Study on Microwave Digestion of Coal for the Determination of Multi-Element by ICP-OES and ICP-MS
WANG Hui1, 2, SONG Qiang1, YAO Qiang1, CHEN Chang-he1, YU Fei-lu2
1. Key Laboratory for Thermal Science and Power Engineering of Ministry of Education, Tsinghua University, Beijing 100084, China 2. Central Research Institute of Building and Construction MCC Group, Co. Ltd., Beijing 100088, China
摘要： 对比了不同温度以及HNO3，HNO3/H2O2，HNO3/HF和HNO3/HF+H3BO3等四种用酸对煤样微波消解效果和元素检测的影响。以SARM20作为煤标准物质。建立了一套两步微波消解及多元素检测方法。即用9 mL的HNO3与1 mL的HF分解0.1 g煤样，再加入10 mL 4%(ρ)的H3BO3中和过量HF及氟化物沉淀。使用ICP-OES检测Al，Ca，Fe，Mg，K，Na，S，Si，Sr和Ti等十种矿物元素，元素回收率在87.5%～98.8%;使用ICP-MS检测Li，Be，Sc，V，Cr，Mn，Co，Ni，Cu，Zn，Ga，As，Se，Zr，Sn，Cs，Ba，Ce，Eu和Pb等20种重金属元素，元素回收率在85%～112.5%。各元素检测的RSD均小于3%。
关键词：煤;微波消解;酸;ICP-OES;ICP-MS;多元素分析
Abstract：Effects of temperature and four acids(HNO3, HNO3/H2O2, HNO3/HF and HNO3/HF+H3BO3)on the coal decomposition by microwave digestion and the multi-element analysis were studied. SARM20 was used as a coal standard reference material. The contents of 10 mineral elements(Al, Ca, Fe, Mg, K, Na, S, Si, Sr and Ti)in the coal SARM20 were determined by inductively coupled plasma-optical emission spectrometry(ICP-OES). And the contents of 20 heavy metals(Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, As, Se, Zr, Sn, Cs, Ba, Ce, Eu and Pb)were determined by inductively coupled plasma-mass spectrometry(ICP-MS). The results showed that the coal was completely decomposed by microwave digestion with HNO3/HF+H3BO3 at 210 ℃. Good recoveries for all elements in the coal SARM20 were obtained by this two-step microwave digestion method. The recoveries of the 10 mineral elements were from 87.5% to 98.8%, and the recoveries of the 20 heavy metals were from 85% to 112.5%. All RSDs of tests were below 3%.
王 珲1，2，宋 蔷1，姚 强1，陈昌和1，俞非漉2 . ICP-OES/ICP-MS测定煤中多种元素的微波消解方法研究[J]. 光谱学与光谱分析, 2012, 32(06): 1662-1665.
WANG Hui1, 2, SONG Qiang1, YAO Qiang1, CHEN Chang-he1, YU Fei-lu2 . Study on Microwave Digestion of Coal for the Determination of Multi-Element by ICP-OES and ICP-MS. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2012, 32(06): 1662-1665.
