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氧瓶燃烧法测定煤中痕量汞的改进

Modification of the Method for Determination of Total Mercury in Coal by Oxygen Flask Combustion

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【作者】 申世刚谢明树晁春艳梁淑轩

【Author】 SHEN Shi-gang,XIE Ming-shu,CHAO Chun-yan,LIANG Shu-xuan(Hebei Provincial Key Laboratory of Analytical Science,College of Chemistry and Environmental Science,Hebei University,Baoding 071002,China)

【机构】 河北省分析科学重点实验室河北大学化学与环境科学学院河北省分析科学重点实验室河北大学化学与环境科学学院 保定071002保定071002

【摘要】 在氧瓶中采用镍铬电炉丝加热燃烧煤样,燃烧过程中形成的汞蒸气被酸性高锰酸钾溶液吸收并氧化成汞离子,经还原后用流动注射-氢化物发生冷原子吸收法测定。方法的相对标准偏差4.8%,相关系数0.999 7,回收率在91.4%~97.3%间,此方法特别适用于批量样品常规分析。

【Abstract】 Modification of the method for determination of total mercury in coal by oxygen flask combustion was proposed.Coal sample was burned in a crucible heated electrically by nichrome wire in an oxygen flask.Mercury vapour evolved was absorbed in a solution of potassium permanganate in sulfuric acid(1+9).The divalent mercury ion in the solution after reduction of permanganate with hydroxylamine hydrochloride solution was ready for determination of its content by FI-HG-AAS(cold vapour).Linearity between the absorbance and concentration of mercury(expressed as μg·L-1) was obtained with a correlation coefficient of 0.999 7.In analyzing 10 portions of the same sample by the method proposed,average value of mercury content found was 0.558 μg·L-1 with RSD(n=10) of 4.8%.Test for recovery was made by addition of standard mercury solutions of 3 different concentrations to a same coal sample,and results obtained were in the range of 91.4%-97.3%.It was proved that this method is feasible for the routine analysis of large number of samples.

  • 【文献出处】 理化检验(化学分册) ,Physical Testing and Chemical Analysis(Part B:Chemical Analysis) , 编辑部邮箱 ,2007年01期
  • 【分类号】TQ533
  • 【被引频次】10
  • 【下载频次】180
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