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.
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