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本文拟定了用示波极谱仪测定二氧化铀中氧/铀比的方法。采用1.4M H_3PO_4+1.6MH_2SO_4为底液,测定范围溶解后立刻测定为10—100微克/毫升及氧化后总铀测定为600—1200微克/毫升。样品用磷酸溶解,以硫酸稀释防止产生磷酸铀(Ⅳ)胶状沉淀;取出一份溶液直接极谱测定铀(Ⅵ),再取出另一份溶液用高锰酸钾将四价铀氧化成六价,用亚硫酸钠破坏过量的高锰酸钾,测定总铀量,以差减法求出铀(Ⅳ),实验的结果与库博塔(H.Kubota)计算法和伯德(R.M.Burd)图解法一致。方法的精密度为±2%,微量的铁(Ⅲ)、镍(Ⅱ)、硼(Ⅳ)、硅(Ⅳ)、铜(Ⅱ)、铝(Ⅲ)、钨(Ⅵ)、锰(Ⅱ)、钼(Ⅵ)、钒(Ⅴ)等杂质元素对铀的测定无影响,方法简便、快速,不需分离,适宜于工厂例行分析。
In this paper, a method for the determination of oxygen / uranium ratio in uranium dioxide by oscillopolarography was developed. Using 1.4M H_3PO_4 + 1.6MH_2SO_4 as the bottom liquid, the measurement range immediately after the dissolution of 10-100 μg / ml and the determination of total uranium was 600-1200 μg / ml. The sample is dissolved with phosphoric acid and diluted with sulfuric acid to prevent gelatinous precipitate of uranium phosphate (Ⅳ). A solution is taken to directly measure uranium (Ⅵ), and the other solution is taken out and potassium permanganate is used to oxidize the tetravalent uranium into six Valence, destroying excess potassium permanganate with sodium sulfite, determining the total amount of uranium and determining the uranium (IV) by the subtractive method. The experimental results are in agreement with H. Kubota’s calculation and RMBurd’s graphic method Consistent. The precision of the method is ± 2%. The trace iron (Ⅲ), nickel (Ⅱ), boron (Ⅳ), silicon (Ⅳ), copper (Ⅱ), aluminum (Ⅲ), tungsten (Ⅵ) , Molybdenum (Ⅵ), vanadium (Ⅴ) and other impurity elements have no effect on the determination of uranium. The method is simple, rapid and does not require separation. It is suitable for routine analysis in the factory.