A new certified reference material for size and shape analysis of nanorods using electron microscopy
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RESEARCH PAPER
A new certified reference material for size and shape analysis of nanorods using electron microscopy Vikram Kestens 1 & Tsvetelina Gerganova 1,2 & Gert Roebben 1,3 & Andrea Held 1 Received: 29 July 2020 / Revised: 25 September 2020 / Accepted: 1 October 2020 # The Author(s) 2020
Abstract A new certified reference material (CRM) for size and shape analysis of elongated nanoparticles has been developed by the European Commission’s Joint Research Centre. The CRM consists of titanium dioxide nanorods dispersed in 1-butanol, was coded ERM-FD103 and has been certified for different electron microscopy–based operationally defined measurands such as the modal and median values of the particle number-weighted distributions of the minimum and maximum Feret diameter, the maximum inscribed circle diameter, the area-equivalent circular diameter and the aspect ratio. The nanorods have nominal dimensions of 15 nm in width and 55 nm in length. Homogeneity and stability measurements were performed using transmission electron microscopy. The relative standard uncertainty for homogeneity ranged from 0.3 to 1.7%. No significant instability was detected for a shelf life of 18 months and a storage temperature of 18 °C. The certified values have been determined from the results of an interlaboratory comparison in which qualified expert laboratories participated with scanning and transmission electron microscopy. The certified values are traceable to the unit of length in the International System of Units, the metre, and the relative expanded uncertainties (confidence level of approximately 95%) range from 4 to 6%. These properties allow the CRM to be used for quality assurance and calibration of electron microscopy methods for nanoparticle size and shape analysis in ranges relevant for the implementation of EU legislation related to nanomaterials. The presented study discusses the purpose and results of the different steps that were followed to turn an industrially relevant raw titanium dioxide nanorod material into a fit-forpurpose CRM. Keywords Certified reference material . Electron microscopy . Nanorods . Particle shape . Particle size . Titanium dioxide
Introduction Nanoparticles, as well as materials containing them, are widely used in many applications and products because of their desirable unique chemical and physical properties. Their increased Electronic supplementary material The online version of this article (https://doi.org/10.1007/s00216-020-02984-z) contains supplementary material, which is available to authorized users. * Vikram Kestens [email protected] 1
European Commission, Joint Research Centre (JRC), 2440 Geel, Belgium
2
Present address: European Commission, EUROSTAT, 2920 Luxembourg, Luxembourg
3
Present address: European Commission, Directorate-General for Internal Market, Industry, Entrepreneurship and SMEs, 1049 Brussels, Belgium
use, and the resulting higher likelihood of exposure, has led to concerns about the potential nano-specific impact [1, 2]. In the European Union (EU),
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