石油炼制与化工 ›› 2025, Vol. 56 ›› Issue (3): 127-133.

• 分析与评定 • 上一篇    下一篇

能量色散X射线荧光光谱法快速测定原油及渣油中铁、镍、钒含量的研究

李贤发1,吴梅1,褚小立1,章群丹1,刘日元2   

  1. 1. 中石化石油化工科学研究院有限公司
    2. 北京东方慧博企业管理服务有限公司
  • 收稿日期:2024-09-05 修回日期:2024-11-26 出版日期:2025-03-12 发布日期:2025-02-25
  • 通讯作者: 章群丹 E-mail:zhangqd.ripp@sinopec.com

RAPID DETERMINATION OF IRON, NICKEL AND VANADIUM IN CRUDE OIL AND RESIDUAL OIL BY ENERGY DISPERSIVE X-RAY FLUORESCENCE METHOD


  • Received:2024-09-05 Revised:2024-11-26 Online:2025-03-12 Published:2025-02-25
  • Contact: Qun-Dan ZHANG E-mail:zhangqd.ripp@sinopec.com

摘要: 建立能量色散X射线荧光光谱法快速测定原油及渣油中Fe,Ni,V含量的方法,考察基质干扰、定量曲线拟合方式等因素对测定结果的影响,探索固化剂固化原油的可行性方案。研究结果表明,固化剂能避免Fe元素在原油中快速沉降,保证Fe在原油中均匀分布,固化后的原油元素分析数据稳定准确。原油和渣油中的高含量S元素是最大的基质干扰因素,使用经验系数法可较好地对S元素等基质效应进行校正,使所建方法能在8min左右准确测定原油和渣油中Fe,Ni,V的含量。该方法测定原油和渣油中Fe,Ni,V含量的精密度均小于3%,测定原油样品的加标回收率为95.1%~102.7%,Fe,Ni,V元素的检出限分别为0.1,0.2,0.2μg/g。因此该方法分析精度高、速度快,无需进行样品预处理,在原油快速评价、原料质量把控及后期工业生产中具有巨大的应用价值。

关键词: 能量色散X射线荧光光谱, 固化剂, 基质校正

Abstract: An energy dispersive X-ray fluorescence (ED-XRF) spectrometry method was developed for the rapid determination of Fe, Ni, and V in crude oil and residual oil. The effects of matrix influence, quantitative curve fitting method and other factors on the determination results were investigated. The feasible solution of curing crude oil with curing agent was explored. The study shows that the curing agent can avoid the rapid sedimentation of Fe element in crude oil, ensure the uniform distribution of Fe in crude oil, and the data of cured crude oil are stable, accurate and reliable. The high content of elemental S in crude oil and residual oil is the biggest matrix interfering factor, and the use of the empirical coefficient method can better correct for matrix effects such as elemental S, so that the constructed method can accurately determine the content of Fe, Ni, and V in crude oil and residual oil in about 8 min. The precision of the method for the determination of Fe, Ni and V in crude oil and residual oil was less than 3%, the recoveries of the crude oil samples ranged from 95.1% to 102.7%, and the detection limits of the method for the elements of Fe, Ni and V were 0.1, 0.2 and 0.2 μg/g, respectively. The method has high analytical precision, fast sample analysis speed, and no sample pretreatment, which has great application value in crude oil fast assessment, raw material quality control and later industrial production.

Key words: ED-XRF, curing agent, matrix correction