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氧气反应模式-四极杆ICP-MS定量高温合金中痕量元素及质谱干扰消除机理研究

Quantification of Trace Elements in Superalloy by Quadrupole ICP-MS Based on Oxygen Reaction Mode and Study on the Elimination Mechanism of Spectral Interference

    摘要
  • 摘要: 本研究建立了氧气反应模式-四极杆电感耦合等离子体质谱（Q-ICP-MS）法准确定量高温合金中痕量杂质元素，对不同碰撞/反应模式消除质谱干扰的效果进行研究。结果表明，氧气动态反应池（DRC-O2）模式下，目标元素Cd的多原子离子质谱干扰能够被有效去除；在优化气流为2 mL/min时，信噪比达到最高，检出限较标准模式（STD）降低了近3个数量级。此外，还研究了质谱干扰的消除机理，发现对于元素X（X=Rb、Nb、Mo、Cs、Ta、W或U），当X−O键能大于O−O键能时，质谱干扰组分XO转化成非干扰组分XOO为自发反应，因此，O2充足时更容易生成XOO，从而消除XO干扰。在此基础上，采用高浓度基体模拟溶液（Mo、Nb、Ta、W）分别对痕量Cd、Ag、Au、Hg元素测量的方法学参数进行评估，方法检出限0.08～0.31 μg/g、测量重复性相对标准偏差（RSD）2.3%～3.1%（n=6），加标回收率98%～103%，并进一步使用高温合金标准物质验证了方法的可靠性。最后，对3类典型牌号高温合金样品中的痕量杂质进行测量，证明该方法的分析速度快、检出限低、准确可靠，能够满足高温合金中主量Mo、Nb、Ta、W元素存在时被干扰杂质的测量要求。

     

    Abstract: A method of quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) based on oxygen reaction mode was established for the accurate determination of trace impurity elements in superalloys. The effect of the collision/reaction mode on the removal of mass spectral interference was investigated. By contrast, the polyatomic mass spectral interference on the target element Cd can be effectively removed under oxygen dynamic reaction cell (DRC-O2) mode. The signal-to-noise ratio (SNR) peaked when the gas flow was 2 mL/min, and the detection limit was approximately three orders of magnitude lower than that under standard (STD) mode. In addition, the elimination mechanism of mass spectrometric interference was studied. It was found that for the element X (X=Rb, Nb, Mo, Cs, Ta, W or U), the conversion of the interferent species XO to the non-interferent species XOO is a spontaneous reaction when the bond energy of X−O bond is higher than that of O−O bond. Therefore, it is easier to generate ions of XOO species when there is adequate O2 present in the ion source, so as to eliminate XO interference. Based on these results, experiments were carried out to determine elements of Rb, Nb, Mo, Cs, Ta, W and U. The matrix simulated solutions containing high concentration of Mo, Nb, Ta, and W were used to evaluate the methodological parameters for the measurement of trace Cd, Ag, Au, and Hg impurities, respectively. The limit of detection (LOD) of the trance elements is 0.08-0.31 μg/g, the relative standard deviation (RSD) of the measurement is 2.3%-3.1% (n=6), and the spiked recovery is in the range of 98%-103%. The reliability of the method was further verified by certified superalloy reference materials. Finally, the trace impurities in three types of superalloy samples were measured. The results indicated that the proposed method can achieve rapid, reliable analysis with low detection limit. Besides, it can meet the measurement requirement of trace impurities when the main elements of Mo, Nb, Ta and W exist in superalloy.

     

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