Reproducibility of methods required to identify and characterize nanoforms of substances

Author(s)
Richard K Cross, Nathan Bossa, Björn Stolpe, Frédéric Loosli, Nicklas Mønster Sahlgren, Per Axel Clausen, Camilla Delpivo, Michael Persson, Andrea Valsesia, Jessica Ponti, Dora Mehn, Didem Ag Seleci, Philipp Müller, Frank von der Kammer, Hubert Rauscher, Dave Spurgeon, Claus Svendsen, Wendel Wohlleben
Abstract

Nanoforms (NFs) of a substance may be distinguished from one another through differences in their physicochemical properties. When registering nanoforms of a substance for assessment under the EU REACH framework, five basic descriptors are required for their identification: composition, surface chemistry, size, specific surface area and shape. To make the risk assessment of similar NFs efficient, a number of grouping frameworks have been proposed, which often require assessment of similarity on individual physicochemical properties as part of the group justification. Similarity assessment requires an understanding of the achievable accuracy of the available methods. It must be demonstrated that measured differences between NFs are greater than the achievable accuracy of the method, to have confidence that the measured differences are indeed real. To estimate the achievable accuracy of a method, we assess the reproducibility of six analytical techniques routinely used to measure these five basic descriptors of nanoforms: inductively coupled plasma mass spectrometry (ICP-MS), Thermogravimetric analysis (TGA), Electrophoretic light scattering (ELS), Brunauer-Emmett-Teller (BET) specific surface area and transmission and scanning electron microscopy (TEM and SEM). Assessment was performed on representative test materials to evaluate the reproducibility of methods on single NFs of substances. The achievable accuracy was defined as the relative standard deviation of reproducibility (RSDR) for each method. Well established methods such as ICP-MS quantification of metal impurities, BET measurements of specific surface area, TEM and SEM for size and shape and ELS for surface potential and isoelectric point, all performed well, with low RSDR, generally between 5 and 20%, with maximal fold differences usually <1.5 fold between laboratories. Applications of technologies such as TGA for measuring water content and putative organic impurities, additives or surface treatments (through loss on ignition), which have a lower technology readiness level, demonstrated poorer reproducibility, but still within 5-fold differences. The expected achievable accuracy of ICP-MS may be estimated for untested analytes using established relationships between concentration and reproducibility, but this is not yet the case for TGA measurements of loss on ignition or water content. The results here demonstrate an approach to estimate the achievable accuracy of a method that should be employed when interpreting differences between NFs on individual physicochemical properties.

Organisation(s)
Department of Environmental Geosciences
External organisation(s)
LEITAT Technological Center, Carrer de la Innovació 2, 08225 Terrassa, Barcelona, Spain., Nouryon, Bohus, Sweden., The National Research Centre for the Working Environment (NFA), Lersø Parkallé 105, 2100 Copenhagen East, Denmark., Institute for Environment and Sustainability , BASF SE, Centre for Ecology and Hydrology
Journal
NanoImpact
Volume
27
No. of pages
15
ISSN
2452-0748
DOI
https://doi.org/10.1016/j.impact.2022.100410
Publication date
07-2022
Peer reviewed
Yes
Austrian Fields of Science 2012
105906 Environmental geosciences
Keywords
ASJC Scopus subject areas
Public Health, Environmental and Occupational Health, Safety, Risk, Reliability and Quality, Safety Research, Materials Science (miscellaneous)
Portal url
https://ucrisportal.univie.ac.at/en/publications/36f32123-23fc-4b20-af37-7b8d8afe6d5b