铀、钼分离工艺中铀和钼的测定(I).铀的测定  

Determination of Uranium and Molybdenum in Separation Process of Uranium and Molybdenum (I):Determination of Uranium

作　　者：陆诗洁[1] 游建南[1] 

机构地区：[1]核工业北京化工冶金研究院,北京101149

出　　处：《湿法冶金》2002年第1期49-55,共7页Hydrometallurgy of China

摘　　要：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 %simple and rapid methods for determination of uranium in uranmolybdate,leaching residue,leaching solution,ion exchange resins and uranium chemical concentrates during separation of uranium and molybdenum have been studied The samples of ore and leaching residue are fused with mixed ammonium salt,the resin samples are roasted at high temperature The fused sample is dissolved in phosphoric acid In 60% phosphoric acid medium,uranium(Ⅵ) is reduced to uranium(Ⅳ) by ferrous In 40% phosphoric acid and in the presence of ammonium salt,the excess ferrous is oxidized with sodium nitrite,and excess sodium nitrite is destroyed with urea so as to interference of molybdenum can be eliminated The uranium can be determined by ammonium vanadate volumetric procedure,taking sodium diphenylaminesulfonate and phenyl o amidocarbonic acid as indicators Molybdenum in the samples of high content molybdenum can be separated as molybdenum acid precipitate The uranium products (uranium chemical concentrates)is dissolved with a small amount of hydrochloric acid,then the uranium is titrated directly using ammonium vanadate volumetric procedure The methods are simple and rapid and can be used to determine uranium in various samples The precision of analysis is over ± 10% and recovery rate is 98%～105%.The results are satisfactory

关 键 词：铀钼分离 铀 钼 测定 

分 类 号：TL214[核科学技术—核燃料循环与材料]