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。
A method for determination of calcium, iron, sodium, nickel, vanadium in asphalt by microwave ashinginductively 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.
出处
《光谱实验室》
CAS
CSCD
2012年第6期3620-3624,共5页
Chinese Journal of Spectroscopy Laboratory
基金
国家质检总局科技项目(2009IK069)
质检公益性项目(2012424041)
