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含碘附银硅胶是附银硅胶与放射性碘发生吸附反应形成的固体废物，其银含量的准确测定对研究其吸附性能及放射性碘净化处理具有重要意义。含碘附银硅胶中的银主要以碘化银的形式存在，碘化银较难溶解，且银含量较高，这一特性使银的准确测定变得十分困难。旨在建立一种准确测定含碘附银硅胶中高含量银的分析方法。以硝酸和氢氟酸体系消解样品，其中硝酸氧化碘离子生成碘单质，加热使碘挥发，促进碘化银的溶解，氢氟酸用于去除硅胶基体。消解后，在盐酸-硫脲介质中提取银，并采用电感耦合等离子体原子发射光谱法（ICP-OES）进行测定。本研究考察了硝酸和氢氟酸用量、盐酸浓度及硫脲的体积对测定结果的影响，结果表明：硝酸和氢氟酸用量对消解效果影响较小，而盐酸浓度和硫脲用量是影响银含量测定结果的关键因素，适量硫脲在酸性条件下能有效增强银的溶解能力。对样品进行精密度和准确度实验，结果显示：该方法精密度优于5%，加标回收率介于95.8%～104.0%之间，表明该方法具有较好的重复性和准确性。因此该方法适用于含碘附银硅胶中高含量银的测定，为该类复杂基质中银的分析提供了有效技术手段。
Abstract：Silver-loaded silica gel with iodine is a solid waste formed from the reaction of silver-loaded silica gel and radioactive iodine. The accurate determination of silver content is of great significance for studying its adsorption performance and radioactive iodine purification. Silver in silver-loaded silica gel with iodine mainly exists in the form of silver iodide, which is of high content and poorly soluble, making the accurate determination of silver quite challenging. This study aims to establish a reliable analytical method for the determination of high silver content in silver-loaded silica gel with iodine. Samples were digested using a nitric acid-hydrofluoric acid system, where nitric acid oxidizes iodide ions to iodine, which volatilizes upon heating to promote the decomposition of silver iodide, while hydrofluoric acid removes the silica gel matrix. After digestion, silver was extracted in a hydrochloric acid-thiourea medium and determined by inductively coupled plasma atomic emission spectrometry(ICP-OES). The effects of nitric acid and hydrofluoric acid dosage,hydrochloric acid concentration,and thiourea volume on the determination results were investigated. The results show that the dosage of nitric acid and hydrofluoric acid had little effect on digestion efficiency,while hydrochloric acid concentration and thiourea volume were the key factors affecting silver content. An appropriate amount of thiourea can effectively enhance silver solubility under acidic conditions. Precision and accuracy experiments were conducted on samples, with relative standard deviations(RSD) below 5 % and spiked recoveries ranging from 95.8 % to 104.0 %. The results show that the method has good repeatability and accuracy. In conclusion, this method is suitable for the determination of high silver content in silver-loaded silica gel with iodine and provides an effective technical means for the analysis of silver in such complex matrices.
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基本信息:
中图分类号:TL24;O657.31
引用信息:
[1]王利,谢胜凯,张良圣,等.电感耦合等离子体原子发射光谱(ICP-OES)法测定含碘附银硅胶中的高含量银[J].世界核地质科学,2026,43(01):109-116.
基金信息:
中国原子能科学研究院碘废物固化技术研究项目（编号：BG202306000322）资助~~
2026-01-14
2026-01-14
2026-01-14