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Russian Geology and Geophysics

2015 year, number 8

ELECTRON PROBE MICROANALYSIS OF MINERALS: MICROANALYZER OR SCANNING ELECTRON MICROSCOPE?

Yu.G. Lavrent’ev, N.S. Karmanov, L.V. Usova
V.S. Sobolev Institute of Geology and Mineralogy, Siberian Branch of the Russian Academy of Sciences, pr. Akademika Koptyuga 3, Novosibirsk, 630090, Russia
Keywords: Электронно-зондовый микроанализ, спектрометрия с волновой дисперсией, спектрометрия с энергетической дисперсией, метрологические характеристики, породообразующие минералы, Electron probe microanalysis, wavelength-dispersive spectrometry, energy-dispersive spectrometry, metrological characteristics, rock-forming minerals

Abstract

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 ~0.5% for WDS and ~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 ~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%.