碱熔-丁二酮肟分离-电感耦合等离子发射光谱(ICP-OES)法测定钯灰中钯含量
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作者单位:

1.昆明理工大学 国土资源工程学院, 云南 昆明 650093 ; 2.云南省战略金属矿产资源绿色分离与富集重点试验室, 云南 昆明 650093 ;3.西南联合研究生院, 云南 昆明 650093 ; 4.贵研检测科技(云南)有限公司, 云南 昆明 650106

作者简介:

鲁瑞智(1987—),云南昆明人,硕士研究生,工程师,研究方向为矿产资源分析与综合利用。

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中图分类号:

O657.31

基金项目:

云南省西南联合研究生院科技专项“复杂锰银多金属共生矿梯度磁选-化学分离-胶体聚沉新方法”(202302AO370002);云南省磷资源技术创新中心“智能开采与绿色分选技术研究”(202305AK340002)


Determination of palladium content in palladium ash by inductively coupled plasma emission spectrometry (ICP-OES) with alkali fusion- butyl diketoxime separation
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1.Faculty of Land Resource Engineering,Kunming University of Science and Technology, Kunming 650093 , China ; 2.Yunnan Key Laboratory of Green Separation and Enrichment of Strategic Mineral Resources, Kunming 650093 , China ; 3.Southwest United Graduate School, Kunming 650093 , China ; 4.Sino-Platinum Metals Testing Technology(Yunnan)Co., Ltd., Kunming 650106 , China

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    摘要:

    我国对钯资源市场需求量很大,但储量匮乏,回收含钯二次资源对我国的工业发展意义重大。钯灰是回收含钯二次资源过程的一种产物,建立一种快速、准确、易掌握的检测方法为提高钯回收率和贸易提供了有力保障。本文采用过氧化钠在750±10℃对试样进行熔融后用盐酸浸出分解试样,加入丁二酮肟络合钯形成沉淀后分离杂质,再通过盐酸-过氧化氢返溶丁二酮肟钯沉淀;使用电感耦合等离子发射光谱在最佳工作条件下对试样进行测定,选择分析谱线Pd340.458nm计算结果。该方法分别与碱熔-碲共沉淀法、密闭消解法和容量法比对,测定结果高度吻合,方法加标回收率为97.8%~100.7%,相对标准偏差(RSD)为0.36%~0.80%,测定范围为1%~15%,是一种简单、高效、准确的检测方法。

    Abstract:

    Palladium resource market in China has a large demand but lack of reserves. The recovery of secondary palladium resources is of great significance to the industrial development of our country. Palladium ash is the product of palladium containing secondary resources recovery. Establishing a rapid, accurate and easy-to-master detection method provides a strong guarantee for improving palladium recovery and trade. In this paper, the sample was melt with sodium peroxide at 750±10℃, The impurities are separated after palladium complexation by diketoxime is precipitated, and then through hydrochloric acid-hydrogen peroxide resolubilization of palladium butanedione oxime precipitated,the contents of palladium were determination by inductively coupled plasma emission spectrometry (ICP-OES) under optimal operating conditions. It is selection wavelength Pd340.458nm to result computation.The results of this method are highly consistent with alkali melt-telluriumco-precipitation, acid dissolution and volumetric method. The recoveries were 98.2%~100.8% and the relative standard deviation (RSD) was 0.36%~0.80% and the measurement range was 1%~15%. This method is a simple, efficient and accurate method.

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鲁瑞智, 申培伦, 谢海云,等. 碱熔-丁二酮肟分离-电感耦合等离子发射光谱(ICP-OES)法测定钯灰中钯含量[J].中国有色冶金,2025,54(2):107-113.

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  • 收稿日期:2024-10-11
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  • 在线发布日期: 2025-12-18
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