摘要:
样品采用HCl-HF-HNO3-HClO4四酸溶矿、H2SO4-HF-HNO3三酸溶矿、KOH碱熔3种分解方法进行处理,电感耦合等离子体发射光谱法(ICP-AES)测定钒钛磁铁矿中的铁、钛、钒。结果表明,3种样品处理方法应用于ICP-AES测定是可行的。KOH碱熔适用于方法比对,三酸溶矿适用于样品内检分析,四酸溶矿适用于大批量样品测定。对铁、钛、钒三元素选择适合的分析谱线,以冶金行业钒钛磁铁矿标准样品制备的溶液绘制标准曲线,可消除试液基体和介质不一致对测定结果的影响。样品试液中主要共存离子对选择的分析线干扰小。采用四酸溶矿ICP-AES测定铁、钛、钒的方法检出限分别为0.0032%、0.0024%、0.0003%,方法精密度(RSD,n=12)为0.43%~5.06%。经实验室间比对和批量样品方法比对实验,测定值无明显系统偏差。建立的方法具有样品分解完全、测定含量范围宽、分析简便快速、结果准确等优点,适用于钒钛磁铁矿样品中铁、钛、钒的测定。
Abstract:
A method for the determination of Fe, Ti and V in vanadium titanomagnetite ore sample by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) is presented. The sample was digested by 3 different systems: 4 acid digestion of HCl-HF-HNO3-HClO4, 3 acids digestion of H2SO4-HF-HNO3 and KOH alkali fusion. The results verify all 3 digestion methods as being applicable for vanadium titanomagnetite ore samples by ICP-AES. KOH alkali fusion made a good comparison among the different methods, 3 acids digestion was suitable for internal testing and 4 acids digestion was suitable for a large amount of samples. The optimal analytical lines were selected for the determination of V, Ti and Fe. Work calibration curves were established by using the standard material of vanadium titanomagnetite ore for the metallurgy industry, which avoids the matrix effect during the measurement. The main ions in the sample solution have little interference for the selected analytical lines. The detection limits of V, Ti and Fe by ICP-AES with 4 acids digestion were 0.0032%, 0.0024% and 0.0003%, respectively. The RSDs were between 0.43%-5.06%. Applicability and feasibly of the method were verified by comparison of results obtained by different laboratories without significant system deviation. This method has the advantages of complete digestion, fast, accurate determination, and a wide range of measured contents. It is suitable for determining Fe, Ti and V in vanadium titanomagnetite ore.
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