Chemical Sciences Division and ‡Materials Measurement Science Division, Material Measurement Laboratory, National Institute of Standards and Technology , Gaithersburg, Maryland 20899, United States.
Anal Chem. 2014 Apr 1;86(7):3405-14. doi: 10.1021/ac403775a. Epub 2014 Mar 11.
The increasing application of engineered nanomaterials (ENMs) in consumer and medical products has motivated the development of single-particle inductively coupled plasma mass spectrometry (spICP-MS) for characterizing nanoparticles under realistic environmental exposure conditions. Recent studies have established a set of metrological criteria and evaluated the feasibility of spICP-MS for sizing or quantifying various highly commercialized ENMs. However, less is known about the performance of spICP-MS for detecting nanoparticles with sizes greater than 80 nm. This paper presents a systematic study on spICP-MS for accurate size measurement of gold nanoparticles from 10 to 200 nm. We show that dwell time contributes significantly to the quality of data, with the optimal dwell time that limits split particle events, particle coincidences and false positives being 10 ms. A simple approach to correct for split particle events is demonstrated. We show that transient features of single particle events can be temporally resolved on a conventional quadrupole ICP-MS system using a sufficiently short dwell time (0.1 ms). We propose an intensity-size diagram for estimating the linear dynamic size range and guiding the selection of ICP-MS operating conditions. The linear dynamic size range of the ICP-MS system under standard (highest) sensitivity conditions is 10 to 70 nm but can be further extended to 200 nm by operating in less sensitive modes. Finally, the ability of spICP-MS to characterize heterogeneous forms of metal containing nanoparticles is evaluated in mixtures containing both dissolved and poly disperse nanoparticulate Au.
工程纳米材料(ENMs)在消费品和医疗产品中的应用不断增加,这促使人们开发了用于在实际环境暴露条件下对纳米颗粒进行表征的单颗粒电感耦合等离子体质谱(spICP-MS)。最近的研究已经建立了一套计量标准,并评估了 spICP-MS 对各种商业化 ENMs 进行尺寸或定量分析的可行性。然而,对于 spICP-MS 检测尺寸大于 80nm 的纳米颗粒的性能知之甚少。本文对 spICP-MS 进行了系统研究,以实现从 10nm 到 200nm 的金纳米颗粒的精确尺寸测量。我们表明,停留时间对数据质量有很大的影响,最佳的停留时间限制了分裂颗粒事件、颗粒重合和假阳性的发生,为 10ms。我们展示了一种简单的方法来校正分裂颗粒事件。我们表明,使用足够短的停留时间(0.1ms),可以在传统的四极电感耦合等离子体质谱系统上对单个颗粒事件的瞬态特征进行时间分辨。我们提出了一种强度-尺寸图来估计线性动态尺寸范围,并指导 ICP-MS 操作条件的选择。在标准(最高)灵敏度条件下,ICP-MS 系统的线性动态尺寸范围为 10nm 至 70nm,但通过在较低灵敏度模式下操作,可以进一步扩展到 200nm。最后,评估了 spICP-MS 在含有溶解态和多分散纳米金的混合物中对含金属纳米颗粒的异质形态进行特征描述的能力。