电感耦合等离子体发射光谱法同时测定钒钛磁铁矿中钒钛钴镍
Determination of V, Ti, Co and Ni in Vanadium and Titano Magnetite by Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 钒钛磁铁矿样品经过氧化钠熔融,盐酸提取,溶液分取稀释后用电感耦合等离子体发射光谱法同时测定其中的V2O5、TiO2、Co、Ni。实验确定过氧化钠的用量为1.5 g,盐酸的用量为10 mL,选择干扰元素较少和背景干扰较小的V、Ti、Co、Ni分析谱线分别为292.4 nm、334.9 nm、230.7 nm、231.6 nm,在稀释因子为10(总稀释因子5000)的条件下进行分析,方法检出限为0.05~0.17 μg/g。用国家一级钒钛磁铁矿标准物质GBW 07225(原矿)、钒钛磁铁矿标准物质GBW 07226a(精矿)、钒钛磁铁矿标准物质GBW 07227(尾矿)验证方法精密度和准确度,方法精密度(RSD,n=12)为0.41％~1.91％;除含量较低的Ni和Co外,相对误差(RE,n=4)均小于5％。通过安装氩气加湿器有效地解决了盐分较大带来的影响,在标准系列中加入等量空白溶液,保持基体与试样一致,消除了基体效应。方法分解样品彻底完全,分析流程简单,易于掌握,一次熔样可以同时测定多种元素,可适用于大批量样品分析。Abstract: Vanadium and titano magnetite was melted by sodium peroxide, then extracted by HCl. The sample solution was diluted before V2O5, TiO2, Co and Ni were simultaneously directly determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES). 1.5 g Na2O2 and 10 mL HCl were used in the chemistry procedure. The analysis spectral lines of 292.4 nm, 334.9 nm, 230.7 nm and 231.6 nm were selected to measure V, Ti, Co and Ni based on less interference elements and matrix interference. The detection limits of the method were 0.17 μg/g for V2O5, 0.05 μg/g for TiO2, 0.06 μg/g for Co and 0.011 μg/g for Ni under the dilution factor of 10 (the sum dilution factor was 5000). The reliability of the method has been tested by determination of those elements in national standard reference materials of GBW 07225, GBW 07226a and GBW 07227. The results were in good agreement with certified values, with a precisions of 0.41%-1.91% (RSD, n=12). The REs were less than 5% except for Ni and Co. The instalment of an Ar humidifier resolved the effect of high salinity. The matrix effect was overcome by the addition of the same amount of blank solution with the standard solution. This method exhibited simplicity, rapidity, good reproducibility and wide linearity making it suitable for multi-elemental determination.
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