As one of the most concerned radionuclides, ⁹⁹technetium (Tc) usually exists as pertechnetate (TcO₄⁻) and low-valence Tc(IV) in the environment. The speciation analysis of ⁹⁹Tc plays a crucial role in understanding its toxicity, bioavailability and mobility, and developing effective remediation strategies. However, conventional hyphenated techniques for ⁹⁹Tc speciation analysis usually require a large sample volume and tedious operation process. In this work, a simple but highly effective system, coupling capillary electrophoresis to inductively coupled plasma mass spectrometry (CE-ICP-MS), was developed to analyze total rhenium (TRe), Re(IV), and Re(VII), known as the analogues of technetium. It is worth noting that by the use of a sprayer with a direct-injection nebulizer as the interface, the CE and ICP-MS were efficiently coupled as an entity that shares the advantages of both modules. In comparison to conventional techniques, the proposed CE-ICP-MS dominates in terms of less sample consumption and higher sample introduction efficiency, thus results in improved sensitivity, reduced radioactive waste, and more significantly, alleviated radiological exposure to operators. Under the optimized conditions, LODs of 0.02 μg L⁻¹ and 0.01 μg L⁻¹ were obtained for TRe and Re(VII), respectively, with relative standard deviations (RSDs) better than 3.0%. In addition, the accuracy and practicability of this hyphenated system were validated by analyzing simulated Hanford site groundwater samples with satisfactory recovery and separation of TRe, Re(IV), and Re(VII). The proposed method retains the great potential for the speciation analysis of ⁹⁹Tc in various samples.

作为最有关的放射性核素中的一个，⁹⁹锝（Tc），通常存在如高锝酸盐（TCO ₄ ^- ）和（IV）在环境中的低化合价锝。⁹⁹ Tc的形态分析在理解其毒性，生物利用度和迁移性以及制定有效的补救策略方面起着至关重要的作用。但是，对于^99的常规连字技术Tc形态分析通常需要大量的样品和繁琐的操作过程。在这项工作中，开发了一种简单但高效的系统，将毛细管电泳与电感耦合等离子体质谱（CE-ICP-MS）耦合，以分析已知的总（（TRe），Re（IV）和Re（VII）。作为of的类似物。值得注意的是，通过使用带有直接喷射雾化器的喷雾器作为接口，CE和ICP-MS可以有效地结合在一起，成为共享这两个模块优点的实体。与传统技术相比，建议的CE-ICP-MS在减少样品消耗和提高样品引入效率方面占主导地位，从而提高了灵敏度，减少了放射性废物，并且更显着地减轻了操作员的放射线暴露。对于TRe和Re（VII）分别获得^-1和0.01μgL ^-1，相对标准偏差（RSD）优于3.0％。此外，通过分析模拟的汉福德场地地下水样品，对TRe，Re（IV）和Re（VII）进行了令人满意的回收和分离，验证了该联用系统的准确性和实用性。所提出的方法为各种样品中⁹⁹ Tc的形态分析保留了巨大的潜力。