Development of pure manganese flake reference material for X-ray energy/wave dispersive spectrometer calibration

IF 1 4区工程技术 Q4 CHEMISTRY, ANALYTICAL

Accreditation and Quality Assurance Pub Date : 2025-08-18 DOI:10.1007/s00769-025-01667-5

Donghui Tian, Tao Song, Zhigang Wang, Yaling Chen, Gang Hu, Xu Li, Fang Cheng, Cheng Pu

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引用次数: 0

Abstract

Reference material is of great significance to the measurement accuracy of X-ray energy/wave dispersive spectrometer (EDS/WDS). In this work a reference material of manganese (Mn) content (mass fraction, %) of pure Mn flake for EDS/WDS calibration was developed. The surfaces of Mn flakes were finely treated by mechanical grinding and argon ion polishing, and the Mn flakes with high cleanliness and low roughness were obtained. The homogeneity and stability of Mn content of the Mn flakes were analyzed carefully using electron probe micro-analyzer (EPMA). The Mn content of the reference material was determined using inductively coupled plasma optical emission spectrometer (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS). The sources of uncertainty components of Mn reference material were fully analyzed and evaluated. The results show that the homogeneity of the pure Mn flake reference material meet the requirements. The Mn content of the vacuum-packed pure Mn flake is stable for up to one year at ambient temperature. The Mn content reference material of the pure Mn flake reference material is 99.5 %, and its expanded uncertainty is 0.9 % (k = 2). The pure Mn flake reference material can meet the calibration requirements of X-ray EDS/WDS, and guarantee the accuracy and consistency of measurement results. The content of this study complies with the definition of reference materials in ISO 17034 and can be used to calibrate measurement systems. The Mn content reference material can be widely used for element measurement in the fields of scientific research, manufacturing and trade activities.

Graphical abstract

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x射线能量/波色散光谱仪标定用纯锰片标准物质的研制

参考物质对x射线能量/波色散光谱仪（EDS/WDS）的测量精度具有重要意义。本文研制了一种用于EDS/WDS定标的纯锰片锰（Mn）含量（质量分数，%）标准物质。采用机械研磨和氩离子抛光对锰片表面进行了精细处理，获得了高清洁度、低粗糙度的锰片。利用电子探针微量分析仪（EPMA）对锰片进行了均匀性和稳定性分析。采用电感耦合等离子体发射光谱仪（ICP-OES）和电感耦合等离子体质谱法（ICP-MS）测定标准物质中Mn的含量。对Mn标准物质不确定度的来源进行了全面的分析和评价。结果表明，纯锰片标准物质的均匀性满足要求。真空包装的纯锰片的锰含量在室温下可稳定达一年。纯锰片标准物质的Mn含量为99.5%，其扩展不确定度为0.9% （k = 2）。纯锰片标准物质能够满足x射线EDS/WDS的校准要求，保证了测量结果的准确性和一致性。本研究的内容符合ISO 17034标准物质的定义，可用于校准测量系统。锰含量标准物质可广泛用于科研、制造和贸易等领域的元素测量。图形抽象

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来源期刊

Accreditation and Quality Assurance 工程技术-分析化学

CiteScore

1.80

自引率

22.20%

发文量

审稿时长

6-12 weeks

期刊介绍： Accreditation and Quality Assurance has established itself as the leading information and discussion forum for all aspects relevant to quality, transparency and reliability of measurement results in chemical and biological sciences. The journal serves the information needs of researchers, practitioners and decision makers dealing with quality assurance and quality management, including the development and application of metrological principles and concepts such as traceability or measurement uncertainty in the following fields: environment, nutrition, consumer protection, geology, metallurgy, pharmacy, forensics, clinical chemistry and laboratory medicine, and microbiology.