Abstract

AbstractAnalytical centrifugation (AC) has recently shown great potential for the accurate determination of particle size distributions. The well‐established LUMiSizer(R) is customized by a new design allowing for higher rotor speeds, improved thermal insulation, and measurement cell assembly. The latter enables sedimentation analysis of nanoparticles (NPs) in sector‐shaped centerpieces. The measurement window of AC experiments is assessed by the Peclet (Pe) number. It is shown that at low Pe numbers (0.7 < Pe < 30), sedimentation, and diffusion can be accurately and simultaneously analyzed from the sedimentation boundaries within one experiment. Moreover, sedimentation properties can be reliably determined up to Pe numbers of 4000. The thermal characteristic throughout the sedimentation analysis is validated by measuring polystyrene particles at elevated temperatures. Moreover, the performance of the setup is demonstrated by determining the sedimentation properties of SiO2 NPs at intermediate Pe numbers in excellent agreement with results from analytical ultracentrifugation experiments. Finally, for the first time, an accurate analysis of the core–shell properties of Au NPs via AC is presented. By combining the analysis of sedimentation and diffusional properties at low Pe numbers, the shell thickness of the stabilizer cetyltrimethylammonium bromide alongside the core diameter distribution of the Au NPs is determined.

Highlights

  • LUMiSizer(R) is customized by a new design allowing for higher rotor speeds, improved thermal insulation, and measurement cell assembly

  • Evaluation of Measurement Range of analytical centrifugation (AC) Based on the Pe Number

  • The most common operation mode for AC represents Sedimentation velocity (SV) experiments, where the evolution of the concentration profile is monitored over space and time

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Summary

Commercial SiO2 NPs

Spherical SiO2 NP dispersions of various sizes (nominal dia­ meters of 200, 300, and 500 nm) were obtained from Micromod. GmbH (Germany) at a particle concentration of 50 mg mL–1. The particle dispersions were diluted with ultrapure water (18.2 MΩ cm). The effective particle density of the particles is 1.8 g cm–3 as provided from the supplier, and the solvent properties are equal to the properties of water.[30]. Www.particle-journal.com spun at up to 5300 rpm with this instrument. The rotor speed was varied such that all NP systems sedimented within 2 h

Commercial Polystyrene Particles
Synthesis of Au NPs
AC with Sector-Shaped Cells
Analytical Ultracentrifugation
BD Simulations
Evaluation of Measurement Range of AC Based on the Pe Number
Development of Sector-Shaped Cells for AC
Reduction of Layering Effects in Sedimenting Particle Suspension
Evaluation of Measurement Range for Bimodal PSD
Size and Effective Density Determination of Core–Shell Au NPs by AC
Conflict of Interest
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