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Impact of pump flow fluctuations on post column online ID-ICP-MS

机译:泵流量波动对柱后在线ID-ICP-MS的影响

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摘要

In post column online isotope dilution mass spectrometry (IDMS), the stability of the spike mass flow is a key element. Changes in viscosity or fluctuations in the pump rate of the peristaltic pump may affect the results of post column online IDMS measurements. It was shown by simulating random fluctuations and studying the changes in the resulting integrals of the isotope ratio chromatogram of the sample that even small fluctuations, observable when using peristaltic pumps, can influence the result and especially its uncertainty. The use of a balance to continuously monitor the mass flow of the spike during the measurement which we presented in a previous publication allows now to correct the isotope ratio chromatogram for these fluctuations. Subsequently, the simulated effect was verified experimentally for the determination of Se-Met in the human serum reference material BCR 637, where the corrected mass fraction was plainly closer to the mass fraction obtained by species specific IDMS. Additional attention was paid to the fact that there is a time shift between the observation of the fluctuations in the pump rate and the detection of these fluctuations in the ICP-MS.
机译:在柱后在线同位素稀释质谱法(IDMS)中,加标质量流量的稳定性是关键要素。粘度变化或蠕动泵的泵速波动可能会影响柱后在线IDMS测量结果。通过模拟随机波动并研究样品的同位素比色谱图所得积分的变化表明,使用蠕动泵时即使观察到很小的波动也会影响结果,尤其是不确定性。在以前的出版物中介绍的测量过程中,使用天平连续监控尖峰的质量流量,现在可以校正这些波动的同位素比色谱图。随后,通过实验验证了模拟效果,用于测定人血清参考物质BCR 637中的Se-Met,校正后的质量分数显然接近于通过物种特异性IDMS获得的质量分数。还要特别注意以下事实:在观察泵速波动和在ICP-MS中检测这些波动之间存在时间偏移。

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