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氧气反应模式-电感耦合等离子体串联质谱法测定土壤中的镉

Determination of Cadmium in Soil Samples by ICP-MS/MS Using Oxygen Reaction Mode

  • 摘要: 应用电感耦合等离子体质谱法(ICP-MS)分析土壤中的镉元素时,锆的氢氧化物、钼的氧化物、锡的同位素会对镉造成严重的干扰,导致准确测定土壤中镉的难度较大。本文采用电感耦合等离子体串接质谱法(ICP-MS/MS),选取无同质异位素干扰的111Cd为分析谱线,在MS/MS模式下碰撞反应池中通入的氧气可以与94Zr16O1H+95Mo16O+进行电子转移、去氢、加氧等反应,抑制这些多原子离子对111Cd的重叠干扰。结果表明:氧气流量越大,去除多原子离子的效果越好,当氧气流量在0.45mL/min时,溶液中2000μg/L以下的锆、1000μg/L以下的钼在111Cd处形成的多原子重叠干扰小于0.005μg/L。实验在石墨消解仪中采用氢氟酸-硝酸-高氯酸消解样品,盐酸复溶,溶液定容稀释至1000倍测定,方法检出限(3δ)达到0.003μg/g;本方法经过国家土壤一级标准物质验证,11个国家土壤一级标准物质的测量值和认定值的相对误差在±7%以内,3个国家土壤一级标准物质的精密度(RSD,n=12)小于5%。本方法可以作为土壤样品中痕量镉元素的分析方法。

     

    Abstract:
    BACKGROUNDWhen using inductively coupled plasma-mass spectrometry (ICP-MS) to analyze soil, the zirconium hydroxide, molybdenum oxide, and tin isotopes can cause serious interference on cadmium, which makes it difficult to accurately determine cadmium in soil samples.
    OBJECTIVESTo develop a method for accurate determination of Cd in soil samples.
    METHODSICP-MS/MS was used, and 111Cd without isobaric interference was selected as the analysis line. In MS/MS mode, the oxygen introduced into the collision reaction cell can be reacted with 111Zr16O1H+, 111Mo16O+, inducing electron transfer, dehydrogenation, oxygenation and other reactions to inhibit the overlapping interference of these polyatomic ions on 111Cd.
    RESULTSOxygen flow was the key factor in this method. 0.45mL/min oxygen flow can reduce oxide interference to less than 0.005μg/L when zirconium concentration was lower than 2000μg/L and molybdenum concentration was below 1000μg/L. The method has been verified by the national reference materials. The relative error of the measured value and recognized value of the 11 national reference materials was within ±7%, and the relative standard deviation (n=12) of three soil reference materials was less than 5%.
    CONCLUSIONSTriple quadrupole ICP-MS oxygen reaction mode can eliminate Zr and Mo polyatomic ion interference on Cd, and this method can be used for the determination of trace Cd in soil samples.

     

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