4.7 Article

A new certified reference material for size and shape analysis of nanorods using electron microscopy

Journal

ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 413, Issue 1, Pages 141-157

Publisher

SPRINGER HEIDELBERG
DOI: 10.1007/s00216-020-02984-z

Keywords

Certified reference material; Electron microscopy; Nanorods; Particle shape; Particle size; Titanium dioxide

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A new certified reference material for size and shape analysis of elongated nanoparticles has been developed by the European Commission's Joint Research Centre. The certified values, traceable to the unit of length in the International System of Units, range from 4 to 6% relative expanded uncertainties and can be used for quality assurance and calibration of electron microscopy methods for nanoparticle size and shape analysis, relevant for EU legislation related to nanomaterials.
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 degrees 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-for-purpose CRM. Graphical abstract

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