Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling

LI Ying-chun; ZHANG Lei; ZHOU Wei; SHANG Wen-yu

doi:10.15898/j.cnki.11-2131/td.201912250178

Rock and Mineral Analysis > 2020 > 39(6): 828-838. > DOI: 10.15898/j.cnki.11-2131/td.201912250178

LI Ying-chun, ZHANG Lei, ZHOU Wei, SHANG Wen-yu. Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling[J]. Rock and Mineral Analysis, 2020, 39(6): 828-838. DOI: 10.15898/j.cnki.11-2131/td.201912250178

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Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling

National Research Center for Geoanalysis, Beijing 100037, China

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Received Date: May 28, 2020
Revised Date: July 23, 2020
Accepted Date: September 18, 2020
Published Date: October 31, 2020

Abstract

HIGHLIGHTS
(1) Major and trace elements were simultaneously determined by WD-ED X-ray fluorescence spectrometer.

(2) The voltage and current conditions of some elements were modified, and the energy spectrum measurement time was effectively prolonged. The accuracy of major and minor elements was evaluated.

(3) The quantitative analysis of major and minor elements in complex mineralized samples was discussed by summing major elements of Ba, Cu and Ni in mineralized samples.

ABSTRACT

BACKGROUNDAt present, the major elements in silicate samples are generally determined by X-ray fluorescence spectrometry with fusion sample preparation. Not only can the single element determination results not exceed the limit, but also the percentage sum must meet the requirements of sum quality (99.3%-100.7%). However, for the analysis of mineralized samples, due to the high content of trace elements, it is often not possible to meet the requirements of sum quality. The wavelength and energy dispersive X-ray fluorescence spectrometer are fully utilized. The advantages of the determination can make the analysts to get the information of sample composition as soon as possible, which is of great significance to evaluate the data quality of mineralized samples.
OBJECTIVESTo develop a method for determination of major elements in mineralized samples.
METHODSThe wavelength-energy dispersive X-ray fluorescence spectrometer was used to determine the major elements while adding more minor elements to the determination without prolonging the analysis time. The main elements were quantified by wavelength dispersion, while the minor elements were mainly determined by energy dispersion. Under the condition of ensuring the accuracy of the major elements, the measurement conditions were reasonably set and the energy spectrum measurement time was extended.
RESULTSThe method achieved the measurement of the major elements within 12 minutes using wavelength dispersion, and also provided results of 14 minor elements such as Rb, Sr, Y, Zr, Ba, Cu, Zn and the semi-quantitative results of 10 elements with narrow linear range or low content such as Co, Ge, Pr and Ta. The maximum limit of detection of 24 minor elements was 16.76μg/g.
CONCLUSIONSThrough the accuracy assessment, the determination results of major elements are consistent with the certified values, and the determination of minor elements with high content also meets the requirements of quantitative analysis. This method makes the analysts to get the information of sample composition quickly, provides a basis for more accurate and reliable data, and effectively solves the determination of major elements in complex mineralized samples.

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Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion Sampling

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