关键方法检测、大小和量化纳米银的关键方法的关键性实验评估。
Critical experimental evaluation of key methods to detect, size and quantify nanoparticulate silver.
机构信息
Institute for Health and Consumer Protection, Joint Research Centre, European Commission , Via E. Fermi 2749, 21027 Ispra (VA), Italy.
出版信息
Anal Chem. 2014 Dec 16;86(24):12143-51. doi: 10.1021/ac503307r. Epub 2014 Nov 25.
Different analytical techniques, sedimentation flow field fractionation (SdFFF), asymmetrical flow field flow fractionation (AF4), centrifugal liquid sedimentation (CLS) and dynamic light scattering (DLS) have been used to give complementary size information about suspensions of silver nanoparticles (AgNPs) in the size range of 20-100 nm by taking advantage of the different physical principles on which are based. Particle morphology was controlled by TEM (Transmission Electron Microscopy). Both SdFFF and AF4 were able to accurately size all AgNPs; among sedimentation based techniques, CLS underestimated the average sizes of larger samples (70 and 100 nm), but it produced the best separation of bimodal mixtures Ag40/60 and Ag40/70 mix compared to SdFFF. On the contrary, DLS overestimated the average sizes of the smallest samples (20 and 30 nm) and it was unable to deal with bimodal mixtures. Quantitative mass and number particle size distributions were also calculated starting from UV-vis signals and ICP-MS data and the results evaluated as a means to address the issue of determining nanoparticle size distributions as required for implementation of European regulations relating to labeling of nanomaterials in consumer products. The results are discussed in light of possible particle aggregation state, analysis repeatability, size resolution and quantitative recoveries.
不同的分析技术,如沉降流场分级(SdFFF)、不对称流场流分级(AF4)、离心液体沉降(CLS)和动态光散射(DLS),已经被用于通过利用不同的物理原理来提供关于银纳米粒子(AgNPs)悬浮液的尺寸信息,这些原理的尺寸范围为 20-100nm。颗粒形态由透射电子显微镜(TEM)控制。SdFFF 和 AF4 都能够准确地对所有 AgNPs 进行尺寸分析;在基于沉降的技术中,CLS 低估了较大样品(70nm 和 100nm)的平均尺寸,但与 SdFFF 相比,它能够更好地分离双峰混合物 Ag40/60 和 Ag40/70 混合物。相反,DLS 高估了最小样品(20nm 和 30nm)的平均尺寸,并且无法处理双峰混合物。还可以从 UV-vis 信号和 ICP-MS 数据计算质量和数量的粒径分布,并将结果评估为确定纳米粒子尺寸分布的一种手段,这是实施与消费品中纳米材料标签相关的欧洲法规所必需的。根据可能的颗粒聚集状态、分析重复性、尺寸分辨率和定量回收率讨论了结果。