微波消解-氢化物发生原子荧光光谱法测定粉煤灰中的硒  

Determination of Selenium in Coal Ash with Microwave Digestion and Hydride Generation-Atomic Fluorescence Spectrometry

作　　者：陶秋丽 韩张雄 熊英 牟乃仓 雒虹 王曦婕 

机构地区：[1]陕西省矿产资源勘查与综合利用重点实验室,陕西省地质矿产实验研究所,陕西西安710054

出　　处：《岩矿测试》2013年第3期445-448,共4页Rock and Mineral Analysis

基　　金：陕西省自然科学基础研究计划项目(2012JM5006);陕西省地质矿产实验研究所总工基金项目(2012-01)

摘　　要：粉煤灰中含有的硒元素较高,有综合利用价值。由于基体的复杂性,并未形成成熟可靠的测定技术。本文参考煤炭样品和土壤样品中硒的原子荧光光谱分析方法,采用氢化物发生-原子荧光光谱法测定粉煤灰中的硒。样品经氢氟酸-硝酸-双氧水体系微波消解得到清亮、透明的消解液,消解液经浓盐酸还原后,加入三价铁盐消除共存元素的干扰,所加的铁盐量不干扰硒的测定。方法检出限为0.020μg/g;平行测定5份粉煤灰样品,相对标准偏差低于4.2%;加标回收率为94.0%～105.0%。应用建立的方法对煤飞灰标准物质进行分析,测定值与标准值基本相符;对不同地区的实际粉煤灰样品进行分析,证实方法可靠,可用于粉煤灰中硒元素的测定。Coal ash containing higher than usual selenium has a comprehensive utilization value. Although selenium in coal ash samples has been studied in some areas, there is no formed reliable method to determine the selenium content in coal ash due to the complex matrix. In the paper, referring to the analysis of coal and soil samples, a method to determine selenium in coal ash by Hydride Generation-Atomic Fluorescence Spectrometry （HG-AFS） is described. The samples were first digested by microwave digestion in HF ＋ HNO3 ＋ H2O2 without other pretreatment. The obtained clear and transparent digestion solution was reduced by 30% HCl. The interferences of coexisting elements were eliminated by adding Fe （Ⅲ ） salt without interference with Se. The detection limit was 0. 020 μg/g. The relative standard deviation was less than 4.2% （ n = 5）. Recoveries of samples were in the range of 94.0% - 105.0%. The method has been validated by analysis of standard reference coal fly ash and the analytical results are in agreement with certified values, which indicates that it is a feasible method to detect Se in coal ash.

关 键 词：粉煤灰 硒 微波消解 氢化物发生-原子荧光光谱法 

分 类 号：TQ536.4[化学工程—煤化学工程] O613.52[理学—无机化学]