石油炼制与化工 ›› 2023, Vol. 54 ›› Issue (11): 109-116.

• 分析与评定 • 上一篇    下一篇

石油焦中微量元素含量的测定

吴梅,侯小敏,章群丹   

  1. 中石化石油化工科学研究院有限公司
  • 收稿日期:2023-03-08 修回日期:2023-07-31 出版日期:2023-11-12 发布日期:2023-10-29
  • 通讯作者: 吴梅 E-mail:wumei.ripp@sinopec.com
  • 基金资助:
    中国石油化工股份有限公司合同项目

DETERMINATION OF TRACE ELEMENTS IN PETROLEUM COKE


  • Received:2023-03-08 Revised:2023-07-31 Online:2023-11-12 Published:2023-10-29
  • Contact: Wu Mei E-mail:wumei.ripp@sinopec.com

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R2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5.4,1.4,2.1,2.8 μg/g。

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

Abstract: 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 the α-empirical coefficient method could be used to correct 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 R2 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, 2.8 μg/g, respectively.

Key words: petroleum coke, trace element, energy dispersive, X-ray fluorescence spectrometer, matrix correction