X射线荧光光谱法测定硝酸铒溶液中铒

Determination of erbium in erbium nitrate solution by X-ray fluorescence spectrometry

铒在核反应堆中常做为可燃毒物,该类可燃毒物在制造过程中需对铒进行精确测量,即对工艺过程中的硝酸铒溶液中铒进行测量。实验建立了X射线荧光光谱法(XRF)测定硝酸铒溶液中铒含量的分析方法。结果表明,当选择LiF200晶体时,铒的角度扫描图峰形比较完整;当选择准直器150μm时,铒的峰背比最为好;当选择功率为40kV×40mA时,仪器的综合性能和计数率比较好。铒的质量浓度在1~15mg/mL范围内与其特征线ErLα的强度呈线性,校准曲线的相关系数为0.993 6。对硝酸铒标准溶液和硝酸铒实际样品溶液进行测定,并与电感耦合等离子体原子发射光谱(ICP-AES)的测定结果进行比对,两种方法的测定结果一致,实验方法测定结果的相对标准偏差(RSD,n=6)低于0.7%。

Erbium is usually used as burnable poison in nuclear reactor.The content of erbium in this type of burnable poison should be accurately determined in production process.In other words,it is necessary to measure the content of erbium in erbium nitrate solution.The analysis method of erbium in erbium nitrate solution by X-ray fluorescence spectrometry（XRF）was established.The results showed that the peak shape of erbium in angle scanning was relatively complete when LiF200 crystal was selected.The peak-to-background ratio of erbium was best when 150μm-collimator was used.In addition,the overall performance and count rate of instrument were good when the power was 40kV×40mA.The mass concentration of erbium in range of 1-15 mg/mL was linear to the strength of characteristic line ErLα.The correlation coefficient of calibration curve was 0.993 6.The erbium nitrate standard solution and actual erbium nitrate sample were determined according to the experimental method.The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry（ICP-AES）.The relative standard deviations（RSD,n=6）were less than 0.7%.