ICP-AES法分析辉锑矿

Analysis of Stibnite by ICP-AES

本文针对辉锑矿成分复杂、主元素Sb易水解、部分元素易挥发,酸不溶元素的存在以及元素之间的干扰等问题,拟定了酸溶和碱熔分解试样的分析流程。在酸溶系统中结合TBP萃淋树脂和巯基棉分离富集分组,ICP-AES法测定Fe、Ca、Mg、Cu、Mn、Pb、Zn、Co、Ni、Au、Ag、In、Tl、Cd、Bi、Ga、Mo、Se、Te、As等20个元素。碱熔系统不分离主元素,用校正因素校正元素间光谱干扰并采用内标法ICP-AES测定Al、Ti、V、Ba、Sr、Sn、Sc、Cr、Be、Si和Sb等11个元素。试样验证表明,方法可行。

Several procedures have been established for the analysis of stibnite by ICP-AES. In the first procedure, 17 elements are determinable. The sample is dissolved in aqua reqia, the matrix element, Sb, and associated elements, As and Se, are volatilised with HBr as bromide. Some elements, such as In, TI, Bi, Cd, Au and Ag are quantitatively extracted onto TBP Levextrel resin from 0.8mol/L HBr medium, and eluted with different eluents. Whereas Ga, Mo, Fe, Ca, Mg, Co, Ni, Pb, Zn and Mn pass directly into the effluent, Ga and Mo in the effluent are Separated again from other metals in 3mol/L HC1 by TBP. In the second scheme, trace amounts of Se (Ⅳ) and Te(Ⅳ) are adsorbed by Sulfhydryl Cotton Fiber in 1mol/L HCl and determined after deadsorption in HCl + HNO3(3 + 2). Arsenic is also adsorbed by the Fiber after reducing to As (Ⅲ) with KI and SnCl2 in 5mol/L HCl. Fusion with in a graphite crucible is suggested for metal oxides which are insoluble in acids. The melt is dissolved in 15% HCl-2% Citric acid solution and 11 elements are determined.