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

作　　者：申世刚[1] 谢明树[1] 晁春艳[1] 梁淑轩[1] 

机构地区：[1]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

出　　处：《理化检验（化学分册）》2007年第1期51-53,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

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。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 samnles.

关 键 词：氧瓶燃烧法 镍铬丝 流动注射-氢化物发生原子吸收法 煤 汞 

分 类 号：O657.31[理学—分析化学]