氧弹分解-原子荧光法快速测定煤中汞方法的改进  

The improvement of rapid determination of mercury in coal by oxygen flask combustion-atomic fluorescence spectrometry

作　　者：杨常青 萧达辉[2] 康菲[3] 蒋钊[3] 白冰[3] 李芳[3] YANG Chang-qing XIAO Da-hui KANG Eel JIANG Zhao BAI Bing LI Fang(Inner Mongolia Entry-Exit Inspection And Quarantine Bureau, Hohhot 010020 Guangdong Entry-Exit Inspection And Quarantine Bureau, Guangzhou 510326 Jingtanggang Office of Hebei Entry-Exit Inspection And Quarantine Bureau, Tangshan 063600)

机构地区：[1]内蒙古出入境检验检疫局,呼和浩特010020 [2]广东出入境检验检疫局技术中心,广州510326 [3]河北出入境检验检疫局京唐港办事处,唐山063600

出　　处：《分析试验室》2017年第10期1184-1187,共4页Chinese Journal of Analysis Laboratory

基　　金：检验检疫行业标准计划(2015B068);国家质检总局科技项目(2014IK270)资助

摘　　要：改进了氧弹燃烧分解-原子荧光法快速测定煤中汞含量方法。在之前研究结果的基础上,进一步考察了氧气含量、样品质量对测定结果的影响,以及该方法对不同煤种、不同灰分含量煤炭样品的适应性。结果表明,维持前方法的其他条件不变,通过反复充放氧气提高氧弹内氧气的含量,样品质量可由原来的0.2 g增加至约1.0 g,回收率可达98%以上;当样品中的汞含量较低时,适当减小样品质量仍能获得理想的回收率。经与权威标准方法比对,该方法对无烟煤、烟煤、褐煤都有很好的适应性,灰分含量在9.76%~46.62%(干基)范围内检测结果不受灰分含量影响。经过有证国家标准物质验证,方法准确可靠。改进后的方法可以促进煤炭样品的充分燃烧、煤中汞的释放以及被酸性高锰酸钾溶液转化吸收,克服了原方法对汞含量低的样品回收率低以及由于称样量小而导致的称量误差大、样品代表性差的缺点,同时提高了仪器的响应值,降低了方法检出限,具有更强的实用价值,可用于煤中汞含量的快速检测。The rapid method for determination of mercury in coal by oxygen flask combustion atomic fluorescence spectrometry （OFC-AFS） was improved. Based on our previous studies, the effects of oxygenation content, sample weight on the results and the adaptability of the method to coal samples with different types and ash contents were studied. The results show that the oxygen content in the bomb can be increased by repeating oxygen injection, and thus the mass of the sample could be increased from 0. 2 g to 1.0 g, and the recovery could reach over 98%. When the mercury content in sample was low, the ideal recovery could also be obtained by appropriately reducing the mass of the sample. By comparing with authoritative standard method, the method had good adaptability to anthracite, bituminous and lignite coal and the results were not affected by ash content in the range of 9.76% - 46.62% （dry basis）. Certified by national standards, the method was accurate and reliable. The improved method c could promote the full burning of coal samples, the release of mercury in coal and the transformation and absorption by acid potassium permanganate solution, and overcame the shortcomings of the original method, such as large weighing error and poor sample representation,low recovery rate of low mercury content sample, and enhanced the response value of the instrument and reduced the method detection limit （MDL）, and thus had stronger practical value, and could be used for rapid detection of mercury content in coal.

关 键 词：煤炭 汞 氧弹分解 原子荧光 改进 

分 类 号：TQ041.7[化学工程]