氧弹分解-原子荧光法快速测定煤中汞  

Rapid determination of mercury in coal by oxygen flask combustion-atomic fluorescence spectrometry method

作　　者：杨常青[1] 张双双[1] 李芳[1] 甄建辉[1] 张妍[1] 徐志彬[2] 

机构地区：[1]河北出入境检验检疫局京唐港办事处,唐山063600 [2]河北出入境检验检疫局曹妃甸办事处,唐山063600

出　　处：《分析试验室》2016年第5期565-567,共3页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科技项目(2014IK270)资助

摘　　要：建立了氧弹分解一原子荧光法快速测定煤中Hg含量的方法。考察了吸收液种类、样品质量、吸收液体积、静置吸收时间对测定结果的影响，并对吸收反应机理进行了分析。结果表明，0．01mol／LKMn04（3％H2SO4）溶液作为吸收剂时，对煤中Hg的吸收最好，回收率在96％～102％；随着样品质量的增加，回收率下降，0．2g样品量最为适宜；5mL吸收液、静置吸收10min效果较好。校准曲线在0～2．0ng／mLHg范围线性良好，相关系数大于0．9995；方法检出限为7ng／g。经t检验，氧弹分解一原子荧光法与直接测汞仪法无统计学意义上的差异，方法可用于煤中Hg含量的快速检测。The method for rapid determination of mercury in coal by oxygen flask combustion atomic fluorescence spectrometry（ OFC-AFS） was established. The effect factors,including the kind of absorbent,the mass of coal,the volume of absorbent and the static adsorption time,were studied. The absorption reaction mechanism was analyzed. The results showed that the highest recovery of Hg（ 96% - 102%） was obtained by the OFC-AFS method when 0. 01 mol / L KMn O4solution（ 3% H2SO4） was employed as the solvent. The recovery of Hg was declined with the increase of the mass of coal. When the mass of the sample was 0. 2 g,the recovery of Hg was appropriate. The best result was obtained when the volume of absorbent was 5 m L and the static adsorption time was 10 min. The standard curve exhibited good linearity in the range of 0 - 2. 0 ng / m L,with the correlation coefficient higher than 0. 9995. The detection limit of method was 7 ng / g. There was no statistically significant difference between OFC-AFS and the direct mercury analyzer method. The samples could be decomposed completely,demonstrating its important practical value in the rapid detection of the mercury in coal.

关 键 词：煤炭 汞 氧弹分解 原子荧光 

分 类 号：TQ041.7[化学工程]