Determination of 34 trace elements in iron ore by high resolution inductively coupled plasma mass spectrometry with microwave digestion
GAN Zhaoxiang1,2, MIN Hong2, QIN Yeqiong2, LIU Shu*2, ZHANG Linping*1
1. College of Chemistry and Chemical Engineering, Donghua University,Shanghai 201620, China; 2. Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs District,Shanghai 200135, China
摘要 铁矿石中痕量元素的含量具有产地特征,准确测定其含量对揭示铁矿石产地信息具有重要意义。采用6 mL HNO3、1 mL HF、2 mL HCl微波消解铁矿石样品,经150 ℃赶酸,2%HNO3复溶,以103Rh为内标,选择高分辨模式测定Tb、Dy、Er、Tm、Lu,中分辨模式测定Zn、Gd,低分辨模式测定其余元素,建立微波消解-高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定铁矿石中包含稀土元素在内的34种痕量元素(Be、Cr、Mn、Co、Y、Nb、Mo、Cs、Sb、Ba、Nd、Sm、Ta、Pb、Bi、Th、U、V、Zn、Rb、Sr、Sn、La、Ce、Pr、Eu、Tb、Gd、Dy、Ho、Tm、Yb、Lu)的分析方法。在优化的实验条件下,目标元素校准曲线线性相关系数均在0.999 7以上,检出限在0.001 8～0.3 mg/kg之间。选择铁矿石标准样品进行方法学验证,各元素回收率在90%～109%之间,实验室内变异系数在0.6%～6.9%之间。选取澳大利亚、巴西、南非3个国家铁精粉样品进行检测,铁精粉样品实验室内变异系数范围为0.31%～11.2%,表明方法稳定可靠。分析了不同产地铁精粉痕量元素的差异,可为利用痕量元素差异鉴别不同产地铁矿石提供数据支撑。
Abstract：The contents of trace elements in iron ore have characteristics of original producing area, so the accurate determination of elemental content is of great significance to the study of the origin information of iron ore. In experiments, 6 mL of HNO3, 1 mL of HF and 2 mL of HCl were used for the microwave digestion of iron ore samples. After evaporation of acid at 150 ℃, the sample was redissolved with 2%HNO3. 103Rh was used as the internal standard to determine Tb, Dy, Er, Tm and Lu were in high-resolution pattern, to determine Zn and Gd in mid-resolution pattern and to determine the remaining elements in low resolution pattern. The method for the determination of 34 trace elements (Be, Cr, Mn, Co, Y, Nb, Mo, Cs, Sb, Ba, Nd, Sm, Ta, Pb, Bi, Th, U, V, Zn, Rb, Sr, Sn, La, Ce, Pr, Eu, Tb, Gd, Dy, Ho, Tm, Yb and Lu) in iron ores by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) with microwave digestion was established. Under the optimized experimental conditions, the linear correlation coefficients of 34 elements were all greater than 0.999 7, and the limits of detection of the method were in range of 0.001 8-0.3 mg/kg. The iron ore standard sample was selected for method verification. It was found that the recoveries of elements were in range of 90%-109%, and the intra-laboratory variable coefficients were in range of 0.6%-6.9%. Three representative fine iron powder samples from Australia, Brazil and South Africa were selected for testing. The intra-laboratory variable coefficients were in range of 0.31%-11.2%, which indicated the proposed method was stable and reliable. The differences of trace elements in fine iron powder from different areas were analyzed, which provided data support for the identification of iron ores from different producing areas.
干兆祥, 闵红, 秦晔琼, 刘曙, 张琳萍. 微波消解-高分辨电感耦合等离子体质谱法测定铁矿石中34种痕量元素[J]. 冶金分析, 2023, 43(5): 17-26.
GAN Zhaoxiang, MIN Hong, QIN Yeqiong, LIU Shu, ZHANG Linping. Determination of 34 trace elements in iron ore by high resolution inductively coupled plasma mass spectrometry with microwave digestion. , 2023, 43(5): 17-26.
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