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    有机进样系统-电感耦合等离子体原子发射光谱法测定轻质油品中铁、锰、铅、硅的含量

    Determination of Ferrum, Manganese, Lead and Silicon in Lightweight Oil by Inductively Coupled Plasma-Atomic Emission Spectrometry Combined with Organic Sampling System

    • 摘要: 建立了有机进样系统-电感耦合等离子体原子发射光谱法(ICP-AES)测定轻质油品中铁、锰、铅、硅含量的方法。称取5.000 0 g轻质油品于塑料瓶中,加入45 g内标溶液,得到待测轻质油品溶液。利用有机进样系统直接进样分析,内标法定量。在ICP-AES分析中,铁、锰、铅、硅的分析谱线分别为238.204,257.610,220.353,251.611 nm,射频功率为1 100~1 300 W,辅助气流量为2.0 L·min-1,雾化气流量为0.30 L·min-1,冷却气流量为16 L·min-1,加氧量为20~35 mL·min-1。结果显示:铁、锰、铅、硅校准曲线的线性范围均在5.0 mg·kg-1以内,检出限(2.821s)均小于0.01 mg·kg-1;于2 h内对0.2 mg·kg-1基质匹配的混合标准溶液进行测定,各元素测定值的相对标准偏差(RSD,n=8)小于6.0%;对0.1,0.2,1.0 mg·kg-1基质匹配的混合标准溶液进行测定,各待测元素测定值的RSD (n=6)为2.6%~7.9%;对实际样品进行加标回收试验,回收率为97.7%~103%。

       

      Abstract: A method for determination of ferrum, manganese, lead and slicon in lightweight oil by inductively coupled plasma-atomic emission spectrometry (ICP-AES) combined with organic sampling system was established. Lightweight oil of 5.000 0 g was placed in plastic bottle, and internal standard solution of 45 g was added to prepare lightweight oil solution for test. Internal standard method was used for quantitative analysis by organic sampling system. In ICP-AES analysis, analytical spectral lines of ferrum, manganese, lead and silicon were 238.204, 257.610, 220.353 nm and 251.611 nm, respectively, with radio frequency power of 1 100-1 300 W, auxiliary gas flow rate of 2.0 L·min-1, atomization gas flow rate of 0.30 L·min-1, cooling gas flow rate of 16 L·min-1, oxygen flow rate of 20-35 mL·min-1. It was showed that linear ranges of calibration curves of ferrum, manganese, lead and silicon were within 5.0 mg·kg-1, and detection limits (2.821s) were less than 0.01 mg·kg-1. RSDs (n=8) of determined values of each analyted element on 0.2 mg·kg-1 matrix matching mixed standard solution were less than 6.0% within 2 h. Matrix matching mixed standard solutions with mass fractions of 0.1, 0.2, 1.0 mg·kg-1 were determined, and RSDs (n=6) of determined values for each analyted element were in the range of 2.6%-7.9%. Recovery test was made on substantial samples by standard addition method, giving results in the range of 97.7%-103%.

       

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