氢化物发生-电感耦合等离子体发射光谱法测定铀矿地质样品中痕量硒
| 1. | 河南省核工业放射性核素检测中心, 河南郑州 450044 |
| 2. | 珀金埃尔默仪器(上海)有限公司, 上海 201203 |
Determination of Trace Selenium in Uranium-bearing Geological Samples by Hydride Generation-Inductively Coupled Plasma-Optimal Emission Spectrometry
| 1. | Henan Radionuclide Detection Center of Nuclear Industry, Zhengzhou 450044, China |
| 2. | PerkinElmer Instruments(Shanghai) Co., LTD, Shanghai 201203, China |
摘要：采用氢化物发生技术测定地质样品中的硒时, 需要考虑样品的溶解、Se价态的预还原以及抑制共存离子的干扰。本文采用硝酸-盐酸-氢氟酸-高氯酸体系快速溶解样品, 直接加入浓盐酸煮沸将六价硒还原为四价硒, 将氢化物发生器与电感耦合等离子体发射光谱仪联用测定了铀矿地质样品中的痕量硒。样品中除了Cu2+其他离子的含量均不干扰硒的测定, 通过在试液中加入铁盐溶液或在硼氢化钠还原剂中加入铁氰化钾抑制了Cu2+的干扰。方法检出限为0.12μg/L, 精密度(RSD)小于5%。与前人报道的方法相比, 本方法检出限较低, 操作简单快速, 冲洗30 s可消除记忆效应, 适合批量铀矿地质样品中痕量硒的测定。
Determination of Trace Selenium in Uranium-bearing Geological Samples by Hydride Generation-Inductively Coupled Plasma-Optimal Emission Spectrometry
ABSTRACT Using hydride generation to determine selenium in geological samples, the sample dissolution, selenium pre-reduction and the suppression of coexisting ion interference should be considered. In this study, concentrated hydrochloric acid was added to reduce Se(Ⅵ) to Se(Ⅳ) after the sample was dissolved by nitric acid, hydrochloric acid, hydrofluoric acid and perchloric acid. The trace selenium in the sample was determined by hydride generator coupled with Inductively Coupled Plasma-Optimal Emission Spectrometry (ICP-OES). The ions in the sample had no interference on the determination of selenium except Cu2+. Adding ferric salt solution to the sample solution or adding potassium ferricyanide to the reductant are beneficial to suppress the interference of Cu2+. The detection limit of this method was 0.12 μg/L, which is lower than that of a previous study, and RSD was less than 5%. The method was rapid and needed 30 seconds rinsing to eliminate the memory effect, which makes it suitable for the determination of trace selenium in uranium-bearing geological samples.
本文参考文献
| [1] |
苏文峰, 李刚. 焙烧分离-氢化物发生-原子荧光光谱法测定土壤样品中微量硒[J]. 岩矿测试, 2008, 27(2): 120-122. Su W F, Li G. Determination of Trace Selenium in Soil Samples by Hydride Generation-Atomic Fluorescence Spectrometry with Baking Separation[J]. Rock and Mineral Analysis, 2008, 27(2): 120-122. |
| [2] |
Zhang N, Sun G L, Ma H R, et al. Determination of Ultra-trace Selenium in Mineral Samples by Hydride Generation Atomic Fluorescence Spectrometry with Pressurized-PTFE-vessel Acid Digestion[J].Minerals Engineering, 2007, 20(15): 1397-1400. doi: 10.1016/j.mineng.2007.09.001 |
| [3] |
柴昌信, 陈世焱, 陈月源, 等. 氢化物发生-原子荧光光谱法直接测定多金属矿中的硒和碲[J]. 岩矿测试, 2009, 28(2): 143-146. Chai C X, Chen S Y, Chen Y Y, et al. Determination of Selenium and Tellurium in Polymetallic Minerals by Hydride-generation Atomic Fluorescence Spectrophoto-metry[J]. Rock and Mineral Analysis, 2009, 28(2): 143-146. |
| [4] |
王世成, 王颜红, 刘艳辉, 等. 氢化物发生-原子荧光法测定鸭蛋中无机硒和有机硒[J]. 食品科学, 2013, 34(4): 183-185. Wang S C, Wang Y H, Liu Y H, et al. Determination of Inorganic and Organic Selenium in Duck Eggs by Hydride Generation-Atomic Fluorescence Spectrometry[J]. Food Science, 2013, 34(4): 183-185. |
| [5] |
Wei L, Gupta P, Hernandez R, et al. Determination of Ultratrace Selenium and Arsenic at Parts-per-Trillion Levels in Environmental and Biological Samples by Atomic Fluorescence Spectrometry with Flow Injection Hydride Generation Technique[J].Microchemical Journal, 1999, 62(1): 83-98. doi: 10.1006/mchj.1998.1698 |
| [6] |
刘爽, 刘冬莲. 氢化物发生-原子吸收光谱法测定黄芪中硒[J]. 理化检验(化学分册), 2013, 49(1): 81-83. Liu S, Liu D L. HG-AAS Determination of Selenium in Astragalus[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2013, 49(1): 81-83. |
| [7] |
Maleki N, Safavi A, Doroodmand M M, et al. Determination of Selenium in Water and Soil by Hydride Generation Atomic Absorption Spectrometry Using Solid Reagents[J].Talanta, 2004, 66(4): 858-862. |
| [8] |
汪李, 杨远, 易可慧, 等. 氢化物发生-电感耦合等离子体原子发射光谱法测定血样中硒含量[J]. 理化检验(化学分册), 2013, 49(3): 287-289. Wang L, Yang Y, Yi K H, et al. HG-ICP-AES Determination of Selenium in Blood Sample[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2013, 49(3): 287-289. |
| [9] |
辛仁轩. 等离子体发射光谱分析[M] . 北京: 化学工业出版社, 2005: 381-382. Xin R X. Plasma Emission Spectrum Analysis[M] . Beijing: Chemical Industry Press, 2005: 381-382. |
| [10] |
杨金辉, 杨江柳, 胡鄂明, 等. 电感耦合等离子体发射光谱法(ICP-AES)测定铀矿石中微量钪、硒、铼[J]. 南华大学学报(自然科学版), 2004, 18(4): 83-85. Yang J H, Yang J L, Hu E M, et al. The Determination of Sc, Se and Re in Uranium Ore with ICP-AES[J]. Journal of Nanhua University (Science and Technology), 2004, 18(4): 83-85. |
| [11] |
龚治湘, 麻映文. 微型氢化物发生原子吸收光谱法测定砂岩铀矿中微量硒[J]. 分析化学, 2005, 33(6): 831-834. Gong Z X, Ma Y W. Determination of Trace Selenium in Uranium Mineral by Hydride-Generation-Atomic Absorption Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2005, 33(6): 831-834. |
| [12] |
贺攀红, 吴领军, 杨珍, 等. 氢化物发生-电感耦合等离子体发射光谱法同时测定土壤中痕量砷锑铋汞[J]. 岩矿测试, 2013, 32(2): 240-243. He P H, Wu L J, Yang Z, et al. Simultaneous Determination of Trace As, Sb, Bi and Hg in Soils by Hydride Generation-Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2013, 32(2): 240-243. |
| [13] |
陈波, 刘洪青, 邢应香, 等. 电感耦合等离子体质谱法同时测定地质样品中锗硒碲[J]. 岩矿测试, 2014, 33(2): 192-196. Chen B, Liu H Q, Xing Y X, et al. Simultaneous Determination of Ge, Se and Te in Geological Samples by Inductively Coupled Plasma-Mass Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(2): 192-196. |
| [14] |
李岩, 袁爱萍. 碱熔-氢化物发生原子荧光光谱法连续测定锑精矿中的砷铋硒锡[J]. 分析化学, 2008, 36(9): 273-276. Li Y, Yuan A P. Simultaneous Determination of As, Bi, Se and Sn in Antimony Concentrates by Hydride Generation-Atomic Fluorescence Spectrometry through Sodium Peroxide Melting[J]. Chinese Journal of Analytical Chemistry, 2008, 36(9): 273-276. |
| [15] |
傅慧敏, 周益奇, 王巧环, 等. 氢化物发生-电感耦合等离子体原子发射光谱法测定环境样品中痕量硒[J]. 理化检验(化学分册), 2015, 51(2): 157-159. Fu H M, Zhou Y Q, Wang Q H, et al. Determination of Trace Amount of Se in Environmental Samples by HG-ICP-AES[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2015, 51(2): 157-159. |
| [16] |
Pohl P, Zyrnicki W. Study of Chemical and Spectral Interferences in the Simultaneous Determination of As, Bi, Sb, Se and Sn by Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry[J].Analytica Chimica Acta, 2002, 468(1): 71-79. doi: 10.1016/S0003-2670(02)00602-5 |
| [17] |
D'Ulivo A, Gianfranceschi L, Lampugnani L, et al. Masking Agents in the Determination of Selenium by Hydride Generation Technique[J].Spectrochimica Acta Part B:Atomic Spectroscopy, 2002, 57(12): 2081-2094. doi: 10.1016/S0584-8547(02)00166-0 |
| [18] |
杨理勤. Fe3+、碲对硒的氢化物化学干扰机理的实验研究[J]. 光谱学与光谱分析, 1999, 19(6): 399-401. Yang L Q. Experimental Study on the Mechanism of Chemical Interference of Tellurium with Selenium by Hydride-AFS in the Presence of Fe3+[J].Spectroscopy and Spectral Analysis, 1999, 19(6): 399-401. |
| [19] |
陶秋丽, 韩张雄, 熊英, 等. 微波消解-氢化物发生原子荧光光谱法测定粉煤灰中的硒[J]. 岩矿测试, 2013, 32(3): 445-448. Tao Q L, Han Z X, Xiong Y, et al. Determination of Selenium in Coal Ash with Microwave Digestion and Hydride Generation-Atomic Fluorescence Spectrometry[J]. Rock and Mineral Analysis, 2013, 32(3): 445-448. |
| [20] |
金未, 赵承易, 王水锋, 等. 氢化物发生-电感耦合等离子体原子发射光谱法测定环境样品中的痕量硒[J]. 北京师范大学学报(自然科学版), 2005, 41(4): 389-392. Jin W, Zhao C Y, Wang S F, et al. Determination of Trace Selenium in Environmental Samples by Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Journal of Beijing Normal University (Natural Science), 2005, 41(4): 389-392. |
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