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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
【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.
【Key words】 Oxygen flask combustion; Nichrome wire; Flow-injection-hydride-generation-cold vapor atomic absorption spectrometry; Coal; Mercury;
- 【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