UO_2C_2O_4·TRPO配合物中有机磷的测定  

DETERMINATION OF ORGANIC PHOSPHOUS IN UO_2C_2O_4·TRPO COMPLEX

作　　者：郭一飞[1] 袁建华[1] 梁俊福[1] 焦荣洲[1] 刘秀琴[1] 

机构地区：[1]清华大学核能技术设计研究院,北京102201

出　　处：《核化学与放射化学》2001年第4期217-223,共7页Journal of Nuclear and Radiochemistry

摘　　要：以H2 SO4 HNO3 H2 O2 作氧化剂 ,采用湿式灰化法将UO2 C2 O4 ·TRPO配合物中的有机磷氧化成磷酸盐 ,并在 0 14mol/LH2 SO4 介质中 ,以水溶性聚乙烯醇为稳定剂 ,用碱性染料乙基紫与磷钼杂多蓝形成较高灵敏度的离子缔合物 ,在波长 6 2 0nm处用分光光度法测定磷含量。结果表明 ,当溶液中质量比Rm(UO2 2 + /P)≤ 1 4× 10 3 ,Rm(C2 O4 2 - /P)≤ 8 8× 10 2 和Rm(C2 O2 2 - /P)≤ 3 6×10 4 (1次湿式灰化 )时 ,可在水相中直接显色测定磷。与聚乙烯醇 罗丹明B 磷钼杂多蓝测定磷的方法进行对照 ,结果符合良好。本法对有机磷转化为无机磷的平均转化率为 99 8%～ 10 1 1% ,磷的检测限为 0 0 2mg/L ,相对标准偏差为 3% ,回收率为 97%～ 10 3%Organic phosphorus in UO 2C 2O 4·TRPO complex is converted to inorganic phosphorous with H 2SO 4 HNO 3 H 2O 2 wet cinefaction method. In 0.14 mol/L H 2SO 4 solution containing water soluble polyvinylalcohol as stabilizing agent, the highly sensitive ion associates are formed by the reacetion of basic dye ethyl violet with heteropoly molybdophosphoric blue. Spectrophotometric method is used for determination of phosphorus with these ion associates. The absorbance maximum is at 620 nm. Determination of phosphorus is not affected with mass ratioes R (UO 2 2+ /P) ≤1 4×10 3, R (C 2O 4 2- /P)≤8 8×10 2 and R (C 2O 4 2- /P)≤3 6×10 4 (one time wet cinefaction must be corried out). In aqueous phase, phosphorus can be directly developed and determinated. This method is contrasted with polyvinylalcohol Rodamine B heteropoly molybdophosphoric blue, analytical results are in good coincidence. Conversion ratio of phosphorus is 99.8 %～101.1 %. The minimum detection limit is 0.02 mg/L. The relative standard deviation is 3 %. The recovery ratio is 97 %～103 %.

关 键 词：UO2C2O4·TRPO 配合物 有机磷 湿式灰化法 分光光度法 测定 乏燃料后处理 二氧化铀 TOPO流程 萃取 

分 类 号：TL241.14[核科学技术—核燃料循环与材料]