\mu}g$(0.005~0.016%)까지 定量이 可能했다.

A spectrophotometric method for the determination of major impurities, such as iron and copper, in high purity of antimony with 8-hydroxyquinoline (oxine) has been studied. The iron-oxinate is stable at the pH range 5.0 to 5.7, and the copper-oxinate at the pH range 3.5 to 4.0. To mask antimony in sulfuric acid solution of sample, author has investigated the effect of tartaric acid on antimony, and found that 10ml of 0.5M tartaric acid solution could mask up to 600mg of antimony. The absorbance of iron-oxinate was measured at 580$m{\mu}$ and iron could be determined, but it is necessary for copper-oxinate to measure at 410 and 580m respectively after removing heavy metals other than copper by back extraction with 15% solution of sodium hydroxide, and copper could be determined by making a correction for the amounts of iron present. Up to 150 ${\mu}g$ of iron (0.005-0.03%), and 100 ${\mu}g$ of copper (0.005-0.016%), in 500mg of antimony could be determined.