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高压密闭酸溶-电感耦合等离子体发射光谱法测定硼矿石中的硼

Boron Analysis in Boron Ores by Inductively Coupled Plasma-Optical Emission Spectrometry with Sealed Acid Digestion at High Pressure

  • 摘要: 应用电感耦合等离子体发射光谱法(ICP-OES)分析硼矿石中的硼含量,样品分解方法多采用酸溶法和熔融法,硼酸在浓酸溶液中加热蒸发时形成易挥发的BF3或BCl3,造成硼的损失。熔融法可分解难溶于酸的硅硼钙石、电气石等样品,但将大量钠盐引入了样品中,基体较大,检出限高。本文建立了高压密闭酸溶、ICP-OES测定硼矿石中硼含量的方法。样品经硝酸和氢氟酸在高压密闭溶样罐中分解完全、定容稀释后,样品溶液用配备耐氢氟酸进样系统的ICP-OES测定。在ICP-OES中,硼有三条常用分析谱线,选取249.677nm为硼的分析谱线,标准曲线的线性相关系数大于0.9995。采用本方法对硼镁矿、锰方硼石和盐湖型固体硼矿三种类型5个不同含量范围的实际样品进行测定,相对标准偏差(RSD,n=11)为0.39%~2.66%,方法检出限为1.76µg/g,硼含量定量范围为5.87µg/g~10.8%。经标准物质验证,硼含量测定值与标准值一致,与容量法和微波消解法测定结果吻合。本方法试剂用量少,无需蒸干样品溶液,有效地避免了硼酸易挥发和试剂用量大的问题。

     

    Abstract: The literature provides reference for the accurate determination of boron by inductively coupled plasma-optical emission spectrometry (ICP-OES), but most of the studies are conducted on the standard substances of soil and stream sediment. In addition, the range of boron content is low, and the methods for the determination of high boron content in boron ores are few. A method of ICP-OES with sealed acid digestion at high pressure was developed for the determination of boron content in boron ores. Using nitric acid and hydrofluoric acid as reagents, the samples of boron ores were dissolved at high temperature and high pressure without acid drive, and ICP-OES equipped with a hydrofluoric acid-resistant sampling system was used to determine boron. The samples of boromagnesite, ludwigite, chambersite and salt lake type solid boron ore were taken as the research objects. The relative standard deviation (RSD, n=11) was 0.39%−2.66%, the detection limit of the method was 1.76g/g, and the determination range was 5.87g/g−10.8%. The measured values were consistent with the certified values after the verification of the reference materials. Compared with volumetric method and microwave digestion method, the results were in good agreement. This method does not require evaporating the sample solution, which solves the boron volatile loss problem. The BRIEF REPORT is available for this paper at http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202308070131.

     

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