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基体分离-ICP光谱法测试99.999%高纯银中杂质元素

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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.
Determination of Impurity Elements in 99.999%Pure Silver by Matrix Separation-ICP Spectroscopy
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.

matrix separationICP spectroscopy99.999%sterling silverimpurity element

李尚远、赵鲁国、徐剑瑛、王绍娟、陈红灵

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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

基体分离 ICP光谱法 99.999%高纯银 杂质元素

2024

山西化工
山西省煤化工发展促进中心 山西省化工学会

山西化工

影响因子:0.293
ISSN:1004-7050
年,卷(期):2024.44(11)