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酸解微波灰化-ICP-OES测定石油沥青中的钙、铁、钠、镍和钒元素
Determination of Calcium,Iron,Sodium,Nickel,Vanadium in Asphalt by Acid Decomposition Microwave Ashing-ICP-OES
【摘要】 采用微波灰化-电感耦合等离子体-发射光谱法测定石油沥青中的钙、铁、钠、镍和钒元素。石油沥青样品通过硫酸酸解处理,解决了样品无法低温灰化的问题,并对微波灰化温度、硫酸用量、升温程序及样品称样量进行了详细研究,结合差示扫描量热法确立了石油沥青微波灰化前处理的最佳条件。钙、铁、钠、镍和钒元素方法检出限分别为0.04、0.10、0.64、0.28、0.22mg·kg-1。加标回收率在79.7%—97.8%之间,相对标准偏差为3.4%—8.3%,重复性和回收率实验结果表明该方法能满足石油沥青中元素分析的要求。
【Abstract】 A method for determination of calcium,iron,sodium,nickel,vanadium in asphalt by microwave ashing-inductively coupled plasma-optical emission spectrometry(ICP-OES) was developed.The asphalt samples were treated with sulfuric acid in order to solve the problem of low temperature ashing.The temperature of microwave ashing,amount of sulfuric acid,temperature program and weight of sample were studied in detail.Combined with differential scanning calorimetry,the optimum conditions of pre-treatment of microwave ashing were established.The detection limits of calcium,iron,sodium,nickel,vanadium were 0.04,0.10,0.64,0.28,0.22 mg·kg-1,respectively.The recoveries were in the range of 79.7%—97.8% and the relative standard deviations were between 3.4 % and 8.3 %.These results showed that the method met the elemental analysis in the asphalt.
【Key words】 Microwave Ashing; DSC; ICP-OES; Asphalt; Acid Decomposition;
- 【文献出处】 光谱实验室 ,Chinese Journal of Spectroscopy Laboratory , 编辑部邮箱 ,2012年06期
- 【分类号】O657.31;TE626.86
- 【被引频次】4
- 【下载频次】142