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[微波消解石膏用于电感耦合等离子体发射光谱法和电感耦合等离子体质谱法测定多元素的研究]

[Study on microwave digestion of gypsum for the determination of multielement by ICP-OES and ICP-MS].

作者信息

Wang Hui, Song Qiang, Yang Rui-ming, Yao Qiang, Chen Chang-he

机构信息

Key Laboratory for Thermal Science and Power Engineering of Ministry of Education, Tsinghua University, Beijing, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2010 Sep;30(9):2560-3.

Abstract

Three acids (HNO3, HNO3/HF and HNO3 /HF+ H3BO3) were used to decompose gypsum with microwave digestion system. The contents of 10 mineral elements (Al, Ca, Mg, Fe, K, Na, S, Ti, Si and Sr) in gypsum were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) while 6 heavy metals (V, Cr, Mn, Zn, Se and Ce) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). GBW03109a, GBW03110 and FGD-2 were used as gypsum standard reference materials. The results showed that two-step microwave digestion with HNO3/HF at 210 degrees C and then adding H3BO3 for the removal of HF and fluorides completely decomposed the gypsums, while this method achieved good recoveries for all elements in the three gypsum standard reference materials. The recovery was from 88% to 112% and the RSD of tests was below 3%. The method was applied to the elemental analysis for flue gas desulfurization gypsums from three coal-fired power plants.

摘要

使用三种酸(硝酸、硝酸/氢氟酸和硝酸/氢氟酸 + 硼酸)通过微波消解系统分解石膏。采用电感耦合等离子体发射光谱法(ICP - OES)测定石膏中10种矿物元素(铝、钙、镁、铁、钾、钠、硫、钛、硅和锶)的含量,同时采用电感耦合等离子体质谱法(ICP - MS)测定6种重金属(钒、铬、锰、锌、硒和铈)的含量。使用GBW03109a、GBW03110和FGD - 2作为石膏标准参考物质。结果表明,在210℃下用硝酸/氢氟酸进行两步微波消解,然后加入硼酸以完全去除氢氟酸和氟化物,可使石膏完全分解,同时该方法在三种石膏标准参考物质中对所有元素均具有良好的回收率。回收率为88%至112%,测试的相对标准偏差低于3%。该方法应用于三个燃煤电厂烟气脱硫石膏的元素分析。

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