Electron probe microanalysis of minerals: microanalyzer or scanning electron microscope?

Electron probe microanalysis of minerals: microanalyzer or scanning electron microscope?
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DOI:
10.1016/j.rgg.2015.07.006
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发表时间:
2015-08-01
影响因子:
1.1
通讯作者:
Usova, L. V.
Usova, L. V.
中科院分区:
地球科学4区
文献类型:
--
作者:
Lavrent'ev, Yu. G.;Karmanov, N. S.;Usova, L. V.

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比较了几种造岩矿物的波长色散谱(WDS)和能量色散谱(EDS)电子探针分析结果,研究了两种方法的特征。使用具有五个波长色散光谱仪的JXA-8100(JEOL)微量分析仪和装备有印加Energy 450 XMax 80(Oxford Instruments)微量分析系统的MIRA 3 LMU(Tescan)扫描电子显微镜进行测量。对橄榄石、石榴子石、辉石、钛铁矿和铬尖晶石等样品进行了分析,在主要组分的组成范围内(C > 10%),表明单次测定重复性的变异系数分别为WDS的0.5%和EDS的0.9%。对于次要组分(1% < C < 10%),变异系数分别为1.4%和3.0%;对于杂质(0.3% < C < 1%),变异系数分别为2.7%和13%。对于较低的含量,EDS几乎不适用。两种方法所得结果的比值重现性良好,精密度高:主成分变异系数为0.56%,次成分变异系数为1.7%,杂质变异系数也接近8%。偏差的幅度在0.2和3.2相对%之间,结果表明,对于造岩矿物的主次成分,WDS和EDS的测量精度相当。对于杂质,能量色散光谱法不如波长色散光谱法,并且完全不适用于更低的含量。这种方法更容易实现,并且在打开仪器后很快就可以获得结果。波长色散光谱法需要更多的准备时间,但它可以确保对类似成分的样品进行精确高效的大规模分析,即使元素含量低于1%。(C)2015年,VS。索博列夫国际总工会,俄罗斯社会科学院西伯利亚分支。Elsevier B. V.出版,保留所有权利。
The results of electron probe microanalysis of several rock-forming minerals by wavelength-dispersive spectrometry (WDS) and energy-dispersive spectrometry (EDS) are compared, and the metrological characteristics of both methods are studied. The measurements were made with the use of a JXA-8100 (JEOL) microanalyzer with five wavelength-dispersive spectrometers and a MIRA 3 LMU (Tescan) scanning electron microscope equipped with an INCA Energy 450 XMax 80 (Oxford Instruments) microanalysis system. Specimens with olivine, garnet, pyroxene, ilmenite, and Cr-spinel grains were analyzed.The variation coefficients that characterize the repeatability of a single determination are found to be similar to 0.5% for WDS and similar to 0.9% for EDS in the compositional range of the main components (C > 10%). For minor components (1% < C < 10%), the variation coefficients are 1.4% and 3.0%, respectively, and for impurities (0.3% < C < 1%), 2.7% and 13%, respectively. For lower contents EDS is almost inapplicable. The ratio of the results obtained by the two methods is reproduced with high precision: For major components, the variation coefficient is 0.56%; for minor components, 1.7%; and even for impurities, it is similar to 8%. The magnitude of the bias is between 0.2 and 3.2 rel.%, which is acceptable.The results show that the accuracies of WDS and EDS are similar for measuring major and minor components of rock-forming minerals. Energy-dispersive spectrometry is inferior to wavelength-dispersive spectrometry for impurities and is completely inapplicable for still lower contents. This method is easier to implement, and the results are available soon after switching on the instrument. Wavelength-dispersive spectrometry needs more time for preparation, but it ensures a precise high-efficiency large-scale analysis of samples of similar compositions, even when the element contents are lower than 1%. (C) 2015, V.S. Sobolev IGM, Siberian Branch of the RAS. Published by Elsevier B.V. All rights reserved.