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有机相直接进样 ICP-OES 快速测定车用汽油中微量硅

     

摘要

车用汽油样品用异辛烷溶剂适当比例稀释,直接进入电感耦合等离子体光谱仪(ICP-OES)测定硅元素。考察了稀释溶剂及稀释比例、标准物质类型、样品冷却温度、汽油样品组成等因素对硅含量测定的影响。结果表明,汽油样品用异辛烷按1∶1的比例混溶,在雾化室冷却温度为-10℃时,直接进入 ICP-OES测定硅含量效果最佳。在优化的工作条件下,该方法在0.1~10.0 mg·kg-1硅含量范围内线性良好,线性相关系数达0.99996,检出限为0.012 mg·kg-1,回收率在95.8%~98.4%之间,相对标准偏差小于3.0%。该法简便、快速、准确度高,适用于车用无铅汽油、车用乙醇汽油和低比例甲醇汽油中微量硅的快速检测。%A simple and accurate method was developed for determining silicon in gasoline using inductively coupled plasma optical emission spectroscopy (ICP-OES).For sample inroduction a Burgener nubulizer and a Cyclonic spray chamber were used.A gasoline sample was diluted with isooctane and then introduced into the cooled spray chamber of the ICP-OES.Good linearity was achieved in the silicon concentration range 0.1 ~10.0 mg·kg-1 ,and the correlation coefficient was 0.999 96.The detection limit for silicon was 0.012 mg· kg-1 and the silicon recoveries from gasoline samples were 95.8%~98.4%,with relative standard deviations of less than 3.0%.The method was proved to be simple,reliable and highly sensitive,and suitable for deter-mining silicon in samples of motor gasoline,ethanol-gasoline and methanol-gasoline fuel mixtures those contai-ning not more than 15% (V/V )oxygenates.

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