微波碱熔ICP-AES基体匹配法测试石油焦中多元素研究

RESEARCH ON MULTI-ELEMENTS ANALYSIS IN PETCOKE BY MICROWAVE ALKALI FUSION WITH ICP-AES AND MATRIX MATCHING METHOD

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,基体匹配法测定结果更准确。

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.