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磷铍钙石中铍元素的电子探针定量分析

Quantitative Analysis of Be in Herderite by Electron Probe Microanalysis

  • 摘要: 前人使用配有 LDEB 或 LDE3H 的电子探针,建立了针对铍硅酸盐、铍氧化物以及铍硼酸盐中 Be 含量的定量分析方法。然而,缺乏对铍磷酸盐矿物中 Be含量的定量分析方法。目前,使用配备LSA300分光晶体的电子探针对铍磷酸盐矿物进行分析时,P元素的高级次阶峰会抬高Be Kα峰的上背景值,从而导致Be含量的测量结果不准确。本文使用配备LDE3H分光晶体的电子探针,对江西狮子岭花岗岩中的磷铍钙石,采用不同的加速电压和分析束流,进行最佳定量分析条件的探索。实验结果表明:磷铍钙石的最佳电子探针定量分析条件为:加速电压10kV,分析束流20nA。在此条件下,获得的磷铍钙石P2O5平均含量为43.23%,BeO平均含量为15.39%,CaO平均含量为33.89%,F平均含量为7.94%,BeO标准误差为0.3%。本研究发现配有LDE3H分光晶体的电子探针,可以设置合适的Be背景来消除P的高级次阶峰的干扰。此外,含Be矿物的测量难点与Be特征X射线本身的特征、含Be矿物的晶体结构、化学成分均有关。磷铍钙石定量分析方法的探索,解决了电子探针对铍磷酸盐矿物Be元素进行准确定量时,P元素产生的干扰难题,进一步提升电子探针对铍含量测量的准确度。

     

    Abstract: Previously, researchers employed electron probe microanalysis (EPMA) furnishedwith LDEB or LDE3H to establish a quantitative analysis approach for the Be content in berylliumsilicates, beryllium oxides, and beryllium borates. Nevertheless, a quantitative analysis method forthe Be content in beryllophosphate minerals is still lacking. At present, when EPMA equippedwith LSA300 crystal is used to analyze beryllophosphate minerals, the higher-order peaks of Pwill raise the upper background value of the Be Kα peak, resulting in inaccurate measurementresults of Be content. In this study, the EPMA equipped with LDE3H crystal was used to explorethe optimal quantitative analysis conditions for herderite in Shiziling granite in Jiangxi Provinceby using different accelerating voltages and probe currents. The experimental results show that theoptimal EPMA quantitative analysis conditions for herderite are: acceleration voltage of 10kV, andprobe current of 20nA. Under these conditions, the average content of P2O5, BeO, CaO, F is43.23%, 15.39%, 33.89%, and 7.94%, respectively, and the standard error of BeO is 0.3%. It isfound that the EPMA equipped with LDE3H crystal can set a suitable Be background to eliminatethe interference of the higher order peaks of P. In addition, the difficulty of Be measurement isrelated to Be characteristic X-ray, crystal structures and chemical composition of Be minerals. Theexploration of a quantitative analysis method of herderite solves the problem of interference of Pelement when the EPMA accurately quantifies the Be element of beryllophosphate minerals, andfurther improves the accuracy of the measurement of beryllium content by EPMA.

     

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