陈胜利¹ ，朱秀芹²

收稿日期：2024-06-01，修回日期：2024-06-25，上线日期：2024-10-16。

基金项目：国家重点研发计划资助项目，编号 ：2021YFA1501203。

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】 解决我国激光粒度仪测量上限现状不清楚的问题，研制用于判断激光粒度仪测量上限的毫米级颗粒粒度标准物质。【方法】 利用悬浮聚合再筛分法制备标称粒径为0. 6、0. 8、1. 0、1. 1 mm的聚苯乙烯微珠粒度标准物质；利用经NIST SRM2800测微尺校准的光学显微镜对制得的标准物质进行定值。【结果】 制得的4种粒度标准物质体积中位粒径分别为（0. 553±0. 007）、（0. 749±0. 008）、（0. 925±0. 008）、（1. 07±0. 01）mm；利用制得的粒度标准物质检验了国内外6个公司生产的 7种型号激光粒度仪的测量上限，发现只有部分型号的粒度仪能准确测量毫米级粒度标准物质。【结论】 制得的毫米级粒度标准物质样品均匀、稳定，粒径定值结果溯源至He-Ne激光波长，准确可靠，完善了我国粒度标准物质体系；激光粒度仪测量上限不仅取决于光探测器最内侧单元的半径，还取决于其使用光源的激光质量。

关键词：颗粒粒度；标准物质；聚苯乙烯微珠；激光粒度仪；测量上限

Abstract

Objective To address the unclear measurement upper limits of laser particle size analyzers in China， the study develops millimeter-scale particle size standard materials to evaluate performance of these devices， filling a significant gap in this field.

Methods Polystyrene （PS） microbeads with nominal diameters of 0. 6，0. 8，1. 0， and 1. 1 mm were prepared using suspension polymerization-partial sulfonation-sieving method. These microbeads were designed to serve as particle size standard materials. An optical microscope calibrated with an NIST SRM2800 micrometer was employed to measure the particle sizes of these four standard materials. Their homogeneity and stability were evaluated， and the measurement results were traceable to the wavelength of He-Ne lasers. These millimeter-scale particle size standards were subsequently used to assess several commonly used laser particle size analyzers available on the Chinese market.

Results and Discussion The polystyrene microbeads exhibited excellent sphericity， a narrow particle size distribution， and outstanding homogeneity and stability. The volume median diameters of these samples were（0. 553±0. 007），（0. 749±0. 008），（0. 925±0. 008）， and（1. 07±0. 01） mm， respectively. These measured diameters were accurate， reliable， and traceable to the He-Ne laser wavelength. When tested， only certain particle size analyzers were capable of accurately measuring all four types of millimeter-scale standard materials. Some analyzers could only measure 1-2 sample types accurately， while others failed to measure millimeter-scale particle size standards at all. Analyzers with the smallest measurement deviations were produced by three companies and used He-Ne laser sources， whereas those with larger deviations used more affordable semiconductor laser sources.

Conclusion The four types of millimeter-scale particle size standard materials fill a critical gap in millimeter-scale particle size standards in China and enhance the country’s overall particle size standard system. To evaluate the measurement upper limits of laser particle size analyzers， multiple reference samples are required. The measurement upper limit of an analyzer is influenced not only by the radius of the innermost unit of the light-receiving detector （i.e.，the minimum receiving angle） but also by the quality of the laser light source used. Higher laser quality is associated with a higher measurement upper limit for the particle size analyzer. Analyzers equipped with He-Ne lasers exhibit a higher measurement upper limit compared to those using semiconductor lasers.

Keywords：particle size； standard reference materials； polystyrene microspheres； laser particle size analyzer； measurement upper limit

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