电感耦合等离子体原子发射光谱法测定高纯石英选冶流程样品中痕量硼  

Determination of trace boron in beneficiation-metallurgy process samples of high purity quartz by inductively coupled plasma atomic emission spectrometry

作　　者：张宏丽[1,2,3] 孙启亮 刘闫 倪文山 刘磊[1,2,3] HANG Hongli;SUN Qiliang;LIU Yan;NI Wenshan;LIU Lei(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China;China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China;Engineering Technology Innovation Center for Development and Utilization of High Purity Quartz,Ministry of Natural Resources,Zhengzhou 450006,China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,河南郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,河南郑州450006 [3]自然资源部高纯石英开发利用工程技术创新中心,河南郑州450006

出　　处：《冶金分析》2023年第7期69-75,共7页Metallurgical Analysis

基　　金：中国地质调查局地质调查工作项目(DD20221698);国家自然科学基金青年基金项目(Nos.21806149)。

摘　　要：石英坩埚原料中硼元素会造成坩埚使用寿命缩短,因此准确评价高纯石英样品中硼的含量,对其产品应用具有指导意义。针对高纯石英选冶流程样品,采用常压混酸溶样法,通过加入甘露醇溶液避免了溶样过程中的硼挥发损失,针对流程样品中不同含量范围的硼元素,采用氢氟酸-硝酸-甘露醇-常压低温浸取-高温赶酸的样品前处理方式,保证高纯石英选冶流程样品中硼元素完全转移入样品溶液;选择B 249.773{135}nm作为硼的分析线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定高纯石英选冶流程样品中硼的方法。试验对样品前处理试剂选择、甘露醇溶液加入量、分析谱线及干扰元素的消除进行了研究。硼质量浓度在0.020~10μg/mL范围内与其发射光谱强度呈线性关系,线性相关系数为0.9998。方法的检出限为0.10μg/g,定量限为0.32μg/g。采用实验方法对7个高纯石英选冶流程样品中硼进行测定,结果的相对标准偏差(RSD,n=9)在2.1%~5.9%之间,加标回收率在96.0%~106%之间;并与电弧发射光谱法进行对比试验,测定结果基本一致。方法满足石英行业发展对产品的测试需求。The boron element in quartz crucible material can shorten the service life of crucible.Therefore,the accurate evaluation of boron element in high-purity quartz has guiding significance in the product application.The beneficiation-metallurgy process sample of high purity quartz was dissolved with mixed acid under atmospheric pressure.Mannitol solution was added to avoid the volatilization loss of boron during sample dissolution.For the different content range of boron in beneficiation-metallurgy process samples,a pretreatment method of hydrofluoric acid-nitric acid-mannitol-leaching at atmospheric pressure and low temperature-acid removal at high temperature was adopted to ensure that boron in beneficiation-metallurgy process sample could be completely transferred into the sample solution.B 249.773{135}nm was selected as the analytical line.The method for the determination of boron in beneficiation-metallurgy process samples of high purity quartz by inductively coupled plasma atomic emission spectrometry(ICP-AES)was established.The selection of pretreatment reagent,the addition amount of mannitol,the analytical line and the elimination of interference elements were studied.The mass concentration of boron in range of 0.020-10μg/mL had a linear relationship with the corresponding emission spectrometry intensity,and the linear correlation coefficient was 0.9998.The limit of detection for boron was 0.10μg/g,and the limit of quantification was 0.32μg/g.The content of boron in seven beneficiation-metallurgy process samples of high purity quartz was determined according to the experimental method,and the relative standard deviations(RSD,n=9)of determination results were between 2.1%and 5.9%.The recoveries were between 96.0%and 106%.Moreover,the arc emission spectrometry method was used for comparison,and the determination results were basically consistent.The proposed method could meet the determination requirements of products in the development of quartz industry.

关 键 词：高纯石英 选冶流程样品 硼 甘露醇 电感耦合等离子体原子发射光谱法(ICP-AES) 

分 类 号：O657.63[理学—分析化学] TF125.3[理学—化学]