微波消解-冷原子荧光法测定煤中痕量汞  

Determination of Trace Mercury in Coal by Microwave Digestion and Cold Vapor Atomic Fluorescence Spectrometry

作　　者：刘晶[1] 郑楚光[1] 徐杰英[1] 

机构地区：[1]华中科技大学煤燃烧国家重点实验室,湖北武汉430074

出　　处：《光谱学与光谱分析》2004年第9期1133-1135,共3页Spectroscopy and Spectral Analysis

基　　金：国家重点基础研究发展规划项目 (G1 9990 2 2 2 1 2 ;2 0 0 2CB2 1 1 60 2 )资助

摘　　要：微波消解技术具有样品溶解完全、污染少、节约试剂和方便快捷等特点。文章采用微波消解预处理煤样 ,并用冷原子荧光法测定样品中的痕量汞。采用硝酸 盐酸 氢氟酸消解体系 ,进行了微波消解条件的选择 ,并考察了载气流量、屏蔽气流量、负高压和干扰等对测定的影响。在选定的操作条件下 ,汞的检出限为0 0 3ng·mL-1,相对标准偏差 (n =7)小于 5 %。方法准确、快速和方便 ,利用国家标准参考物质煤飞灰GBW 0 84 0 1验证了方法的准确度 。A method of determining trace Hg in coal by microwave digestion and cold vapor atomic fluorescence spectrometry is reported. The digestion system of HNO3-HCl-HF was evaluated. The experimental conditions of microwave digestion, including pressure, temperature, power and time of digestion were evaluated. The operating conditions such as flow rate of carrier gas, flow rate of shield gas and negative high voltage, and interference were also investigated. Testing results show that the detection limit is 0.03 ng(.)mL(-1) and RSD (n = 7) is below 5%. This method is simple and rapid. The treatment method was applicable to determining trace Hg in coal and gave results that were in good agreement with the certified values of the standard reference material.

关 键 词：微波消解 冷原子荧光法 含量测定 煤 痕量分析 汞 

分 类 号：TQ533[化学工程—煤化学工程]