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介绍了铀、钼分离工艺中钼铀矿、浸出渣、淋浸液、离子交换树脂和产品中铀的快速测定方法。矿石和浸出渣样品用混合铵盐熔解 ,树脂样品经高温灼烧灰化 ,以磷酸溶解。在 60 %磷酸介质中 ,用硫酸亚铁铵将铀( )还原成铀 ( )。在 40 %磷酸和铵盐存在下 ,用亚硝酸钠氧化过量的亚铁 ,并立即用尿素破坏过剩的亚硝酸钠 ,以消除钼的干扰。用二苯胺磺酸钠和苯基邻氨基苯甲酸作指示剂 ,以钒酸铵容量法快速测定铀。对钼含量较高的样品 ,在测定铀之前 ,可在硝酸介质中将钼以钼酸形式析出 ,使铀与大量钼分离 ,然后 ,在 3 0 %~ 40 %磷酸溶液中用亚铁还原 -溴水氧化 -钒酸铵容量法快速测定铀。铀产品 (化学浓缩物 )中的铀 ,可借助适量的盐酸溶解试样 ,然后直接用钒酸铵容量法滴定。本法操作简单、快速 ,适用于从铀、钼共生矿中提取铀的工艺过程中各种样品体系中铀的测定。大量实际样品的例行分析结果表明 ,所得结果准确可靠 ,方法精密度优于± 1 0 % ,标准加入回收率为 98%~ 1 0 5 %
The rapid determination method of uranium in molybdenum uranium ore, leaching residue, leaching liquid, ion exchange resin and product in uranium and molybdenum separation process is introduced. Ore and leachate samples were mixed with a mixture of ammonium salt melting resin samples by high temperature ashing, with phosphoric acid dissolved. Uranium () is reduced to uranium (U) by ammonium ferrous sulfate in 60% phosphoric acid. Excess ferrous iron is oxidized with sodium nitrite in the presence of 40% phosphoric acid and ammonium salts, and the excess sodium nitrite is immediately destroyed with urea to eliminate molybdenum interference. Uranium was rapidly determined by ammonium vanadate volumetric method using sodium diphenylamine sulfonate and phenyl anthranilic acid as indicator. For samples with high molybdenum content, molybdenum can be precipitated as molybdic acid in nitric acid medium before the determination of uranium, uranium is separated from a large amount of molybdenum, and then reduced with ferrous iron in a solution of 30% to 40% phosphoric acid - Bromine Water Oxidation - Ammonium Vanadate Volumetric Method for Rapid Determination of Uranium. Uranium in uranium products (chemical concentrates) can be dissolved in a suitable amount of hydrochloric acid and titrated directly with the ammonium vanadate volumetric method. The method is simple and fast to apply to the determination of uranium in various sample systems during the process of extracting uranium from uranium and molybdenum co-occurring ore. Routine analysis of a large number of actual samples showed that the obtained results were accurate and reliable, the precision of the method was better than ± 10%, and the standard recovery rate was 98% ~ 105%