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微波碱熔ICP–AES基体匹配法测试石油焦中多元素研究
引用本文:荣丽丽,王磊,赵铁凯,张岩,孙玲.微波碱熔ICP–AES基体匹配法测试石油焦中多元素研究[J].石油炼制与化工,2020,51(9):92-97.
作者姓名:荣丽丽  王磊  赵铁凯  张岩  孙玲
作者单位:中国石油石油化工研究院大庆化工研究中心
摘    要:为了准确测定石油焦中元素含量,采用微波马弗炉程序升温,对石油焦样品进行灰化处理,于900 ℃高温下以四硼酸锂作助熔剂将样品熔融,在低温下用盐酸溶解熔融后的玻璃液,制得样品水溶液。选择各元素最佳分析谱线,利用基体匹配方法,以电感耦合等离子发射光谱仪对样品溶液中的铝、钙、钠、铁、锰、镍、钒和硅元素进行测定。进行加标回收试验,回收率在95%~105%之间;精密度考察结果表明各元素的相对标准偏差(n = 6)均小于5%,对比未使用基体匹配的方法,结果表明基体匹配法测定结果准确。

关 键 词:ICP-AES  微波碱融  基体匹配  石油焦炭  
收稿时间:2020-03-16
修稿时间:2020-04-17

RESEARCH ON MULTI-ELEMENTS ANALYSIS IN PETCOKE BY MICROWAVE ALKALI FUSION WITH ICP-AES AND MATRIX MATCHING METHOD
Abstract:In order to accurately determine the element content in petcoke, the programmed temperature method in microwave muff furnace was used to ash the petcoke samples, followed by lithium tetraborate fusion treatment at 900 ℃ to prepare molten glass, and then dissolved in hydrochloric acid at low temperature to obtain the sample solutions to be tested. The element content of Al, Ca, Na, Fe, Mn, Ni, V and Si in the sample solutions were determined by the optimum characteristic spectral lines for each element using ICP-AES and matrix matching method. The standard recovery rate was between 95% and 105%, and the relative standard deviation (RSD, n = 6) of each element was less than 5%. The matrix matching method shows lower RSD and higher standard recovery rate than without matrix matching method.
Keywords:ICP-AES  microwave alkali fusion  matrix matching  petcoke  
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