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

BACKGROUND At 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...

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Main Authors: LI Ying-chun, ZHANG Lei, ZHOU Wei, SHANG Wen-yu
Format: Article
Language:English
Published: Science Press, PR China 2020-11-01
Series:Yankuang ceshi
Subjects:
Online Access:http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201912250178
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author LI Ying-chun
ZHANG Lei
ZHOU Wei
SHANG Wen-yu
author_facet LI Ying-chun
ZHANG Lei
ZHOU Wei
SHANG Wen-yu
author_sort LI Ying-chun
collection DOAJ
description BACKGROUND At 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. OBJECTIVES To develop a method for determination of major elements in mineralized samples. METHODS The 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. RESULTS The 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. CONCLUSIONS Through 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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spelling doaj.art-d4c33be94dc94da0992c4f8fe76186d92023-01-13T09:16:34ZengScience Press, PR ChinaYankuang ceshi0254-53572020-11-0139682883810.15898/j.cnki.11-2131/td.201912250178yk201912250178Determination of Major and Minor Elements in Rocks, Soils and Sediments and Complex Samples by Wavelength and Energy Dispersive X-ray Fluorescence Spectrometer with Fusion SamplingLI Ying-chun0ZHANG Lei1ZHOU Wei2SHANG Wen-yu3National Research Center for Geoanalysis, Beijing 100037, ChinaNational Research Center for Geoanalysis, Beijing 100037, ChinaNational Research Center for Geoanalysis, Beijing 100037, ChinaNational Research Center for Geoanalysis, Beijing 100037, ChinaBACKGROUND At 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. OBJECTIVES To develop a method for determination of major elements in mineralized samples. METHODS The 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. RESULTS The 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. CONCLUSIONS Through 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.http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201912250178wavelength dispersive-energy dispersive x-ray fluorescence spectrometerfusion sample preparationmineralized samplessilicate mineralsmajor, minor and trace elements
spellingShingle 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
Yankuang ceshi
wavelength dispersive-energy dispersive x-ray fluorescence spectrometer
fusion sample preparation
mineralized samples
silicate minerals
major, minor and trace elements
title 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
title_full 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
title_fullStr 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
title_full_unstemmed 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
title_short 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
title_sort 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
topic wavelength dispersive-energy dispersive x-ray fluorescence spectrometer
fusion sample preparation
mineralized samples
silicate minerals
major, minor and trace elements
url http://www.ykcs.ac.cn/en/article/doi/10.15898/j.cnki.11-2131/td.201912250178
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