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建立了氧弹分解-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,0.01 mol/L KMn O_4(3%H_2SO_4)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,0.2 g样品量最为适宜;5 m L吸收液、静置吸收10 min效果较好。校准曲线在0~2.0 ng/m L Hg范围线性良好,相关系数大于0.9995;方法检出限为7 ng/g。经t检验,氧弹分解-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。
A method for rapid determination of Hg in coal by oxygen bomb decomposition - atomic fluorescence spectrometry was established. The effects of the type of absorbent, the mass of sample, the volume of absorbent and the time of standing absorption on the determination results were investigated. The mechanism of absorption reaction was also analyzed. The results showed that when 0.01 mol / L KMnO 4 (3% H 2 SO 4) solution was used as absorbent, the Hg absorption in coal was the best and the recovery was between 96% and 102%. With the increase of sample quality, g sample volume is the most appropriate; 5 m L absorbing liquid, static absorption 10 min better. The calibration curve showed a good linearity in the range of 0-2.0 ng / m L Hg with a correlation coefficient greater than 0.9995. The detection limit was 7 ng / g. There was no significant difference between oxygen bomb decomposition - atomic fluorescence spectrometry and direct mercury determination by t test. The method can be used for rapid detection of Hg in coal.