陽極溶出法による希土酸化物中の微量ニッケルの定量
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Anodic stripping method had been studied for the determination of trace amounts of nickel in rare earth oxides. Potassium thiocyanate has been found to be the most suitable supporting electrolyte for this purpose.<BR>Nickel is electrodeposited at -1.0 V (<I>vs</I>. SCE) for 15 min or 1 hr on a platinum wire electrode. An anodic dissolution curve is then recorded by linearly varying potential over a range of -1.0 to 1.0 V (<I>vs</I>. SCE) at a rate of 2.4 V/min.<BR>Platinum wire electrode is polished previously with aluminum oxide powder (about 200 mesh) and with a small piece of filter paper on which a small amounts of sodium bicarbonate is put. It is then treated at +0.4 V (<I>vs</I>. SCE) for about 5 min in the supporting electrolyte solution after washing with nitric acid and water. The electrode could be used many times over.<BR>Suitable concentration range of supporting electrolyte solution was from 0.4 to 0.6<I>M</I>. Dissolution peak current showed the highest and constant value over the pH range from 5.0 to 5.5.<BR>The more pre-electrolysis potential was negative, the higher dissolution peak current was obtained. Gas liberation was found however on the electrode at more negative potential than -1.05 V (<I>vs</I>. SCE), and it seemed to interfere with the electrodeposition of nickel.<BR>Good linear relationship between the concentration of nickel over a range of 1 × 10<SUP>-8</SUP> to 1 × 10<SUP>-6</SUP><I>M</I> and the dissolution peak current. The coefficient of variation was 3.2% in the case of 1 × 10<SUP>-6</SUP><I>M</I> of nickel concentration. Dissolution current depended on the square root of the scanning rate of voltage obeying to the Sevcik's equation.<BR>Nitrate and sulfate did not interfere but chloride more than 0.1<I>M</I> and tartrate, citrate and phosphate interfered.<BR>Although many other metal ions interfered with the determination of nickel, these interference could be eliminated by using dithizone-carbon tetrachloride and dimethylglyoxime-chloroform extraction methods.<BR>Following analytical procedure is proposed : dissolve 0.25 to 2.0 g of rare earth oxides with hydrochloric acid (in the case of ceric oxide, nitric acid and hydrogen peroxide are used) and adjust the pH of the solution to 1.0 after addition of ammonium citrate. Remove copper in the sample solution by the dithizone-carbon tetrachloride extraction method. Then extract nickel with dimethylglyoxime-chloroform solution after adjusting the pH to 9.510.0 and determine the amount of nickel as described above after destruction of organic matter with nitric and sulfuric acids.<BR>About 0.1 to 3 ppm of nickel in the rare earth oxides was determined by the proposed method.
- 社団法人 日本分析化学会の論文
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