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New Prospects for Particle Characterization Using Analytical Centrifugation with Sector‐Shaped Centerpieces
Particle & Particle Systems Characterization ( IF 2.7 ) Pub Date : 2020-06-11 , DOI: 10.1002/ppsc.202000108
Maximilian J. Uttinger 1 , Sebastian Boldt 2 , Simon E. Wawra 1 , Tobias D. Freiwald 1 , Cornelia Damm 1 , Johannes Walter 1 , Dietmar Lerche 2, 3 , Wolfgang Peukert 1
Affiliation  

Analytical 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.

中文翻译:

使用带扇形中心件的分析离心法进行颗粒表征的新前景

最近,分析离心(AC)在准确确定粒度分布方面显示出巨大潜力。完善的LUMiSizer(R)是通过新设计定制的,可实现更高的转子速度,改进的隔热性能以及测量单元的组装。后者可以对扇形中心件中的纳米颗粒(NPs)进行沉降分析。AC实验的测量窗口由Peclet(Pe)数评估。结果表明,在低的Pe值(0.7 <Pe <30)下,可以在一个实验中从沉积边界准确而同时地分析沉积和扩散。此外,可以可靠地确定高达4000的Pe值的沉积性能。通过在高温下测量聚苯乙烯颗粒,可以验证整个沉降分析的热特性。此外,通过确定SiO的沉降特性证明了装置的性能具有中等Pe数的2个NP与分析超速离心实验的结果非常吻合。最后,这是首次通过交流精确分析了金纳米颗粒的核壳性质。通过结合低Pe值下的沉降和扩散特性分析,确定了稳定剂十六烷基三甲基溴化铵的壳厚度以及Au NPs的核径分布。
更新日期:2020-06-11
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