电感耦合等离子体-质谱同时测定煤、焦中砷、溴、碘  

Simultaneous Determination of Arsenic,Bromine,Iodine in Coal and Coke by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion

作　　者：高运川[1] 高勤芬[1] 孙明星[2] 朱志秀[2] 陈宗宏[2] 

机构地区：[1]上海师范大学环境工程系,上海200234 [2]上海出入境检验检疫局,上海200135

出　　处：《分析化学》2007年第8期1175-1178,共4页Chinese Journal of Analytical Chemistry

基　　金：国家质检总局资助项目(No2006IK053)

摘　　要：采用硝酸-氢氟酸-过氧化氢混合酸体系,高温密闭微波技术快速消解了不同国家的煤、焦样品,建立了电感耦合等离子体-质谱法同时测定煤、焦中微量As、Br、I元素的方法。考察了HNO3介质及其它酸对被测元素的影响。筛选出了强氧化剂过硫酸钠可将不同低价态的溴、碘氧化成稳定高价态,解决了因价态不同引起的ICP-MS测定中信号强、波动大且无规则性的问题。加入Ag+可加快氧化速度。用中性混合洗液充分清洗后,可有效降低卤素的高记忆效应。本方法简便快速,方法检出限低(0.1～5.0μg/L),精密度好(1.5%～12.0%),回收率在80%～106.7%范围,结果满意。Using high pressure and closed microwave digestion technology, the imports and exports coal and coke samples from different countries were digested quickly by mixed acids of nitric acid, hydrofluoric acid and hydrogen peroxide solution, a method for simultaneous determination of trace elements, such as arsenic, bromine, and iodine, in coal and coke by ICP-MS was established. The influence of medium of nitric acid and other acids on determined elements was researched. The unstable mass signal of bromine and iodine on account of different valence can be stabled by adding sodium persulfate. And the silver ion can catalyse and accelerate the reaction mentioned above. High memory effect of halogen was effectively decreased by washing with neutral mixed lotion. The low detection limits are in the range of 0.1 - 5.0 μg/L with relative standard deviations of 1.5% - 12.0% and the recoveries are in the range of 80% - 106.7%. The analysis results are satisfied.

关 键 词：微波消解 电感耦合等离子体一质谱 煤炭样品 砷 溴 碘 

分 类 号：TQ533.1[化学工程—煤化学工程] O657.63[理学—分析化学]