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高压密闭酸溶-电感耦合等离子体质谱法测定花岗闪长岩中的微量锆

Determination of Trace Zirconium in Granodiorite by Inductively Coupled Plasma-Mass Spectrometry with Sealed Acid Digestion at High Pressure

  • 摘要: 采用高压密闭酸溶处理样品, 电感耦合等离子体质谱(ICP-MS)测定岩石中的多种微量、痕量元素是地质分析中普遍采用的一种分析方法, 但在分析花岗闪长岩样品时, 由于锆赋存在难溶的副矿物(锆石、金红石)中, 会出现锆溶出率偏低的现象。针对这一现象, 本研究增加了赶硅的预处理过程, 加大氢氟酸用量, 在溶液介质中引入氟离子使锆形成氟络离子改善了锆的稳定性, 将锆的溶出率提高到95%左右, 实现了花岗闪长岩中微量锆的准确测定。本方法的精密度(RSD, n=11) 小于5%, 检出限为0.052μg/g。应用于分析克拉玛依地区花岗闪长岩中的锆, 测定值与过氧化钠、偏硼酸锂碱熔以及X射线荧光光谱法的测定值有良好的一致性, 且基体效应小、检出限低, 还可以满足锂、铍、钪等其他多种微量元素的同时测定。

     

    Abstract: Determination of trace elements in rocks by Inductively Coupled Plasma-Mass Spectrometry with sealed acid digestion at high pressure is widely used in geological analysis.Zirconium occurs as insoluble accessory minerals such as zircon and rutile in granodiorite, so the recovery of zirconium is always low.This study adds the pretreatment process of removing silicon, increasing the amount of hydrofluoric acid and introducing fluoride ions in the solution to form zirconium fluorine complex ions which improves the stability of zirconium.These steps improve the recovery of zirconium(up to 95%) and achieve an accurate determination of trace zirconium in granodiorite.The precision of this method is less than 5%(RSD, n=11) and the detection limit is 0.052μg/g.Zirconium content of granodiorite in the Karamay area is determined by this method, which is consistent with the results determined by the alkaline fusion of Na2O2, LiBO2 and XRF method.Furthermore, this method has a small matrix effect and low detection limit, which can analyze various trace elements(Li, Be, Sc, for example) simultaneously.

     

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