岩矿测试2016，Vol.35Issue(5)：481-487,7.DOI:10.15898/j.cnki.11-2131/td.2016.05.006
微波消解－氢化物发生原子荧光光谱法和质谱法测定高有机质无烟煤中汞砷的可行性研究
Feasibility Study on Content Determination of Mercury and Arsenic in High Organic Anthracite by Microwave Digestion-Hydride Generation-Atomic Fluorescence Spectrometry and Mass Spectrometry
摘要
Abstract
The microwave digestion method can be used for most coal samples,but not for those with ultra-high organic matter because they contain multiple complex high molecular organisms due to the high coalification degree and cannot be digested by digestion techniques currently available.In this paper,the conditions for microwave digestion including digestion reagents,temperature and time were investigated.The digestion system suitable for anthracite with high organic content was investigated and the feasibility on determination of total Hg and As by Hydride Generation-Atomic Fluorescence Spectrometry (HG-AFS ) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)was investigated.Results show that using nitric acid-sulfuric acid-hydrofluoric acid (6 ∶4∶0.5)as the digestion reagent and the digestion temperature of 205℃ for 30 minutes,the anthracite with high organic content can be completely digested due to the key role of sulfuric acid.The detection results of mercury by HG-AFS and ICP-MS were consistent,both recoveries of which reach more than 98%.The result of arsenic by HG-AFS was significantly lower due to incomplete transformation of organic As to inorganic As.Therefore, anthracite with high organic content (81% -90%)can be completely digested to solution by microwave technique, and Hg and As can be determined by ICP-MS.HG-AFS is not an efficient method to analyze mercury.关键词
无烟煤/砷/汞/微波消解/氢化物发生 -原子荧光光谱法/电感耦合等离子体质谱法Key words
anthracite coal/arsenic/mercury/microwave digestion/Hydride Generation-Atomic Fluorescence Spectrometry/Inductively Coupled Plasma-Mass Spectrometry分类
化学化工引用本文复制引用
杨常青,张双双,吴楠,侯艳娜,徐彩春,徐志彬..微波消解－氢化物发生原子荧光光谱法和质谱法测定高有机质无烟煤中汞砷的可行性研究[J].岩矿测试,2016,35(5):481-487,7.基金项目
国家质检总局科技项目---煤炭品质近红外光谱快速分析研究 （）
