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
1. 安捷伦科技(中国)有限公司, 北京 100102; |
2. 湖北省地质实验测试中心, 湖北 武汉 430022; |
3. 中国科学院南京土壤研究所, 江苏 南京 210000 |
Determination of Cadmium in Soil Samples by ICP-MS/MS Using Oxygen Reaction Mode
1. Agilent Technologies(China) Co., LTD, Beijing 100102, China; |
2. Hubei Geological Research Laboratory, Wuhan 430022, China; |
3. Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210000, China |
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，导致土壤中镉的准确测定难度较大。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、1000 μg/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方法使用。
Determination of Cadmium in Soil Samples by ICP-MS/MS Using Oxygen Reaction Mode
ABSTRACT BACKGROUND: When 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.
OBJECTIVES: To develop a method for accurate determination of Cd in soil samples.
METHODS: ICP-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 111ZrOH+, 111MoO+, inducing electron transfer, dehydrogenation, oxygenation and other reactions to inhibit the overlapping interference of these polyatomic ions on 111Cd+.
RESULTS: Oxygen 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%.
CONCLUSIONS: Triple 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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