Validation of dynamic light scattering and centrifugal liquid sedimentation methods for nanoparticle characterisation

Adelina, Braun; Olivier, Couteau; Franks, Katrin; Kestens, Vikram; Roebben, Gert; Lamberty, A.; Linsinger, Thomas P. J.

doi:10.1016/j.apt.2010.11.001

Cited by 70 publications

(60 citation statements)

References 5 publications

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“…2,3,17,[26][27][28][29][30][31] Thus here only the information helping to understand the derived relationships between ESD's and MED's will be given.…”

Section: Introductionmentioning

confidence: 99%

A uniform measurement expression for cross method comparison of nanoparticle aggregate size distributions

Dudkiewicz

Wagner

Lehner

et al. 2015

Analyst

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Available measurement methods for nanomaterials are based on very different measurement principles and hence produce different values when used on aggregated nanoparticle dispersions. This paper provides a solution for relating measurements of nanomaterials comprised of nanoparticle aggregates determined by different techniques using a uniform expression of a mass equivalent diameter (MED). The obtained solution is used to transform into MED the size distributions of the same sample of synthetic amorphous silica (nanomaterial comprising aggregated nanoparticles) measured by six different techniques: scanning electron microscopy in both high vacuum (SEM) and liquid cell setup (Wet-SEM); gas-phase electrophoretic mobility molecular analyzer (GEMMA); centrifugal liquid sedimentation (CLS); nanoparticle tracking analysis (NTA); and asymmetric flow field flow fractionation with inductively coupled plasma mass spectrometry detection (AF4-ICP-MS). Transformed size distributions are then compared between the methods and conclusions drawn on methods' measurement accuracy, limits of detection and quantification related to the synthetic amorphous silca's size. Two out of the six tested methods (GEMMA and AF4-ICP-MS) cross validate the MED distributions between each other, providing a true measurement. The measurement accuracy of other four techniques is shown to be compromised either by the high limit of detection and quantification (CLS, NTA, Wet-SEM) or the sample preparation that is biased by increased retention of smaller nanomaterials (SEM). This study thereby presents a successful and conclusive cross-method comparison of size distribution measurements of aggregated nanomaterials. The authors recommend the uniform MED size expression for application in nanomaterial risk assessment studies and clarifications in current regulations and definitions concerning nanomaterials.

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“…2,3,17,[26][27][28][29][30][31] Thus here only the information helping to understand the derived relationships between ESD's and MED's will be given.…”

Section: Introductionmentioning

confidence: 99%

A uniform measurement expression for cross method comparison of nanoparticle aggregate size distributions

Dudkiewicz

Wagner

Lehner

et al. 2015

Analyst

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“…There are a wide variety of analytical methods for particle size measurements, including electron microscopy, dynamic light scattering [6], centrifugal liquid sedimentation, small-angle x-ray scattering, field flow fractionation, particle tracking analysis, atomic force microscopy [7] and x-ray diffraction [8]. These methods are based on different measurands, and a comparison between methods should be made with care.…”

Section: Introductionmentioning

confidence: 99%

Particle size distributions by transmission electron microscopy: an interlaboratory comparison case study

Rice¹,

Chan²,

Brown³

et al. 2013

Metrologia

132

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This paper reports an interlaboratory comparison that evaluated a protocol for measuring and analysing the particle size distribution of discrete, metallic, spheroidal nanoparticles using transmission electron microscopy (TEM). The study was focused on automated image capture and automated particle analysis. NIST RM8012 gold nanoparticles (30 nm nominal diameter) were measured for area-equivalent diameter distributions by eight laboratories. Statistical analysis was used to (1) assess the data quality without using size distribution reference models, (2) determine reference model parameters for different size distribution reference models and non-linear regression fitting methods and (3) assess the measurement uncertainty of a size distribution parameter by using its coefficient of variation. The interlaboratory area-equivalent diameter mean, 27.6 nm ± 2.4 nm (computed based on a normal distribution), was quite similar to the area-equivalent diameter, 27.6 nm, assigned to NIST RM8012. The lognormal reference model was the preferred choice for these particle size distributions as, for all laboratories, its parameters had lower relative standard errors (RSEs) than the other size distribution reference models tested (normal, Weibull and Rosin–Rammler–Bennett). The RSEs for the fitted standard deviations were two orders of magnitude higher than those for the fitted means, suggesting that most of the parameter estimate errors were associated with estimating the breadth of the distributions. The coefficients of variation for the interlaboratory statistics also confirmed the lognormal reference model as the preferred choice. From quasi-linear plots, the typical range for good fits between the model and cumulative number-based distributions was 1.9 fitted standard deviations less than the mean to 2.3 fitted standard deviations above the mean. Automated image capture, automated particle analysis and statistical evaluation of the data and fitting coefficients provide a framework for assessing nanoparticle size distributions using TEM for image acquisition.

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“…81 An example is the validation of CLS and DLS for characterization of spherical NMs in pristine dispersions. 82 Method uncertainty regarding the size characterization of NMs has however been discussed, mainly relating to the reference materials of NMs in pristine dispersions, 36,83e85 although recently a study on reference material of synthetic amorphous silica in tomato soup has also been published. 29 …”

Section: Quality Assurance and Controlmentioning

confidence: 99%

Case Study – Characterization of Nanomaterials in Food Products

Tiede

Dudkiewicz

Boxall

et al. 2015

Characterization of Nanomaterials in Complex Environmental and Biological Media

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Validation of dynamic light scattering and centrifugal liquid sedimentation methods for nanoparticle characterisation

Cited by 70 publications

References 5 publications

A uniform measurement expression for cross method comparison of nanoparticle aggregate size distributions

A uniform measurement expression for cross method comparison of nanoparticle aggregate size distributions

Particle size distributions by transmission electron microscopy: an interlaboratory comparison case study

Case Study – Characterization of Nanomaterials in Food Products

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