Rosenkranz Daniel, Kriegel Fabian L, Mavrakis Emmanouil, Pergantis Spiros A, Reichardt Philipp, Tentschert Jutta, Jakubowski Norbert, Laux Peter, Panne Ulrich, Luch Andreas
Department of Chemical and Product Safety, German Federal Institute for Risk Assessment (BfR);
Department of Chemical and Product Safety, German Federal Institute for Risk Assessment (BfR).
J Vis Exp. 2020 Sep 24(163). doi: 10.3791/61653.
Metal-containing nanoparticles (NP) can be characterized with inductively coupled plasma mass spectrometers (ICP-MS) in terms of their size and number concentration by using the single-particle mode of the instrument (spICP-MS). The accuracy of measurement depends on the setup, operational conditions of the instrument and specific parameters that are set by the user. The transport efficiency of the ICP-MS is crucial for the quantification of the NP and usually requires a reference material with homogenous size distribution and a known particle number concentration. Currently, NP reference materials are available for only a few metals and in limited sizes. If particles are characterized without a reference standard, the results of both size and particle number may be biased. Therefore, a dual-inlet setup for characterizing nanoparticles with spICP-MS was developed to overcome this problem. This setup is based on a conventional introduction system consisting of a pneumatic nebulizer (PN) for nanoparticle solutions and a microdroplet generator (µDG) for ionic calibration solutions. A new and flexible interface was developed to facilitate the coupling of µDG, PN and the ICP-MS system. The interface consists of available laboratory components and allows for the calibration, nanoparticle (NP) characterization and cleaning of the arrangement, while the ICP-MS instrument is still running. Three independent analysis modes are available for determining particle size and number concentration. Each mode is based on a different calibration principle. While mode I (counting) and mode III (µDG) are known from the literature, mode II (sensitivity), is used to determine the transport efficiency by inorganic ionic standard solutions only. It is independent of NP reference materials. The µDG based inlet system described here guarantees superior analyte sensitivities and, therefore, lower detection limits (LOD). The size dependent LODs achieved are less than 15 nm for all NP (Au, Ag, CeO2) investigated.
含金属纳米颗粒(NP)可通过电感耦合等离子体质谱仪(ICP-MS),利用该仪器的单颗粒模式(spICP-MS)对其尺寸和数量浓度进行表征。测量的准确性取决于仪器的设置、操作条件以及用户设定的特定参数。ICP-MS的传输效率对于NP的定量分析至关重要,通常需要一种尺寸分布均匀且颗粒数浓度已知的参考物质。目前,仅少数几种金属有NP参考物质,且尺寸有限。如果在没有参考标准的情况下对颗粒进行表征,尺寸和颗粒数的结果可能会有偏差。因此,开发了一种用于用spICP-MS表征纳米颗粒的双进样装置来克服这一问题。该装置基于传统的进样系统,由用于纳米颗粒溶液的气动雾化器(PN)和用于离子校准溶液的微滴发生器(µDG)组成。开发了一种新型灵活接口,以促进µDG、PN和ICP-MS系统的耦合。该接口由现有的实验室组件组成,可在ICP-MS仪器仍在运行时对装置进行校准、纳米颗粒(NP)表征和清洗。有三种独立的分析模式可用于确定颗粒尺寸和数量浓度。每种模式基于不同的校准原理。虽然模式I(计数)和模式III(µDG)在文献中已有报道,但模式II(灵敏度)仅用于通过无机离子标准溶液确定传输效率。它独立于NP参考物质。此处描述的基于µDG的进样系统保证了卓越的分析物灵敏度,因此具有更低的检测限(LOD)。对于所有研究的NP(金、银、二氧化铈),实现的尺寸相关LOD小于15纳米。