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基于生成氟硼酸钾的电感耦合等离子体原子发射光谱法测定多晶硅中硼
引用本文:黄艳芳,李核,郭长娟,陈红雨,钟梦婷.基于生成氟硼酸钾的电感耦合等离子体原子发射光谱法测定多晶硅中硼[J].冶金分析,2012,32(8):51-54.
作者姓名:黄艳芳  李核  郭长娟  陈红雨  钟梦婷
作者单位:(华南师范大学化学与环境学院,广东广州 510006)
基金项目:国家重点基础研究发展计划资助课题(2009CB226109);广东省科技计划项目(2010B010800027);广东省自然科学基金(10151063101000011)
摘    要:为了快速简便地运用电感耦合等离子体原子发射光谱法(ICP-AES)检测微量硼的含量,减少硼在消解过程中的损失,通过采用氢氟酸-硝酸消解样品,加入KF使硼生成的HBF4转化为一种非常稳定的化合物KBF4,再用ICP-AES测定试液中硼。探讨了氟化钾用量、挥发时间和温度等因素对测定的影响,并优化了实验参数。用本法测定多晶硅中的硼,其检出限为2.6 pg/mL,样品测定结果的相对标准偏差在3.6%~6.9%之间,加标回收率为98%~102%。

关 键 词:多晶硅  电感耦合等离子体原子发射光谱法  氟化钾    氟硼酸钾  
收稿时间:2011-11-02

Inductively coupled plasma atomic emission spectrometric determination of boron in polycrystalline silicon based on the formation of potassium fluoborate
HUANG Yan-fang,LI He,GUO Chang-juan,CHEN Hong-yu,ZHONG Meng-ting.Inductively coupled plasma atomic emission spectrometric determination of boron in polycrystalline silicon based on the formation of potassium fluoborate[J].Metallurgical Analysis,2012,32(8):51-54.
Authors:HUANG Yan-fang  LI He  GUO Chang-juan  CHEN Hong-yu  ZHONG Meng-ting
Affiliation:(School of Chemistry and Environment,South China Normal University,Guangzhou 510006,China)
Abstract:In order to rapidly and simply determine the content of trace boron in polycrystalline silicon by inductively coupled plasma atomic emission spectrometry(ICP-AES) and reduce the volatilization loss of boron during digestion procedure,a novel method was proposed in this study.The sample was decomposed with hydrofluoric acid and hydrogen nitrate.Then,KF was added to make HBF4 formed from boron changing to a very stable compound KBF4.Finally,the content of boron in testing solution was determined by ICP-AES.The effect of KF dosage,evaporation time and temperature on the determination was discussed.The experimental parameters were optimized.The proposed method was applied to the determination of boron in polycrystalline silicon.The detection limit was 2.6 pg/mL,the relative standard deviation(RSD) was 3.6 %-6.9 %,and the recoveries were 98 %-102 %.
Keywords:polycrystalline silicon  inductively coupled plasma atomic emission spectrometry(ICP-AES)  potassium fluoride  boron  potassium fluoborate
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