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Size measurement uncertainties of near-monodisperse, nearspherical nanoparticles using transmission electron microscopy and particle-tracking analysis

机译:透射电子显微镜和颗粒跟踪分析法测量近单分散,近球形纳米颗粒的尺寸不确定度

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摘要

Particle-tracking analysis (PTA) in combination with systematic imaging, automatic image analysis, and automatic data processing is validated for size measurements. Transmission electron microscopy (TEM) in combination with a systematic selection procedure for unbiased random image collection, semiautomatic image analysis, and data processing is validated for size, shape, and surface topology measurements. PTA is investigated as an alternative for TEM for the determination of the particle size in the framework of the EC definition of nanomaterial. The intra-laboratory validation study assessing the precision and accuracy of the TEMand PTA methods consists of series of measurements on three gold reference materials with mean area-equivalent circular diameters of 8.9 nm (RM-8011), 27.6 nm (RM-8012), and 56.0 nm (RM- 8013), and two polystyrene materials with modal hydrodynamic diameters of 102 nm (P1) and 202 nm (H1). By obtaining a high level of automation, PTA proves to give precise and non-biased results for the modal hydrodynamic diameter in size range between 30 and 200 nm, and TEM proves to give precise and non-biased results for the mean area-equivalent circular diameter in the size range between 8 and 200 nm of the investigated near-monomodal near-spherical materials. The expanded uncertainties of PTA are about 9 % and are determined mainly by the repeatability uncertainty. This uncertainty is two times higher than the expanded uncertainty of 4 % obtained by TEM for analyses on identical materials. For the investigated near-monomodal and near-spherical materials, PTA can be used as an alternative to TEM for measuring the particle size, with exception of 8.9 nm gold, because this material has a size below the detection limit of PTA.
机译:结合系统成像,自动图像分析和自动数据处理的粒子跟踪分析(PTA)已通过尺寸测量验证。透射电子显微镜(TEM)结合用于无偏随机图像收集,半自动图像分析和数据处理的系统选择程序,已针对尺寸,形状和表面拓扑测量进行了验证。研究了PTA作为TEM的替代方法,用于在EC纳米材料定义的框架内确定粒径。评估TEM和PTA方法的精密度和准确性的实验室内部验证研究包括对三种金参考材料的一系列测量,这些材料的平均面积当量圆直径为8.9 nm(RM-8011),27.6 nm(RM-8012),和56.0 nm(RM- 8013),以及两种模态流体力学直径分别为102 nm(P1)和202 nm(H1)的聚苯乙烯材料。通过获得高度的自动化,PTA证明了在30至200 nm尺寸范围内的模态流体动力直径可提供精确且无偏差的结果,而TEM证明可为平均面积当量圆提供精确且无偏差的结果研究的近单峰近球形材料的直径在8到200 nm之间。 PTA的扩展不确定度约为9%,主要由重复性不确定度决定。此不确定度比通过TEM在相同材料上进行分析获得的4%的扩展不确定度高两倍。对于研究的接近单峰和接近球形的材料,PTA可以替代TEM来测量粒径,但金8.9 nm除外,因为该材料的尺寸低于PTA的检测极限。

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