Determination of trace boron in beneficiation-metallurgy process samples of high purity quartz by inductively coupled plasma atomic emission spectrometry
ZHANG Hongli1,2.3, SUN Qiliang1,2.3, LIU Yan1,2.3, NI Wenshan1,2.3, LIU Lei1,2.3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006,China; 2. China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China; 3. Engineering Technology Innovation Center for Development and Utilization of High Purity Quartz,Ministry of Natural Resources,Zhengzhou 450006,China
Abstract：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 0.020-10 μg/mL had a linear relationship with the corresponding emission spectrometry intensity, and the linear correlation coefficient was 0.999 8. The limit of detection for boron was 0.10 μg/g, and the limit of quantification was 0.32 μg/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.
张宏丽, 孙启亮, 刘闫, 倪文山, 刘磊. 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[J]. 冶金分析, 2023, 43(7): 69-75.
ZHANG Hongli, SUN Qiliang, LIU Yan, NI Wenshan, LIU Lei. Determination of trace boron in beneficiation-metallurgy process samples of high purity quartz by inductively coupled plasma atomic emission spectrometry. , 2023, 43(7): 69-75.
[1] 王九一. 高纯石英——二氧化硅中的“大熊猫”[J].地球(Earth),2022(1):17-21. [2] 王九一.全球高纯石英原料矿的资源分布与开发现状[J].岩石矿物学杂志,2021,40(1):131-141. WANG Jiuyi.Global high purity quartz deposits:resources distribution and exploitation status[J].Acta Petrologica et Mineralogica,2021,40(1):131-141. [3] 贾德龙,张万益,陈丛林,等.高纯石英全球资源现状与我国发展建议[J].矿产保护与利用,2019,39(5):111-117. JIA Delong,ZHANG Wanyi,CHEN Conglin,et al.Global resource status and China's development suggestions of high purity quartz [J].Conservation and Utilization of Mineral Resources,2019,39(5):111-117. [4] 中华人民共和国国家发展和改革委员会.JC/T 1048—2007单晶硅生长用石英坩埚[S].北京:中国标准出版社,2007. [5] 王艳,汪灵,李彩侠,等.高纯石英质量的ICP检测技术初步研究[J].矿物学报(Acta Mineralogica Sinica),2012,32(S1):116-117. [6] 汪灵,党陈萍,李彩侠,等.中国高纯石英技术现状与发展前景[J].地学前缘,2014,21(5):267-273. WANG Ling,DANG Chenping,LI Caixia,et al.Technology of high-purity quartz in China:Status quo and prospetct[J].Earth Science Frontiers,2014,21(5):267-273. [7] 中华人民共和国工业和信息化部. JC/T 2027—2010高纯石英中杂质含量的测定方法——电感耦合等离子体原子发射光谱法[S].北京:中国标准出版社,2010. [8] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 32650—2016电感耦合等离子体质谱法检测石英砂中痕量元素[S].北京:中国标准出版社,2016. [9] 张宏丽,倪文山,刘磊,等.冷焰模式-电感耦合等离子体质谱法测定高纯石英中痕量铁[J].冶金分析,2021,41(7):28-34. ZHANG Hongli,NI Wenshan,LIU Lei,et al.Determination of ultra-trace iron in high-purity quartz by cool flame mode-inductively coupled plasma mass spectrometry[J].Conservation and Utilization of Mineral Resources,2021,41(7):28-34. [10] 岩石矿物分析编写组.岩石矿物分析[M].3版.北京:地质出版社,1991:232-243. [11] 李晓丽.ICP-AES法测定保护渣中微量硼的研究[J].包钢科技,2000(2):54-58. LI Xiaoli.Study of ICP-AES method in determining micro boron in mould powder[J].Science & Technology of Baotou Steel (Group) Corporation,2000(2):54-58. [12] 安中庆,方海燕,范兴祥,等.电感耦合等离子体原子发射光谱法测定镍硼合金中硼[J].冶金分析,2020,40(2):76-80. AN Zhongqing,FANG Haiyan,FAN Xingxiang,et al.Determination of boron in nickel-boron alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2020,40(2):76-80. [13] 闫春燕,伊文涛,马培华,等.微量硼的测定方法研究进展[J].理化检验(化学分册),2008,44(2):197-201. YAN Chunyan,YI Wentao,MA Peihua,et al.Recent progress of methods for determination of micro-amounts of boron [J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2008,44(2):197-201. [14] 龚仓,帅林阳,夏祥,等.交流电弧直读光谱法快速测定地质样品中银、锡、钼、硼和铅[J].理化检验(化学分册),2020,56(12):1320-1325. GONG Cang,SHUAI Linyang,XIA Xiang,et al.Rapid determination of Ag,Sn,Mo,B and Pb in geological samples by AC arc direct reading spectrometry[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2020,56(12):1320-1325. [15] 沈真.电感耦合等离子体原子发射光谱法测定铬铁中痕量硼[J].冶金分析,2022,42(7):82-86. SHEN Zhen.Determination of trace boron in ferrochrome by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2022,42(7):82-86. [16] 戚振南,任玲玲,杨晓倩,等.微波消解-电感耦合等离子体原子发射光谱法测定镍基合金中硅铬硼[J].冶金分析,2021,41(1):87-91. QI Zhennan,REN Lingling,YANG Xiaoqian,et al.Determinnation of silicon,chromium and boron in nickle-based alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2021,41(1):87-91. [17] 李绿叶,杜米芳.电感耦合等离子体原子发射光谱法测定船用钢中硼锆铌钨[J].冶金分析,2021,41(1):75-79. LI Lüye,DU Mifang.Determination of boron,zirconium,niobium and tungsten in steel for ship by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2021,41(1):75-79. [18] 冯静霞,赵恒泽,齐艺裴,等.硼酸对水玻璃基保温材料性能影响研究[J].硅酸盐通报,2022,41(5):1830-1837. FENG Jingxia,ZHAO Hengze,QI Yipei,et al.Effect of boric acid on properties of thermal insulation material fabricated by sodium silicate[J].Bulletin of the Chinese Ceramic Society,2022,41(5):1830-1837. [19] 中华人民共和国国土资源部.DZ/T 0130—2006 地质矿产实验室测试质量管理规范[S].北京:中国标准出版社,2006. [20] 杜宝华,盛迪波,罗志翔,等.低压密闭消解-电感耦合等离子体发射光谱法测定地质样品中的硼[J].岩矿测试,2020,39(5):690-698. DU Baohua,SHENG Dibo,LUO Zhixiang,et al.Determination of boron in geological samples by ICP-OES with low-pressure closed digestion[J].Rock and Mineral Analysis,2020,39(5):690-698.
