石油学报(石油加工)2024,Vol.40Issue(3) :813-819.DOI:10.3969/j.issn.1001-8719.2024.03.026

ICP-MS/MS测定轻质油中痕量氯含量

Determination of Trace Chlorine Content in Light Oil by ICP-MS/MS

李爱阳 陈宇 殷子懿 陈林
石油学报(石油加工)2024,Vol.40Issue(3) :813-819.DOI:10.3969/j.issn.1001-8719.2024.03.026

ICP-MS/MS测定轻质油中痕量氯含量

Determination of Trace Chlorine Content in Light Oil by ICP-MS/MS

李爱阳 1陈宇 1殷子懿 1陈林2
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作者信息

  • 1. 湖南工学院化学与环境工程学院,湖南衡阳 421002
  • 2. 湖南省中医药研究院中药研究所,湖南长沙 410013
  • 折叠

摘要

基于H2反应模式下的质量转移反应消除干扰,建立电感耦合等离子体串联质谱(ICP-MS/MS)测定轻质油中痕量Cl的分析方法.轻质油经简单稀释后直接采用ICP-MS/MS进行测定,在MS/MS模式下使用H2作为反应气,利用在碰撞/反应池(CRC)中Cl+与H2发生二次H原子转移反应形成的子离子(H2Cl+)进行测定,消除所有质谱干扰,获得Cl的灵敏度和检出限(LOD)明显优于O2反应模式,LOD低至7.56 μg/kg.通过与扇型磁场ICP-MS(SF-ICP-MS)对比分析标准参考物质NIST SRM 1634c,评价方法的准确可靠性.结果表明,标准参考物质的分析结果与认证值基本一致,相对标准偏差(RSD)为3.1%~4.7%,2种方法的对比分析结果在95%的置信度水平无显著性差异.所建立分析方法的灵敏度、准确度和和精密度高,MS/MS模式和H2质量转移法的结合可无干扰测定轻质油中的Cl,适用于轻质油中痕量Cl的质量控制与评估.

Abstract

Based on the removal of interference by mass-transfer reaction in the H2 reaction mode,an analytical method for determining trace Cl in light oil by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS)was established.The light oil samples were directly determined by ICP-MS/MS after simple dilution.In the MS/MS mode,using H2 as the reaction gas,the product ion H2Cl+formed by the secondary H-atom transfer reaction between Cl+and H2 in the collision/reaction cell(CRC)was used for determination.In the case of eliminating all the spectral interference,the Cl sensitivity and the limit of detection(LOD)were obviously better than those in O2 reaction mode,and the LOD was as low as 7.56 μg/kg.The accuracy and reliability of the method were evaluated through comparative analysis of the standard reference material NIST SRM 1634c by use of the sector field ICP-MS(SF-ICP-MS).The results reveal that the analysis results of the standard reference materials are basically consistent with the certified values,and the relative standard deviation(RSD)is between 3.1%and 4.7%.There is no significant difference between the results of two methods at the 95%confidence level.The developed analytical method has high sensitivity,accuracy and precision.The combination of MS/MS mode and H2 mass-transfer method allows for the interference-free determination of Cl,which is suitable for the quality evaluation and control of trace Cl in light oil.

关键词

轻质油/电感耦合等离子体串联质谱/Cl/碰撞/反应池/H原子转移

Key words

light oil/inductively coupled plasma tandem mass spectrometry/Cl/collision/reaction cell/H-atom transfer

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基金项目

国家自然科学基金面上项目(21975289)

湖南省教育厅重点项目(20A140)

湖南省应用特色学科项目(湘教通[2018]469号)

湖南省大学生创新训练项目(3980)

出版年

2024
石油学报(石油加工)
中国石油学会

石油学报(石油加工)

CSTPCD北大核心
影响因子:0.764
ISSN:1001-8719
参考文献量20
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