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

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5.0000g轻质油品于塑料瓶中,加入45g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238.204,257.610,220.353,251.611nm,射频功率为1100~1300W,辅助气流量为2.0L·min^(-1),雾化气流量为0.30L·min^(-1),冷却气流量为16L·min^(-1),加氧量为20~35mL·min^(-1)。结果显示:铁、锰、铅、硅校准曲线的线性范围均在5.0mg·kg^(-1)以内,检出限(2.821s)均小于0.01mg·kg^(-1);于2h内对0.2mg·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0.1,0.2,1.0mg·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%。

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 5.0000g was placed in plastic bottle,and internal standard solution of 45g 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 238.204,257.610,220.353nm and 251.611nm,respectively,with radio frequency power of 1100-1300W,auxiliary gas flow rate of 2.0L·min^(-1),atomization gas flow rate of 0.30L·min^(-1),cooling gas flow rate of 16L·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 5.0mg·kg^(-1),and detection limits(2.821s)were less than 0.01mg·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 2h.Matrix matching mixed standard solutions with mass fractions of 0.1,0.2,1.0mg·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%.