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

Abstract

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.

Keywords

• wavelength dispersive-energy dispersive x-ray fluorescence spectrometer
• fusion sample preparation
• mineralized samples
• silicate minerals
• major, minor and trace elements