ISSN 1008-5548

CN 37-1316/TU

最新出版

玻璃微珠粒度分布标准物质的研制及在激光粒度仪性能评估中的应用

Development of glass microbead particle size distribution reference materials and their application in performance evaluation of laser particle size analyzers

陈胜利1, 朱秀芹2

1. 中国石油大学(北京) 化学工程与环境学院,北京 102249; 2.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. 玻璃微珠粒度分布标准物质的研制及在激光粒度仪性能评估中的应用[J]. 中国粉体技术, 2026, 32(5): 1-13.

Chen Shengli, Zhu Xiuqin. Development of glass microbead particle size distribution reference materials and their application in performance evaluation of laser particle size analyzers[J]. China Powder Science and Technology, 2026, 32(5): 1-13.

DOI:10.13732/j.issn.1008-5548.2026.05.012

收稿日期: 2026-05-03, 修回日期: 2026-08-24, 上线日期: 2026-08-30。

基金项目: 国家自然科学基金项目,编号 :22472201。

第一作者: 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】 研制单峰宽分布粒度标准物质,并用于研究激光粒度仪的测量性能。 【方法】 采用喷雾成型-筛分法,制备11 种粒径在20~150 μm 窄分布玻璃微珠粒度标准物质,通过将窄分布标准物质按质量比例定量混合,获得呈拟正态分布和拟均匀分布的宽分布粒度标准物质(QBW12030 和 QBW12031);窄分布标准物质的定值采用光学显微镜法;2种宽分布粒度标准物质的粒径量值,由构成它们的窄分布标准物质的定值结果及混合比例计算得到;利用标准物质,对我国市售多种型号的激光粒度仪进行检验。 【结果】 激光粒度仪均能较准确地测量窄分布标准物质的Dv(50)值,绝大部分仪器测量误差在2%以内;对宽分布标准物质的测量误差明显大于窄分布标准物质,尤其是Dv(1)、Dv(2.5)、Dv(97.5)和Dv(99)的误差较大;测量均匀分布粒度标准物质的误差又大于测量正态分布标物的误差,Dv(1)和Dv(2.5)的测量值总体上比标准值偏小,而Dv(97.5)和Dv(99)的测量值总体上比标准值偏大,即仪器测得的粒径分布峰较实际峰有所展宽;不同品牌的激光粒度仪之间,测量宽分布标准物质的误差差异较大。 【结论】 所研制的标准物质稳定性良好,定值结果准确可靠;对激光粒度仪而言,准确测量宽分布样品(尤其是非正态分布样品)的 Dv(1)、Dv(2.5)、Dv(97.5)和Dv(99)值,在未来仍然是一项挑战。

关键词: 颗粒粒度标准物质; 宽分布颗粒体系; 玻璃微珠; 激光粒度仪

Abstract

Objective China still lacks broad-distribution particle size reference materials (PSRMs) that provide Dv(1) to Dv(99) values for evaluating the measurement performance of laser particle size analyzers. This study aims to develop unimodal broad-distribution PSRMs and use them to evaluate the performance of current laser particle size analyzers.

Methods First, eleven narrow-distribution glass microbead PSRMs with particle sizes ranging from 20 µm to 150 µm were prepared using spray forming and sieving methods, and their reference material numbers were QBW12004, QBW12005, …, and QBW12015, respectively. Subsequently, broad‑distribution reference materials with quasi‑normal and quasi‑uniform distributions were obtained by mixing the narrow‑distribution materials at appropriate ratios, and their reference material numbers were QBW12030 and QBW12031, respectively. The narrow‑distribution PSRMs were certified using an optical microscope calibrated with the NIST SRM 2800 stage micrometer, and the certified values were traceable to the He–Ne laser wavelength. The particle size values of the broad‑distribution reference materials were calculated and certified based on the certified values of the narrow‑distribution samples and their mixing ratios. Using the developed reference materials, the performance of commercially available laser particle size analyzers in the Chinese market was evaluated and analyzed.

Results and Discussions The developed narrow‑distribution glass microbead PSRMs provided mean particle size values (Dv(50) and D(4,3)). The two broad‑distribution reference materials provided continuous distribution values (Dv(1) to Dv(99)). All current brands of laser particle size analyzers could measure the Dv(50) of narrow‑distribution samples relatively accurately, with errors within 2% for the vast majority of instrument models. However, the errors in measuring broad‑distribution reference materials were significantly larger than those for narrow‑distribution materials, and the error for the quasi‑uniform distribution sample (QBW12031) was markedly larger than that for the quasi‑normal distribution sample (QBW12030). In practice, current laser particle size analyzers could not accurately measure the uniform‑distribution sample; instead, they measured it as a normal distribution. When measuring broad‑distribution samples, the errors for data points in the middle of the distribution were relatively small, whereas those for data points at the two ends of the distribution were considerably larger, especially for Dv(1), Dv(2.5), Dv(97.5), and Dv(99). The measurement errors for the coarse‑end data (Dv(97.5) and Dv(99)) were even greater than those for the fine‑end data (Dv(1) and Dv(2.5)). The accuracy of measuring broad‑distribution reference materials varied considerably among different brands of laser particle size analyzers. For the foreseeable future, measuring Dv(1), Dv(2.5), Dv(97.5), and Dv(99) in broad‑distribution samples (especially non‑normal distribution samples) using laser particle size analyzers would remain a challenge.

Conclusions Eleven narrow‑distribution glass microbead PSRMs with sizes ranging from 20 µm to 150 µm, as well as two broad‑distribution reference materials, are successfully developed. The broad‑distribution reference materials fill the gap in China’s continuous broad‑distribution particle size reference materials. All current brands of laser particle size analyzers can measure the Dv(50) of narrow‑distribution samples relatively accurately, while the errors in measuring broad‑distribution materials are significantly larger than those for narrow‑distribution materials. The measurement error of a laser particle size analyzer depends not only on the performance of the instrument itself but also on the width and type of the particle size distribution of the sample. Current technical standards for laser particle size analyzers (ISO 13320:2020 and GB/T 19077‑2024) specify requirements for instrument measurement errors, but they do not specify requirements for the width and type of the sample particle size distribution. This is an aspect that needs to be improved in future revisions of the standards. As laser particle size analyzer technology advances, future standards will gradually incorporate measurement error requirements for more data points at both extremes of the distribution (e.g., Dv(5) and Dv(95), and even Dv(1) and Dv(99)).

Keywords: particle size reference material; broad-distribution particle systems; glass microbeads; laser particle size analyzer

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