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电感耦合等离子体质谱法测定菱镁矿中8种痕量元素

Determination of 8 trace elements in magnesite by inductively coupled plasma mass spectrometry

  • 摘要: 菱镁矿作为一种重要的工业矿物原料,其痕量元素的准确测定对环境保护、资源利用及地质研究具有重要意义。传统分析方法因灵敏度不足、多元素同步检测能力有限,难以满足痕量元素的高效分析需求。为此,本研究建立了一种基于电感耦合等离子体质谱法(ICP-MS)测定菱镁矿中As、Co、Cu、Pb、Th、La、U、Li等8种痕量元素的分析方法。通过对样品前处理条件的系统优化,确定以HNO3-HF-HClO4-HCl混酸体系(5 mL-2 mL-1.5 mL-1.5 mL)于180℃密闭消解6 h,称样量为0.100 0 g。针对高镁基体产生的多原子离子干扰,采用碰撞反应池技术,在碰撞(KED)模式(含2%H2的He)下消除As、La、U等元素的质谱干扰,在标准(STD)模式(He碰撞)下测定Co、Cu、Th、Li等元素,并优化了各元素的测定质量数。通过在线加入103Rh内标进行动态校正,有效克服了基体效应和仪器信号漂移。各元素校准曲线的线性相关系数均大于0.999;方法检出限为0.001~0.008μg/g,定量限为0.004~0.025μg/g。按照实验方法测定菱镁矿成分分析标准物质GBW07865和GBW07866中As、Co、Cu、Pb、Th、La、U、Li,各元素测定结果的相对标准偏差(RSD,n=6)为2.6%~3.4%,相对误差|RE|为1.75%~4.88%;对5个实际菱镁矿样品的分析结果显示,8种痕量元素含量均处于较低水平;其中选取2个样品进行方法比对(本法与微波消解-ICP-MS),结果吻合良好,进一步验证了所建方法的可靠性。

     

    Abstract: Magnesite is an important industrial mineral raw material. The accurate determination of trace elements in magnesite is of great significance for the environmental protection, resource utilization, and geological research. Traditional analytical methods suffer from low sensitivity and inadequate capabilities in multi-element simultaneous detection, which cannot meet the efficient analysis requirements for trace elements. Therefore, an analysis method for the determination of eight trace elements(including As, Co, Cu, Pb, Th, La, U, and Li) in magnesite by inductively coupled plasma mass spectrometry(ICP-MS) was established in this study. The pretreatment conditions of sample were systematically optimized: the mixed acid system was composed of 5 mL HNO3, 2 mL HF, 1.5 mL HClO4 and 1.5 mL HCl; the sample was digested in closed system at 180 ℃ for 6 h; the sample mass was 0.100 0 g. The collision reaction cell technology was employed to eliminate the polyatomic ion interference caused by high-magnesium matrix. The mass spectrometry interference of As, La and U could be eliminated under kinetic discrimination(KED) mode(using He gas with 2% H2). The contents of Co, Cu, Th, and Li were determined under standard(STD) mode(He collision). In addition, the mass numbers of elements for determination were optimized. 103Rh was introduced online as an internal standard for the dynamic calibration, which effectively overcame the matrix effects and instrumental signal drift. The linear correlation coefficients of calibration curves for testing elements were all higher than 0.999. The limits of detection ranged from 0.001 to 0.008 μg/g, and the limits of quantification were between 0.004 and 0.025 μg/g. The contents of As, Co, Cu, Pb, Th, La, U and Li in CSMs magnesite composition analysis(GBW07865 and GBW07866) were determined according to the experimental method. The relative standard deviations(RSD, n=6) of determination results were between 2.6% and 3.4%, and the relative errors(|RE|) were between 1.75% and 4.88%. The analysis results of five actual magnesite samples indicated that the contents of eight trace elements were all at low level. Two samples of them were selected for the method comparison(this method and microwave digestion-ICP-MS). The measurement results showed good consistency, which further proved the reliability of proposed method.

     

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