Comparative Study of Three Mixing Methods in Fusion Technique for Determining Major and Minor Elements Using Wavelength Dispersive X-ray Fluorescence Spectroscopy

Abstract

Accurate analysis using a simple and rapid procedure is always the most important pursuit of analytical chemists. In this study, a new sample preparation procedure, namely the shaker cup (SH) method, was designed and compared with two sample preparation procedures, commonly used in the laboratory, from three aspects: homogeneity of the sample–flux mixture, potential for sample contamination, and sample preparation time. For the three methods, a set of 54 certified reference materials (CRMs) was used to establish the calibration curves, while another set of 19 CRMs was measured to validate the results. In the calibration procedures, the matrix effects were corrected using the theoretical alpha coefficient method combined with the experimental coefficient method. The data of the major oxides (SiO2, TiO2, Al2O3, TFe2O3, MnO, MgO, CaO, Na2O, K2O, and P2O5) and minor elements (Cr, Cu, Ba, Ni, Sr, V, Zr, and Zn) obtained by wavelength dispersive X-ray fluorescence spectroscopy (WD-XRF) were compared using two derivative equations based on the findings by Laurence Whitty-Léveillé. The results revealed that the WD-XRF measured values using the SH method best agreed with the values recommended in the literature.

Petrology and geochemistry of ultramafic rocks in the Mogok belt, Myanmar: Cumulates from high‐pressure crystallization of hydrous arc melts

“…Detailed analytical procedures are similar to those in Zhang et al (2020). Triplicate measurements of the standard GSR-1 yielded the 95% confidence limits of < ±0.05% for all oxides.…”

In Situ Investigation Of The Valence States Of Iron-Bearing Phases In Chang’E-5 Lunar Soil Using FIB, AES, And TEM-EELS Techniques

“…44 Glass discs for WD-XRF analysis were prepared upon the fusion of 0.6 g of the standard sample with 6.0 g of lithium tetraborate : metaborate (2:1) (Lithium borates 67-33, Claisse, Canada) using a Pt-Au crucible and mould employing electric fusion equipment (Claisse Fluxy, Corporation Scientific Claisse Inc., Quebec, Canada). 45 GSR-1, GSR-2, and GSR-3 were used to monitor the preparation process and instrument status.…”

MK-1 Orthopyroxene—A New Potential Reference Material for In-Situ Microanalysis

“…The PANalytical AXIOS Minerals equipped with a Rh anode X-ray tube and 4 kW excitation power is a sequential instrument with a single goniometer based measuring channel covering the complete elemental measurement range from F to U in the concentration range from 1.0 g g −1 to % level, determined in vacuum media [31]. Glass discs for WD-XRF analysis were prepared via the fusion of 0.6 g of the standard sample with 6.0 g of lithium tetraborate: metaborate (2:1) (Lithium borates 67-33, Claisse, Canada), using Pt-Au crucibles and molds employing electric fusion equipment (Claisse Fluxy, Corporation Scientific Claisse Inc., Quebec, Canada) [32]. Each disc was analyzed fifteen times, and greater variability between discs was seen than between repeated measurements with the RSD < 1% for all elements that were > 0.1% oxide in mass fraction.…”