ICP-AES法测定二氧化镎粉末中的杂质元素
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摘要
建立了采用电感耦合等离子体发射光谱(ICP-AES)法测定二氧化镎粉末中Ca、Be、Cd等12种金属杂质元素含量的分析方法。采用HNO_3-HF混酸体系于聚四氟乙烯坩埚中溶解二氧化镎粉末样品,样品溶液进行调价后再用TEVA树脂柱进行预处理,接收的样品测试液采用ICP-AES法进行测量。结果表明,最佳分析条件为:取样量30 mg、样品溶解液采用过氧化氢在常温下调价约5 min、5 mol/L硝酸为淋洗液。在此条件下,元素的收率大于95%,各元素测量值的相对标准偏差为0.6%～4.8%(n=6),方法的加标回收率为93%～108%、检测限为0.07～8μg/g。
The determination method of impurity metal elements in the neptunium dioxide powder was built by ICP-AES, which could detect twelve impurity metal elements such as calcium, beryllium, cadmium, etc. In this work, a HNO_3-HF acid system was used to dissolve the neptunium dioxide powder in polytetrafluoroethylene crucible, then the solution was dealt with TEVA resin column after valence adjustment, and the sample test solution was detected by ICP-AES. The results show that the optimum analytical conditions are as follows: Sample dissolution adjusted with hydrogen peroxide about 5 min, sample amount of 30 mg, and 5 mol/L nitric acid as eluent. Under these conditions the recoveries of most elements are more than 95%, the relative standard deviations(n=6) are between 0.6% and 4.8% with 93%-108% recoveries, and the detection limits of this method are 0.07-8 μg/g.
The determination method of impurity metal elements in the neptunium dioxide powder was built by ICP-AES, which could detect twelve impurity metal elements such as calcium, beryllium, cadmium, etc. In this work, a HNO_3-HF acid system was used to dissolve the neptunium dioxide powder in polytetrafluoroethylene crucible, then the solution was dealt with TEVA resin column after valence adjustment, and the sample test solution was detected by ICP-AES. The results show that the optimum analytical conditions are as follows: Sample dissolution adjusted with hydrogen peroxide about 5 min, sample amount of 30 mg, and 5 mol/L nitric acid as eluent. Under these conditions the recoveries of most elements are more than 95%, the relative standard deviations(n=6) are between 0.6% and 4.8% with 93%-108% recoveries, and the detection limits of this method are 0.07-8 μg/g.
引文
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[12] 王江,韩小元,张瑞荣,等. 环境样品中237Np的ICP-MS分析研究进展[J]. 环境监测管理与技术,2010,22(3):11-19. WANG Jiang, HAN Xiaoyuan, ZHANG Ruirong, et al. Analysis advance of 237Np in environmental samples by inductively coupled plasma mass spectrometry[J]. The Administration and Technique of Environmental Monitoring, 2010, 22(3): 11-19(in Chinese).
[13] 刘勇,王怀胜,沈岚,等. 萃取分离ICP-AES法测定含铪铀中微量杂质元素[J]. 分析试验室,2002,21(1):55-57. LIU Yong, WANG Huaisheng, SHEN Lan, et al. Determination of impurity elements in U samples containing Hf by ICP-AES[J]. Chinese Journal of Analysis Laboratory, 2002, 21(1): 55-57(in Chinese).
[14] 王立平,冯海涛,董亚萍,等. 标准加入ICP-AES法测定铬酸钠中杂质元素[J]. 光谱学与光谱分析,2015,35(2):523-526. WANG Liping, FENG Haitao, DONG Yaping, et al. Standard addition determination of impurities in Na2CrO4 by ICP-AES[J]. Spectroscopy and Spectral Analysis, 2015, 35(2): 523-526(in Chinese).
[15] SHIGEO T, MASAHIKO Y, NAOKI S. Determination of neptunium in a reprocessing plant by an on-line solid-phase extraction/electrochemical detection system[J]. Journal of Radioanalytical and Nuclear Chemistry, 2014, 299: 1 539-1 545.
[16] ADYA V C, SENGUTA A, SK J, et al. Development of a methodology for the determination of trace metallic constituents in presence of neptunium[J]. Journal of Radioanalytical and Nuclear Chemistry, doi: 10.1007/s10967-015-4636-x.
[17] MAHANTY B, BHATTACHARYYA A, MOHAPATRA P K. Separation of neptunium(Ⅳ) from actinides by solid phase extraction using a resin containing Aliquat 336[J]. Journal of Chromatography A, doi: 10.1016/j.chroma.2018.06.026.
[18] GUSTOVA M V, MASLOV O D, SABEL'NIKOV A V. Application of TEVA resin for the separation of the products of photonuclear reaction 237Np(γ,n)236Np→(β-)236Pu[R]. Russia: Flerov Laboratory of Nuclear Reactions, 2016.
[19] 牟凌,李丰龙,覃波,等. PuO2粉末中杂质元素的ICP-AES测定[J]. 核化学与放射化学,2013,35(5):291-298. MU Ling, LI Fenglong, QIN Bo, et al. Determination technology of trace impurity elements in the PuO2 powder by ICP-AES[J]. Journal of Nuclear and Radiochemistry, 2013, 35(5): 291-298(in Chinese).
[20] 邹阳,杨远,罗悠,等. 电感耦合等离子体原子发射光谱(ICP-AES)法测定锂云母中的锂、钽、铌等7种元素[J]. 中国无机分析化学,2016,6(1):41-44. ZOU Yang, YANG Yuan, LUO You, et al. Determination of seven elements (lithium, tantalum, niobium, etc.) in lepidolite by inductively coupled plasma emission spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2016, 6(1): 41-44(in Chinese).
[2] 刘权卫,吴继宗,肖国平,等. 铀产品中镎和钚的分离与测定[J]. 核化学与放射化学,2008,30(3):178-183. LIU Quanwei, WU Jizong, XIAO Guoping, et al. Separation and determination of neptunium and plutonium in the uranium product[J]. Journal of Nuclear and Radiochemistry, 2008, 30(3): 178-183(in Chinese).
[3] 金花,苏玉兰,应浙聪,等. 大量钚中镎的分离方法[M]//中国原子能科学研究院年报. 北京:中国原子能出版社,2014.
[4] 高燕,郑永章,刘英,等. 阳离子交换富集/ICP-MS测定高纯硒中13种杂质[J]. 分析试验室,2011,30(5):35-39. GAO Yan, ZHENG Yongzhang, LIU Ying, et al. Determination of 13 impurities in high-purity selenium by ICP-AES after preconcentrated though cation exchange[J]. Chinese Journal of Analysis Laboratory, 2011, 30(5): 35-39(in Chinese).
[5] 吉艳琴,李金英,刘峻岭,等. 萃取色层分离ICP-MS测定环境样品中的Np[M]//中国原子能科学研究院年报. 北京:原子能出版社,2000.
[6] 辛仁轩,王建强. 色谱分离法测定高纯度八氧化三铀中的13种微量杂质[J]. 化学分析计量,2002,11(6):33-34. XING Renxuan, WANG Jianqiang. Determination of 13 elements in uranium by chromatography separation and ICP-AES[J]. Chemical Analysis and Meterage, 2002, 11(6): 33-34(in Chinese).
[7] 侯列奇,王树安. TBP柱上分离-ICP-AES法测定二氧化铀中微量杂质元素[J]. 理化检验:化学分册,1998(2):72-74. HOU Lieqi, WANG Shu'an. Determination of impurity elements in uranium dioxide by TBP column separation and ICP-AES[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis, 1998(2): 72-74(in Chinese).
[8] 杜方才,陈秋莲. 离子交换预分离富集-ICP-AES测定钽中微量杂质元素[J]. 硬质合金,2004,21(1):45-47.
[9] 梁俊福,康君波. 草酸体系中镎、钚的阴离子交换分离[J]. 原子能科学技术,2001,35(增刊):27-33. LIANG Junfu, KANG Junbo. Anion exchange separation of Np and Pu in oxalic acid system[J]. Atomic Energy Science and Technology, 2001, 35(Suppl.): 27-33(in Chinese).
[10] 朱道宏,张桂芹. 化学光谱法测定二氧化镎中八个杂质元素[J]. 原子能科学技术,1975(1):30-36.
[11] 包蕊,李建强,季春红,等. ICP-AES分析超导粉中杂质元素的干扰系数矩阵校正法[J]. 光谱学与光谱分析,2008,28(6):1 390-1 393. BAO Rui, LI Jianqiang, JI Chunhong, et al. Correction of spectral interference coefficient matrix for determination of impurities in bi-based superconductor powder by inductively coupled plasma emission spectrometry[J]. Spectroscopy and Spectral Analysis, 2008, 28(6): 1 390-1 393(in Chinese).
[12] 王江,韩小元,张瑞荣,等. 环境样品中237Np的ICP-MS分析研究进展[J]. 环境监测管理与技术,2010,22(3):11-19. WANG Jiang, HAN Xiaoyuan, ZHANG Ruirong, et al. Analysis advance of 237Np in environmental samples by inductively coupled plasma mass spectrometry[J]. The Administration and Technique of Environmental Monitoring, 2010, 22(3): 11-19(in Chinese).
[13] 刘勇,王怀胜,沈岚,等. 萃取分离ICP-AES法测定含铪铀中微量杂质元素[J]. 分析试验室,2002,21(1):55-57. LIU Yong, WANG Huaisheng, SHEN Lan, et al. Determination of impurity elements in U samples containing Hf by ICP-AES[J]. Chinese Journal of Analysis Laboratory, 2002, 21(1): 55-57(in Chinese).
[14] 王立平,冯海涛,董亚萍,等. 标准加入ICP-AES法测定铬酸钠中杂质元素[J]. 光谱学与光谱分析,2015,35(2):523-526. WANG Liping, FENG Haitao, DONG Yaping, et al. Standard addition determination of impurities in Na2CrO4 by ICP-AES[J]. Spectroscopy and Spectral Analysis, 2015, 35(2): 523-526(in Chinese).
[15] SHIGEO T, MASAHIKO Y, NAOKI S. Determination of neptunium in a reprocessing plant by an on-line solid-phase extraction/electrochemical detection system[J]. Journal of Radioanalytical and Nuclear Chemistry, 2014, 299: 1 539-1 545.
[16] ADYA V C, SENGUTA A, SK J, et al. Development of a methodology for the determination of trace metallic constituents in presence of neptunium[J]. Journal of Radioanalytical and Nuclear Chemistry, doi: 10.1007/s10967-015-4636-x.
[17] MAHANTY B, BHATTACHARYYA A, MOHAPATRA P K. Separation of neptunium(Ⅳ) from actinides by solid phase extraction using a resin containing Aliquat 336[J]. Journal of Chromatography A, doi: 10.1016/j.chroma.2018.06.026.
[18] GUSTOVA M V, MASLOV O D, SABEL'NIKOV A V. Application of TEVA resin for the separation of the products of photonuclear reaction 237Np(γ,n)236Np→(β-)236Pu[R]. Russia: Flerov Laboratory of Nuclear Reactions, 2016.
[19] 牟凌,李丰龙,覃波,等. PuO2粉末中杂质元素的ICP-AES测定[J]. 核化学与放射化学,2013,35(5):291-298. MU Ling, LI Fenglong, QIN Bo, et al. Determination technology of trace impurity elements in the PuO2 powder by ICP-AES[J]. Journal of Nuclear and Radiochemistry, 2013, 35(5): 291-298(in Chinese).
[20] 邹阳,杨远,罗悠,等. 电感耦合等离子体原子发射光谱(ICP-AES)法测定锂云母中的锂、钽、铌等7种元素[J]. 中国无机分析化学,2016,6(1):41-44. ZOU Yang, YANG Yuan, LUO You, et al. Determination of seven elements (lithium, tantalum, niobium, etc.) in lepidolite by inductively coupled plasma emission spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2016, 6(1): 41-44(in Chinese).