电感耦合等离子体原子发射光谱法测定铀铌混合氧化物中镉、锡和锌
ICP-AES Determination of Cd, Sn and Zn in Uranium-Niobium Mixed Oxide
摘 要
铀铌混合氧化物样品0.200 0 g用硝酸8 mL，氢氟酸2 mL进行微波消解后，经苯乙烯-二乙烯苯-磷酸三丁酯萃取柱分离铀与镉、锡、锌，采用电感耦合等离子体原子发射光谱法测定淋洗液中镉、锡和锌的含量。选择镉、锡、锌的分析谱线依次为226.502，189.989，213.856 nm。3种元素的质量浓度均在一定范围内与其对应的发射强度呈线性关系，方法的检出限（3s）为0.003~0.02 mg·L-1。加标回收率为94.0%~101%，测定值的相对标准偏差（n=6）为3.7%~7.4%。
铀铌混合氧化物
元素
ICP-AES
uranium-niobium mixed oxide
element
Abstract
The uranium-niobium mixed oxide sample (0.200 0 g) was digested with HNO3 (8 mL) and HF (2 mL) in microwave system. The CL-TBP extraction column was used to separate Cd, Sn and Zn from U. ICP-AES was applied to the determination of Cd, Sn and Zn in eluent. Analytical spectral lines of 226.502, 189.989 and 213.856 nm were chosen for the determination of Cd, Sn and Zn respectively. Linear relationships between values of emission intensity and mass concentration of the 3 elements were kept in definite ranges, with detection limits (3s) in the range of 0.003-0.02 mg·L-1. Values of recovery found by standard addition method were in the range of 94.0%-101%, and values of RSD's (n=6) in the range of 3.7%-7.4%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201802015
所属栏目 工作简报
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收稿日期 2017/2/3
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备注杨平(1969-),男,河南驻马店人,技师,研究方向为核燃料及材料化学分析,yp0610@163.com
引用该论文: YANG Ping,WANG Peng,FEI Hao,WANG Zhanming. ICP-AES Determination of Cd, Sn and Zn in Uranium-Niobium Mixed Oxide[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 196～199
杨平,王鹏,费浩,王占明. 电感耦合等离子体原子发射光谱法测定铀铌混合氧化物中镉、锡和锌[J]. 理化检验－化学分册, 2018, 54(2): 196～199
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参考文献
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【2】VIJAYALAKSHMI S, KRISHMA P R, MAHALINGAM T R, et al. Determination of trace metal by inductively coupled plasma mass specfrometry combined with on-line solvent extraction[J]. Journal of Analytical Atomic Spectrometry, 1992,7(3):565-569.
【3】FLOYD M A, MORROW R, FARRAR R B. Inductively coupled plasma-atomic emission spectroscopy the determination of trace impurities in uranium hexafluoride[J]. Spectrochimica Acta, 1983,38(1/2):303-308.
【4】费浩,倪智勇.八氧化三铀中锆测定方法的研究[J].光谱实验室, 2008,25(5):784-787.
【5】刘虎生,冯斌,潘彦霖.电感耦合等离子体发射光谱法测定八氧化三铀中痕量杂质元素[J].分析化学, 1991,19(2):203-206.
【6】吉艳琴,李金英,罗上庚.TOPO萃取色层分离-ICP-MS法测定土壤中痕量铀的同位素丰度比[J].核化学与放射化学, 2004,26(2):89-94.
【7】CROZET M, GUIGUE M. Separation of actinides by extraction chromatography prior to X-ray fluorescence measurement for analytical control of a purex test[J]. Radiochim, 2007,95:629-635.
【8】MORGENSTEM A, APOSTOLIDIS C, CARLOS-MARQUEZ R, et al. Single-column extraction chromatographic separation of U, Pu, Np and Am[J]. Radiochim Acta, 2002,90:81-85.
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