基体分离-ICP光谱法测试99.999%高纯银中杂质元素
Determination of Impurity Elements in 99.999%Pure Silver by Matrix Separation-ICP Spectroscopy
李尚远 1赵鲁国 1徐剑瑛 2王绍娟 2陈红灵2
作者信息
- 1. 山东招金金银精炼有限公司,山东 烟台 265400
- 2. 山东招金金银精炼有限公司,山东 烟台 265400;中恒诺贵金属检测有限公司,山东 烟台 265400
- 折叠
摘要
研究建立了一种通过基体分离-ICP光谱法测试 99.999%高纯银中杂质元素的分析方法.通过加入硝酸溶解高纯银,加入盐酸沉淀银离子,加入王水煮氯化银沉淀,最后合并滤液浓缩体积的方式制备待测试液.试液经过定容后,使用ICP光谱仪进行测试.标准曲线在 0～1.0 mg/L的范围内,28 种杂质元素质量浓度的线性拟合良好,相关系数均大于0.999 4.铝、铁、镁元素检出限为 0.000 02%,定量限为 0.000 07%;其它杂质元素检出限为 0.000 01%,定量限为 0.00002%.在 4 个不同梯度的加标浓度下,方法的加标回收率分别为 93.0%～105.0%、94.5%～104.0%、94.5%～104.3%、95.3%～105.0%,检测结果相对标准偏差(RSD)分别为0.64%～7.37%、0.70%～5.64%、0.98%～3.66%、1.04%～5.89%.对同一样品采用辉光放电质谱法与本方法进行比对,测试结果基本无差异.实验结果表明该方法适用于 99.999%高纯银中 28种杂质元素的测定.
Abstract
A method for the determination of impurity elements in 99.999%pure silver by matrix separation-ICP spectroscopy was developed.The solution to be tested was prepared by adding nitric acid to dissolve high pure silver,adding hydrochloric acid to precipitate silver ions,adding aqua regia to precipitate silver chloride,and finally combining filtrate concentration volume.The liquid was tested by ICP spectrometer after constant volume.In the range of 0～1.0 mg/L,the mass concentrations of 28 impurity elements were linearly fitted well,and the correlation coefficients were all greater than 0.999 4.The detection limit of aluminum,iron and magnesium was 0.000 02%,and the limit of quantification was 0.000 07%.The detection limit of other impurity elements is 0.000 01%,and the limit of quantification is 0.000 02%.The recoveries were 93.0%～105.0%,94.5%～104.0%,94.5%～104.3%and 95.3%～105.0%,respectively,under four different gradient concentrations.Testing results of relative standard deviation(RSD)were 0.64%～7.37%,0.70%～5.64%and 0.98%～3.66%,1.04%～5.89%.The same sample was compared with this method by Glow-discharge mass spectrometry,and the test results showed no difference.The experimental results show that the method is suitable for the determination of 28 impurity elements in 99.999%pure silver.
关键词
基体分离/ICP光谱法/99.999%高纯银/杂质元素Key words
matrix separation/ICP spectroscopy/99.999%sterling silver/impurity element引用本文复制引用
出版年
2024
NETL
NSTL
万方数据