In this study, a new purification procedure for high precision Sb isotopic analysis was developed by using a thiol silica gel column and is applied to determine Sb isotope composition in natural water samples affected by mining activities. In our proposed procedure, Sb(V) was firstly pre-reduced with 0.5% (w/v) KI–ascorbic acid mixed solution and then Sb(III) in the solution could be separated and purified simply by elution with hydrochloric acid. With the developed procedure, the recovery of antimony was greater than 95.2% and blank values were <0.1 ng. An Apex Ω desolvating sample introduction system was used to improve the sensitivity during Sb isotopic measurement by MC-ICP-MS, and the instrumental mass discrimination was corrected using the sample–standard bracketing (SSB) method combined with the In doping technique. Isobaric effects, matrix effects, and concentration effects were all investigated in detail. ¹²³Sb/¹²¹Sb ratios could be measured with a precision of 0.04‰ (2SD). To verify the reliability of the new method, both matrix containing mixed interference elements and a simulated matrix prepared by Sb standard reference material BHVO-2 doping with Spex Sb standard solution were determined. No measurable Sb isotope fractionation was observed with the developed thiol silica gel column procedure. Finally, natural water samples collected from Lengshuijiang were analysed, and significant Sb isotope variations (−0.20 to 0.27‰) were observed, which suggests that Sb isotopes may provide a promising tool to study antimony migration and pollution.

中文翻译：

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基于硫醇硅胶柱的新型纯化方法，用于高精度锑同位素测量

在这项研究中，通过使用硫醇硅胶柱开发了一种用于高精度Sb同位素分析的新纯化程序，并将其用于确定受采矿活动影响的天然水样品中Sb同位素组成。在我们提出的程序中，先用0.5％（w / v）KI-抗坏血酸混合溶液预先还原Sb（V），然后再用Sb（III）还原。溶液中的）可以分离并简单地通过用盐酸洗脱进行纯化。通过开发的程序，锑的回收率大于95.2％，空白值小于0.1 ng。使用ApexΩ脱溶剂样品引入系统提高了通过MC-ICP-MS测定Sb同位素过程中的灵敏度，并使用样品标准包围（SSB）方法和In掺杂技术校正了仪器的质量歧视。等压效应，基质效应和浓度效应均已详细研究。¹²³ Sb / ¹²¹Sb比率的测量精度为0.04‰（2SD）。为了验证新方法的可靠性，确定了含有混合干扰元素的基质和由掺有Spex Sb标准溶液的Sb标准参考材料BHVO-2制备的模拟基质。用已开发的硫醇硅胶柱程序未观察到可测量的Sb同位素分级分离。最后，从冷水江采集的天然水样进行了分析，并观察到了Sb同位素的显着变化（-0.20至0.27‰），这表明Sb同位素可能是研究锑迁移和污染的有前途的工具。