石油炼制与化工 ›› 2020, Vol. 51 ›› Issue (11): 76-81.

• 分析与评定 • 上一篇    下一篇

电感耦合等离子体发射光谱法测定有机钼中的微量元素

王轲,吴梅   

  1. 中国石化石油化工科学研究院
  • 收稿日期:2020-04-28 修回日期:2020-05-22 出版日期:2020-11-12 发布日期:2020-11-24
  • 通讯作者: 王轲 E-mail:wangke.ripp@sinopec.com
  • 基金资助:
     

DETERMINATION OF TRACE ELEMENTS IN ORGANIC MOLYBDENUM BY INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY

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  • Received:2020-04-28 Revised:2020-05-22 Online:2020-11-12 Published:2020-11-24
  • Contact: Ke WANG E-mail:wangke.ripp@sinopec.com
  • Supported by:
     

摘要: 使用有机溶剂按一定比例将油溶性有机钼样品稀释后,采用电感耦合等离子发射光谱仪(ICP-OES)测定样品中铝、钡、钙、铬、铜、铁、钾、镁、锰、钠、镍、磷、铅、硅、钒和锌微量元素的含量,建立有机钼样品中微量元素的分析方法。通过配制、分析钼干扰考察样品,确定被干扰的元素谱线,选择合适的分析谱线消除钼基体的光谱干扰,并对方法的精密度进行考察,再分别用该方法和国家标准GB/T 17476—1998方法对实际样品中微量元素进行测定。结果表明,将油溶性有机钼样品用稀释剂稀释100倍,选择合适的谱线进行ICP-OES测定,各元素含量的相对标准偏差均小于2%,加标回收率为95%~109%。所建立的分析方法快速、准确,适用于有机钼样品中多种元素的同时测定。

关键词: 钼, 电感耦合等离子发射光谱, ICP-OES, 元素分析

Abstract: The oil soluble organic molybdenum was diluted by organic solvent with certain proportion. The trace element contents in oil-soluble organic molybdenum was determined by inductively coupled plasma optical emission spectrometry(ICP-OES), such as aluminum, barium, calcium, chromium, copper, iron, potassium, magnesium, manganese, sodium, nickel, phosphorus, lead, silicon, vanadium, and zinc. A simplified and rapid method for the analysis of trace elements in organic molybdenum samples was established. The element spectral lines of samples interfered by Mo were determined by preparation and analysis of samples, and the appropriate analytical spectral lines were selected to eliminate the molybdenum matrix spectral interference. The precision of the established method was investigated, and then the trace elements in the actual samples were determined by the method and the GB/T 17476-1998 method, respectively and compared. The results showed that by the new method, the relative standard deviation of each element was less than 2%, and the spike recovery was 95%-109% at the appropriate spectral line when the oil soluble organic molybdenum was diluted 100 times with ICP diluent. The method is rapid, accurate and is able to determine multiple elements in the oil soluble organic molybdenum simultaneously.

Key words: molybdenum, inductively coupled plasma optical emission spectrometry, ICP-OES, element analysis

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