摘要
高纯氧化镁产品纯度达到99.9%,杂质硅含量是评价高纯氧化镁产品等级的重要指标之一,对其进行准确测定显得尤为重要。常规的标准曲线法无法克服镁的基体效应,国内同行常规使用基体匹配法来克服基体效应,但是难以找到含杂元素与高纯氧化镁产品相近且纯度更高的金属镁。采用标准加入法作为技术手段,优点是非常适合高镁基体浓度中(超)痕量元素的分析,准确度高。本研究以盐酸溶解样品,以标准加入法为技术手段,采用电感耦合等离子体发射光谱技术,建立了一种简单、快速、准确的测定方法。该方法在分析谱线251.611 nm处,有良好的线性关系,方法的检出限为0.0183μg/mL,测定下限为0.0610μg/mL。在实际高纯氧化镁产品测试中,加标回收率在97.86%~103.80%之间,适合高纯氧化镁产品中酸溶硅的测定,为解决盐湖化工企业氧化镁产品中酸溶硅含量的测定提供了技术支撑。
High pure magnesium oxide product purity reaches 99.9%.The silicon impurity content is one of the important indicators to evaluate its grade,and it is particularly important to determine it accurately.Routine standard curve methods cannot overcome the matrix effect of magnesium so that domestic counterparts routinely use matrix matching method to overcome such effect,but it is difficult to find magnesium containing miscellaneous elements and higher purity similar to high purity magnesium oxide products.The standard accession method is used as a technical means since its advantage is that it is very suitable for analyzing(super)trace elements in high magnesium matrix concentrations with high accuracy.This study dissolved the samples of hydrochloric acid.Taking the standard addition method as the technical method,inductively coupled plasma emission spectroscopy was used to establish a simple,fast,and accurate assay.The proposed method had a good linear relationship at the analytical spectral line of 251.611 nm,the detection limit of the method was 0.0183μg/mL,and the lower limit of determination was 0.0610μg/mL.In the actual high-purity magnesium oxide product test,the calibration recovery rate was between 97.86%—103.80%,which was suitable for determining acid-soluble silicon in high-purity magnesium oxide products and provided technical support for the determination of acid-soluble silicon content in magnesium oxide products of salt lake chemical enterprises.
作者
王景凤
赖春华
孙康
宋学文
孔会民
王茂盛
隆英兰
WANG Jingfeng;LAI Chunhua;SUN Kang;SONG Xuewen;KONG Huimin;WANG Maosheng;LONG Yinglan(Technology Development of Western Mining Group Co.,Ltd.,Xining 810006,China;The Engineering and Technology Research of Qinghai Western Mining Co.,Ltd.,Xining 810006,China;Qinghai Key Laboratory of Plateau Mineral Processing Engineering and Comprehensive Utilization,Xining 810006,China;Qinghai Nonferrous Mineral Resources Engineering Technology Research Center,Xining 810006,China;College of Material Science and Engineering,Xi'an University of Architecture and Technology,Xi’an 710055,China)
出处
《有色金属科学与工程》
CAS
北大核心
2022年第4期135-140,共6页
Nonferrous Metals Science and Engineering
基金
青海省重大科技专项资助项目(2020-GX-A1)
国家重点研发计划资助项目(2018YFC1903805)
创新平台建设专项(2021-ZJ-Y16)。
