Determination of main components in barite by X-ray fluorescence spectrometry with fusion sample preparation after acetic acid pretreatment
LI Dayong1, WANG Shikui*2, WANG Liang1, ZHANG Zhouwei1
1. Guizhou Central Laboratory of Geology and Mineral Resources,Guiyang 550018,China; 2. No.113 Geological Party,Guizhou Bureau of Geology and Mineral Exploration ＆ Development,Liupanshui 553001,China
Abstract：It is of great significance to determine accurately the main components in barite for the subsequent development and utilization of barite resources. As the determination results of BaSO4 and SrSO4 by X-ray fluorescence spectrometry (XRF) are converted from the determination results of the analysis spectral lines of Ba and Sr, BaCO3 and SrCO3 in the sample will interfere with the determination of BaSO4 and BaSO4. After the carbonate components in the sample were separated by acetic acid pretreatment, the sample was determined by XRF, which successfully avoided the interference of BaCO3 and SrCO3 with BaSO4 and SrSO4. At the same time, the filter slag after acetic acid pretreatment was burned and weighed to calculate the sample loss. The sample mass loss caused by acetic acid pretreatment and burning was compensated by adding mixed flux with the same mass as the sample loss. The sample pellet was prepared by fusion sample preparation with mixed flux of lithium tetraborate and lithium metaborate. Consequently, a method for simultaneous determination of 5 components including BaSO4, Al2O3, SiO2, Fe and BaSO4 in barite was realized by XRF. The national reference material and Guizhou Provincial reference material of barite with a certain level of component content were selected to prepare the calibration curve. The determination coefficients of calibration curves were all not less than 0.999 8. The detection limit of BaSO4 was 0.128%, and detection limits for other components were in range of 0.004%-0.029%. The proposed method was applied to the analysis of barite samples. The results showed that the relative standard deviations (RSD) were not more than 0.2% when the determination results were greater than 5%. The relative standard deviations were not more than 2.0% when the determination results were not more than 5%. The relative errors(RE) were all less than the allowable limits specified in DZ/T 0130-2006 of the specification of testing quality management for geological laboratories.
李大勇, 王士魁, 王亮, 张周位. 醋酸预处理-熔融制样-X射线荧光光谱法测定重晶石中主要组分[J]. 冶金分析, 2023, 43(3): 27-33.
LI Dayong, WANG Shikui, WANG Liang, ZHANG Zhouwei. Determination of main components in barite by X-ray fluorescence spectrometry with fusion sample preparation after acetic acid pretreatment. , 2023, 43(3): 27-33.
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