Nanoparticle Size Distribution Quantification: Results of a SAXS Inter-Laboratory Comparison

TL;DR

This study compares nanoparticle sizing results from multiple laboratories worldwide using SAXS, demonstrating its reliability and consistency in determining size distributions of sub-20 nm particles across various instruments.

Contribution

First comprehensive inter-laboratory comparison of SAXS for nanoparticle size distribution quantification, highlighting method robustness and potential biases.

Findings

Consistent mean radii around 2.76 nm and 3.20 nm from different methods.

Particle concentration determined as 3.00 ± 0.38 g/L.

High-quality data obtained across diverse instruments.

Abstract

We present the first world-wide inter-laboratory comparison of small-angle X-ray scattering (SAXS) for nanoparticle sizing. The measurands in this comparison are the mean particle radius, the width of the size distribution and the particle concentration. The investigated sample consists of dispersed silver nanoparticles, surrounded by a stabilizing polymeric shell of poly(acrylic acid). The silver cores dominate the X-ray scattering pattern, leading to the determination of their radii size distribution using: i) Glatter's Indirect Fourier Transformation method, ii) classical model fitting using SASfit and iii) a Monte Carlo fitting approach using McSAS. The application of these three methods to the collected datasets produces consistent mean number- and volume-weighted core radii of R$_n$ = 2.76 nm and R$_v$ = 3.20 nm, respectively. The corresponding widths of the log-normal radii distribution of the particles were $\sigma_n$ = 0.65 nm and $\sigma_v$ = 0.71 nm. The particle concentration determined using this method was 3.00 $\pm$ 0.38 g/L (4.20 $\pm$ 0.73 $\times$ 10$^{-6}$ mol/L). We show that the results are slightly biased by the choice of data evaluation procedure, but that no substantial differences were found between the results from data measured on a very wide range of instruments: the participating laboratories at synchrotron SAXS beamlines, commercial and home-made instruments were all able to provide data of high quality. Our results demonstrate that SAXS is a qualified method for revealing particle size distributions in the sub-20 nm region (at least), out of reach for most other analytical methods.