摘要
采用能量色散X射线荧光光谱仪建立石油焦中微量元素含量的快速测定方法。考察制样方式、基质影响、定量曲线拟合方式等因素对测定结果的影响。石油焦中高含量的硫元素是最大的基质干扰因素,采用基本参数法和α经验系数法均可较好地进行基质校正,使所建方法可以在10 min内准确测定石油焦中S,Fe,Ni,V,Ca元素的含量。该方法对于各元素的定量曲线在相应的测试范围中均具有良好的线性相关性,决定系数R 2大于0.99。该方法对于S元素质量分数的定量限为0.040%,对于Fe,Ni,V,Ca元素质量分数的定量限分别为5.4,1.4,2.1,2.8μg g。
A rapid method for the determination of trace elements in petroleum coke was established by energy dispersive X-ray fluorescence spectrometer(ED-XRF).The influence of sample preparation method,powder and pressed powder,matrix and quantitative curve fitting on the test results was investigated.The high content of sulfur in petroleum coke was the greatest factor in matrix interference.Both the basic parameter method and theα-empirical coefficient method could be used to c orrect matrix,so that the content of S,Fe,Ni,V,Ca in petroleum coke could be determined accurately within 10 minutes.This method had good linear independence for the quantitative curves of each element in the corresponding test range,and the determination coefficient R 2 was greater than 0.99.The quantification limit of S was 0.040%,and the quantification limits of Fe,Ni,V,Ca were 5.4,1.4,2.1,2.8μg g,respectively.
作者
吴梅
侯小敏
章群丹
Wu Mei;Hou Xiaomin;Zhang Qundan(SINOPEC Research Institute of Petroleum Processing Co.,Ltd.,Beijing 100083)
出处
《石油炼制与化工》
CAS
CSCD
北大核心
2023年第11期109-116,共8页
Petroleum Processing and Petrochemicals
基金
中国石油化工股份有限公司合同项目(CLY21017)。
关键词
石油焦
微量元素
能量色散
X射线荧光光谱
基质校正
petroleum coke
trace element
energy dispersive
X-ray fluorescence spectrometer
matrix correction