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Automated On-Line Isotope Dilution Analysis with ICP-MS Using Sandwich Flow Injection

机译:使用夹心流动注射的ICP-MS自动进行在线同位素稀释分析

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An automated flow injection (FI) manifold is described to perform the addition of isotopic spikes to aqueous samples on-line with ICP-MS for isotope dilution (ID) analysis. The manifold uses the sandwich technique (with the nested loop approach) to perform an injection of the isotopic spike solution within a sample (or standard) plug, the resulting sample-spike-sample sequence being pushed toward the nebulizer by a 1% HNO↓(3) carrier. A standard, which must contain one element not present in the spike solution to allow the determination of the dispersion coefficient, must also be used to allow a reverse isotope dilution analysis, as well as corrections for mass discrimination and/or spectroscopic interferences. Indeed, because the signals from the individual isotopes are monitored continuously, only one isotope free of spectroscopic interference is required for elements whose isotopic distribution does not vary in nature (two isotopes are still needed for the other elements), as a correction for the interference can be made by comparison with the signals from the standard. Furthermore, this automated approach makes ID-ICP-MS a faster method and does not require any pre preliminary analysis of the sample because the concentration profile resulting from FI allows the selection of the best isotopic ratio. It was successfully applied to the determination of Mo in saline water.
机译:描述了一种自动流动进样(FI)歧管,该方法通过ICP-MS在线对含水样品进行同位素加标,以进行同位素稀释(ID)分析。歧管使用三明治技术(采用嵌套循环法)在样品(或标准)塞子中注入同位素加标溶液,所得样品加标样品序列被1%HNO推向雾化器↓ (3)载体。还必须使用一种标准品,该标准品必须包含加标溶液中不存在的一种元素,才能确定弥散系数,还必须使用该标准品,以进行反向同位素稀释分析以及校正质量歧视和/或光谱干扰。确实,由于连续监测来自各个同位素的信号,因此对于同位素分布本质上没有变化的元素,仅需要一个不受光谱干扰的同位素(其他元素仍需要两个同位素),作为对干扰的校正。通过与标准信号进行比较可以得出。此外,这种自动方法使ID-ICP-MS成为一种更快的方法,并且不需要对样品进行任何预先的初步分析,因为FI产生的浓度曲线允许选择最佳同位素比。它已成功地用于测定盐水中的Mo。

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