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Prenormative verification and validation of a protocol for measuring magnetite–maghemite ratios in magnetic nanoparticles
Journal article   Open access   Peer reviewed

Prenormative verification and validation of a protocol for measuring magnetite–maghemite ratios in magnetic nanoparticles

Lara K Bogart, Jeppe Fock, Geraldo M da Costa, Kerstin Witte, Jean-Marc Greneche, Jan Zukrowski, Marcin Sikora, Drew E Latta, Michelle M Scherer, Mikkel Fougt Hansen, …
Metrologia, Vol.59(1), p.15001
12/03/2021
DOI: 10.1088/1681-7575/ac36b6
url
https://doi.org/10.1088/1681-7575/ac36b6View
Published (Version of record) Open Access

Abstract

An important step in establishing any new metrological method is a prenormative interlaboratory study, designed to verify and validate the method against its stated aims. Here, the 57Fe Mössbauer spectrometric 'centre of gravity' (COG) method was tested as a means of quantifying the magnetite/maghemite (Fe3O4/γ-Fe2O3) composition ratio in biphasic magnetic nanoparticles. The study involved seven laboratories across Europe and North and South America, and six samples—a verification set of three microcrystalline mixtures of known composition, and a validation set of three nanoparticle samples of unknown composition. The spectra were analysed by each participant using in-house fitting packages, and ex post facto by a single operator using an independent package. Repeatability analysis was performed using Mandel's h statistic and modified Youden plots. It is shown that almost all (83/84) of the Mandel h statistic values fall within the 0.5% significance level, with the one exception being borderline. Youden-based pairwise analysis indicates the dominance of random uncertainties; and in almost all cases the data analysis phase is only a minor contributor to the overall measurement uncertainty. It is concluded that the COG method is a robust and promising candidate for its intended purpose.
Fe Mössbauer spectrometry iron oxide magnetic nanoparticles magnetite/maghemite

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