1BP中铀钚价态及其含量的分析方法
Determination of Valence and Concentration of Uranium and Plutonium in 1BP Solution
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摘要: 建立了1BP工艺点铀钚价态及其含量的分析方法。通过研究不同价态铀钚的可见吸收光谱,采用多点斜率法拟合了不同价态铀钚在414、480、600、659 nm波长下的摩尔吸光系数ε。利用摩尔吸光系数ε结合多元线性回归法(MLR),建立了1BP中Pu(Ⅲ)、U(Ⅳ)、U(Ⅵ)及Pu(Ⅳ)分析的数学模型。该方法测量了1BP模拟样品:在工艺正常情况下,Pu(Ⅲ)的质量浓度范围为0.50~8.00 g/L,测量精密度优于3.0%(n=6),回收率为94.5%~103.9%;U(Ⅳ)的质量浓度范围为0.45~38.15 g/L,测量精密度优于3.0%(n=6),回收率为95.3%~104.7%;U(Ⅵ)的质量浓度范围为0.45~38.59 g/L,测量精密度优于3.0%(n=6),回收率为96.5%~103.0%;Pu总量的回收率为87.2%~100.6%。方法简单快速,精密度高,属于无损分析。Abstract: A method was developed for determination of valence and concentration of uranium and plutonium in 1BP solution. Absorbance spectrum is exploited in determining the concentration of uranium and plutonium which coexist in several different valences. The molar absorption coefficients of uranium and plutonium in different valences and different wave lengths were fitted by slope method. By which, a mathematical model based on multiple linear regression(MLR) was evaluated for analysis of Pu(Ⅲ), U(Ⅳ), U(Ⅵ) and Pu(Ⅳ) in 1BP solution. A series of synthetic solutions which mixed up different concentration of uranium and plutonium solution were prepared for validating the method. The results show this method has great advantages of determining the valence and concentration of uranium and plutonium in 1BP solution: that Pu(Ⅲ) can be determined in range of 0.50-8.00 g/L and the recovery is 94.5%-103.9%, U(Ⅳ) can be determined in range of 0.45-38.15 g/L and the recovery is 95.3%-104.7%, U(Ⅵ) can be determined in range of 0.45-38.59 g/L and the recovery is 96.5%-103.0%. The relate standard deviation of all the measuring results are less than 3.0%(n=6). The recovery of total plutonium is 87.2%-100.6%. In a word, the method is simple, fast, highly sensitive and non-destructive.
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Keywords:
- 1BP /
- uranium /
- plutonium /
- multiple linear regression
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[1] 王俊峰,章泽甫,张天祥,等.动力堆核燃料后处理工学[M].北京:中国原子能出版社,2013:187. [2] 任凤仪,周镇兴.国外核燃料后处理[M].北京:原子能出版社,2006:138-141. [3] 范明娥,居崇华.用分光光度法测定U(Ⅳ)、U(Ⅵ)、Pu(Ⅲ)和Pu(Ⅵ)含量的研究[J].原子能科学技术,1977,11(3):249-259. [4] 张俊霞,王利.仪器分析技术[M].重庆:重庆大学出版社,2015:23-24. [5] 倪力军,张立国.基础化学计量学及其应用[M].上海:华东理工大学出版社,2011:111-134. [6] 肖松涛,叶国安,刘协春,等.氨基羟基脲与Pu(Ⅳ)的动力学研究[J].原子能科学技术,2011,45(3):277-281. [7] 隗秀芳,张清轩.PMBP萃取法分析硝酸介质中钚的价态[J].原子能科学技术,1991,45(3):62-67. [8] 金惠民,朱荣保,谭亚军,等.混合式K边界技术及其应用的实验室研究(Ⅰ)[J].原子能科学技术,1998,32(3):193-200. [9] 胡晓丹,丁戈龙,刘文斌,等.核分析技术译文集[M].北京:原子能出版社,2008:132-141. [10] 吴文斌,王海生.GB/T 11848.1-2008硫酸亚铁还原-重铬酸钾滴定法[S].北京:中国标准出版社,2008. [11] 李斌,何辉,丁伯发,等.肼为还原剂催化还原U(Ⅵ)制备U(Ⅳ)的工艺条件[J].核化学与放射化学,2013,35(1):24-28.