Laboratory of Analytical Chemistry, EMPA-Swiss Federal Laboratories for Materials Testing and Research, Duebendorf, Switzerland.
Anal Chem. 2012 Mar 20;84(6):2678-85. doi: 10.1021/ac202641d. Epub 2012 Feb 29.
Due to the already prevalent and increasing use of silver-nanoparticle (Ag-NP) products and the raised concerns in particular for the aquatic environment, analytical techniques for the characterization of such products are of need. However, because Ag-NP products are of different compositions and polydispersities, analysis especially of the size distribution is challenging. In this work, an asymmetric flow field flow fractionation (A4F) multidetector system (UV/vis, light scattering, inductively coupled plasma mass spectrometry - ICPMS), in combination with a method to distinguish and quantify the particle and dissolved Ag fractions (ICPMS after ultracentrifugation), for the characterization of Ag-NP products with different degrees of polydispersities is presented. For validation and to outline benefits and limitations, results obtained from batch dynamic light scattering (batch-DLS) and transmission electron microscopy (TEM) were compared. With the developed method a comprehensive understanding in terms of dissolved Ag and Ag-NP concentration as well as an element selective, mass- and number particle size distribution (PSD) was obtained. In relation to batch-DLS, the reliability of the data was improved significantly. In comparison to TEM, faster measurement times and the ability to determine the samples directly in dispersions are clearly advantageous. The proposed setup shows potential for a rapid- and reliable characterization method of virtually any polydisperse metallic NP dispersion, many of them available on the market already.
由于银纳米颗粒(Ag-NP)产品的广泛应用和日益增加,特别是对水生环境的担忧,因此需要对这些产品进行分析。然而,由于 Ag-NP 产品的组成和多分散性不同,分析特别是大小分布具有挑战性。在这项工作中,我们提出了一种不对称流场流分离(A4F)多检测器系统(UV/vis、光散射、电感耦合等离子体质谱法 - ICPMS),结合一种区分和定量颗粒和溶解 Ag 部分的方法(超离心后的 ICPMS),用于不同多分散性程度的 Ag-NP 产品的表征。为了验证并概述优点和局限性,我们比较了批量动态光散射(batch-DLS)和透射电子显微镜(TEM)的结果。使用所开发的方法,我们获得了关于溶解 Ag 和 Ag-NP 浓度以及元素选择性、质量和数量颗粒大小分布(PSD)的全面理解。与 batch-DLS 相比,数据的可靠性显著提高。与 TEM 相比,更快的测量时间和直接在分散体中确定样品的能力显然具有优势。所提出的设置显示出对几乎任何多分散金属 NP 分散体进行快速可靠表征的潜力,其中许多已经在市场上销售。