陈胜利，朱秀芹

中国石油大学（北京）化学工程与环境学院，北京 102249；北京纳微标物科技有限公司，北京 102200

引用格式：

陈胜利，朱秀芹. 动态光散射测量仪粒度标准物质的研制［J］. 中国粉体技术，2024，30（5）：121-131.

CHEN S L， ZHU X Q. Development of particle size standard materials for dynamic light scattering measuring instruments［J］.China Powder Science and Technology，2024，30（5）：121−131.

DOI：10.13732/j.issn.1008-5548.2024.05.012

收稿日期：2024-06-01，修回日期：2024-06-25，上线日期：2024-08-27。

基金项目：国家自然科学基金项目，编号 ：2021YFA1501200。

第一作者简介：陈胜利（1962—），男，教授，博士，博士生导师，研究方向为颗粒体系、石油加工、催化剂及催化反应、标准化。E-mail：slchen@cup. edu. cn。

摘要：【目的】 为了解决我国尚缺动态光散射测量法专用粒度标准物质这一问题。【方法】 采用微乳液聚合法合成标称粒径为40、80 nm的态光散射粒度标准物质，标准物质编号分别是QBW12001和GBW12011b；采用动态光散射多家定值法测定2种粒度标准物质的散射光强调和平均粒径，定值结果溯源至动态光散射法（ISO 22412：2017）。【结果】 合成的2种粒度标准物质均匀且稳定，散射光强调和平均粒径分别为40. 0±0. 5 nm和80±2 nm。不同厂家生产的激光粒度仪测的散射光强度调和平均粒径一致性最好；散射光强度平均粒径一致性较好；体积平均粒径一致性较差；颗粒数目平均粒径一致性最差。同一台仪器测定的平均粒径的重复性好坏顺序一致。

关键词：布粒度；标准物质；聚苯乙烯乳液；动态光散射

Abstract

Objective As there is currently no dedicated particle size standard material for dynamic light scattering （DLS） measurement in China， manufacturers and users of particle size analyzers in China primarily rely on standard materials produced by Thermo Fisher Scientific. The study aims to develop particle size standard materials for dynamic light scattering particle size analyzers.

Methods In this study， dynamic light scattering particle size standard materials with nominal particle sizes of 40 nm and 80 nm were synthesized using microemulsion polymerization. A total of 12 institutes used 14 dynamic light scattering particle size analyzers from different manufacturers to determine the particle size values of the developed standard materials.

Results and Discussion The study results showed that the two synthesized polystyrene microspheres exhibited good sphericity and uniform particle size， with stable and homogeneous sample quality. The harmonic mean particle sizes based on scattering light intensity were 40. 0±0. 5 nm and 80±2 nm， respectively. The measurement uncertainties of the assigned values were comparable to those of similar particle size standard materials from the European Community Bureau of Reference and Thermo Fisher Scientific. Among the dynamic light scattering particle size analyzers produced by different manufacturers， the harmonic mean particle sizes based on scattering light intensity showed the best consistency， the mean particle sizes based on scattering light intensity were relatively consistent， the volume-based mean particle sizes showed less consistency， and the number-based mean particle sizes had the poorest consistency. The repeatability of different mean particle sizes measured by the same instrument followed the same order.

Conclusion Two types of dynamic light scattering polystyrene microsphere particle size standard materials， with sizes of 40 nm and 80 nm， were developed. These standard materials exhibit good sphericity， uniform particle size， and stable sample quality.The harmonic mean particle sizes based on scattering light intensity for these two standard materials were determined to be 40. 0±0. 5 nm and 80±2 nm， respectively， with results traceable to the dynamic light scattering method （ISO 22412：2017）. Among the dynamic light scattering particle size analyzers produced by different manufacturers， the harmonic mean particle sizes based on scattering light intensity showed the best consistency， the mean particle sizes based on scattering light intensity were relatively consistent， the volume-based mean particle sizes showed less consistency， and the number-based mean particle sizes had the poorest consistency.

Keywords：polydispersity； standard materials； polystyrene emulsion； dynamic light scattering

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