采用ICP-OES方法测定高银硝酸分解液与沉钯后液中铂、钯
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湖南水口山有色金属有限责任公司, 湖南 衡阳 421513

作者简介:

李红湘(1994—),女,湖南衡阳人,硕士研究生,从事矿产资源综合利用与无机分析方法研究工作。

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TF03

基金项目:

水口山有色金属有限责任公司青年基金项目(2021)


Detection of platinum and palladium in high-silver nitric acid decomposition solution and palladium precipitated liquid by ICP-OES method
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Hunan Shuikoushan Nonferrous Metals Co.Ltd, Hengyang 421513 , China

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    摘要:

    铂、钯属于重要的贵金属,与其他金属伴生,常可在电解银过程中进行回收。某冶炼企业在生产银产品过程中,需要对高银硝酸分解液和沉钯后液进行铂、钯测定以控制生产。电感耦合等离子体发射光谱法(ICP-OES)具有灵敏度高、检出限低、线性范围广、可同时检验多种元素、快速准确等优点,近年应用较广,但目前文献中还没有应用到对高银硝酸分解液和沉钯后液中铂、钯的测定。本文采用ICP-OES方法对高银硝酸分解液与沉钯后液中的铂、钯进行了测定试验,对比了高银基体干扰、有机沉钯剂干扰、火法试金富集、不同酸介质等试样的测定结果,得出以下结论:基体干扰现象不明显,无需分离银基体;有机物沉钯剂对测定结果无影响;硫酸黏稠度较大,使得测定结果有所偏差,最佳消解方法应为硝酸体系消解;火试金富集方法因合粒含银高,所得值钯偏低30%,铂偏低38%,损耗较大;采用硝酸体系消解,并采用ICP-OES方法测定高银硝酸分解液与沉钯后液中铂、钯,加标回收率在95%~105%以内,相对标准偏差低于5%,测定结果稳定、可靠。试验表明,该法操作便捷,无需发烟、过滤、火试金等繁琐步骤,实用性强,可用于稀贵钯回收项目中高银硝酸分解液与沉钯后液中铂、钯的实际分析工作。

    Abstract:

    Platinum and palladium are important precious metals, which are often recovered in the process of electrolytic silver. In the process of producing silver products, a smelting enterprise needs to determine platinum and palladium in high-silver nitric acid decomposition solution and palladium precipitation solution. Inductively coupled plasma optical emission spectrometry (ICP-OES ) has the advantages of high sensitivity, low detection limit, wide linear range, simultaneous detection of multiple elements, rapid and accurate, and has been widely used in recent years. However, the method to the determination of platinum and palladium in nitric acid decomposition solution and palladium precipitation solution has not been applied in the present literature. In this paper, ICP-OES method was used to determine platinum and palladium in high-silver nitric acid decomposition solution and palladium precipitation solution. The results of high-silver matrix interference test, organic palladium precipitation agent interference test, fire assay enrichment test and different acid media tests were compared. The following conclusions are drawn. The silver matrix interference phenomenon is not obvious, and there is no need to separate the silver matrix. The organic palladium precipitation agent has no interference on the determination results. The viscosity of sulfuric acid makes the determination results deviate, and the best digestion method should be nitric acid system digestion. The results of the fire assay enrichment method is 30% lower for palladium and 38% lower for platinum, and the loss is large. Platinum and palladium in high-silver nitric acid decomposition solution and palladium precipitation solution were determined by ICP-OES method after digestion with nitric acid system, and the recovery rate was within 95%-105%, and the relative standard deviation was less than 5%, which were stable and reliable. The test shows that the method is convenient to operate and has strong practicability. It can be used for actual analysis of platinum and palladium in high-silver nitric acid decomposition solution and palladium precipitation solution.

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李红湘, 蔡亚飞, 揭辉, 等. 采用ICP-OES方法测定高银硝酸分解液与沉钯后液中铂、钯 [J]. 中国有色冶金, 2023, 52(2): 81-87.

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  • 收稿日期:2022-11-21
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  • 在线发布日期: 2025-12-23
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