后处理料液中氨基羟基脲的分析方法研究  

Study on Analytical Method of Hydroxyl-semicarbazide in Reprocessing Solution

作　　者：钱红娟[1] 王玲[1] 张丽华[1] 刘焕良[1] 范德军[1] QIAN Hongjuan;WANG Ling;ZHANG Lihua;LIU Huanliang;FAN Dejun(Department of Radiochemistry,China Institute of Atomic Energy,Beijing 102413,China)

机构地区：[1]中国原子能科学研究院放射化学研究所,北京102413

出　　处：《原子能科学技术》2019年第5期789-796,共8页Atomic Energy Science and Technology

摘　　要：氨基羟基脲(HSC)是一种新型无盐试剂,可有效控制后处理料液中钚的价态,实现铀钚分离和钚的纯化,其含量是后处理工艺中的一项重要参数,需准确测定。本文根据HSC和对二甲氨基苯甲醛在酸性介质中发生显色反应,其产物在456 nm处有明显特征吸收的原理,建立了后处理料液中HSC的分析方法,并优化了分析条件。结果表明,HSC的最佳测量条件为测量波长456 nm、显色温度80～90℃(水浴)、显色时间45 min,NO^-_2、Fe^(3+)、N_2H_4及其他共存组分对HSC的测定无明显影响。HSC含量在2.5～60.0μmol/L范围内符合比耳定律,R^2为0.999 9,测量精密度优于5.0%。在45 d内工作曲线重复性好,具有良好的长期稳定性。真实样品的测量结果显示,其重加回收率在99%～105%之间。As a novel salt-free reductant in U/Pu separation and Pu purification process,hydroxyl-semicarbazide (HSC) can effectively adjust the valence of plutonium in reprocessing solutions,and its concentration is a vital parameter and necessary to be determined accurately.Under the catalysis of acid,color reaction between HSC and paradimethylaminobenzaldehyde can occur,which makes it possible to determine the concentration of HSC by spectrophotometry.Experimental results show that concentrations of HSC within 2.5-60.0 μmol/L with its absorptions conform to Beer law.The linear correlation coefficient R 2 is 0.999 9,the measuring precision of better than 5.0%,and the recoveries of actual samples are 95%-105%.Experimental results also show that the standard curves are good repeatability and conformity in 45 days.

关 键 词：氨基羟基脲 对二甲氨基苯甲醛 后处理料液 光度法 

分 类 号：O622.6[理学—有机化学] O652[理学—化学]