拉曼光谱结合偏最小二乘法定量分析锝洗槽工艺点样品中的锝  

Quantitative Determination of Technetium at TcS Section During the Spent Fuel Reprocessing

作　　者：张倩慈[1] 朱海巧[1] 常志远[1] 李定明[1] 白雪[1] 吴继宗[1] 

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：《核化学与放射化学》2017年第2期174-178,共5页Journal of Nuclear and Radiochemistry

摘　　要：核燃料后处理工艺流程中,锝洗槽中锝含量是一项重要的技术指标。本工作针对锝洗槽(TcS)工艺点,通过实验获得了拉曼光谱法测定锝浓度的数学模型,结合偏最小二乘法研究了不同建模波长及光谱预处理方法对模型的影响,建立了拉曼光谱法定量测定锝洗槽中锝浓度的分析方法。结果表明,校正标准偏差(RMSEC)为0.005,预测标准偏差(RMSEP)为0.004,r=0.999 3,该方法的检测下限为0.015g/L,精密度优于5%(n=6)。同时考察了铀酰离子浓度改变对锝测定结果的影响,当铀质量浓度为25.00~50.00g/L,对锝测量结果无显著影响。该方法分析速度快,无需预处理,可应用于锝洗槽工艺点中锝的分析。The concentration of Tc in technetium scrubbing section（TcS）is an important parameter in the spent fuel reprocessing.This work aims at the TcS point in PUREX process,and with the partial least square（PLS）and Raman spectroscopy the calibration models are established for the determination of pertechnetate.The results show that,the root mean square error of calibration（RMSEC）is 0.005,and the root mean square error of prediction（RMSEP）is 0.004 with the correlation coefficient of 0.999 3.The limit of detection of this method is 0.015g/L,and the precision is better than 5%（n=6）.In addition,the influence of UO_2^2＋ on the determination of Tc was studied in this work.It is found that there is no significant influence on the determination of Tc for the mass concentration of U ranging from 25.00 to 50.00g/L.This method is very fast and needs no pretreatment.It can be applied to the quantitative determination of Tc in TcS potentially.

关 键 词：锝洗槽 高锝酸根 拉曼光谱 偏最小二乘法 定量分析 

分 类 号：O657.37[理学—分析化学]