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| Discussion and verification on the technical route of traceability of elemental film standard samples |
| Received:April 05, 2021 Revised:April 08, 2021 |
| View Full Text View/Add Comment Download reader |
| DOI：10.3969/j.issn.2095-1035.2021.05.010 |
| KeyWord:Atmospheric particulate matter, Elemental thin film standard sample, X-ray fluorescence spectrometry, Plasma atomic emission spectrometry，Metrological traceability |
| Author | Institution |
| REN Lijun |
国家环境分析测试中心 |
| Huang Chong |
绍兴开立尚谱环保科技有限公司 |
| FANG Shuang |
国环绿洲（固安）环境科技有限公司 |
| YIN Hui-min |
国家环境分析测试中心 |
| DU Zhen-yu |
国家环境分析测试中心 |
| Li Yuwu |
国家环境分析测试中心 |
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| Abstract: |
| Elemental thin film standard sample is an essential experimental material for the determination of inorganic elements in atmospheric particulate matter samples by X-ray fluorescence spectrometry (XRF). The development of domestic element film standard samples that meet the requirements of metrological traceability is of great significance for establishing XRF calibration curves in analysis of atmospheric particulate matter and to reduce the cost of purchasing film standard samples for users in XRF laboratories. A technical route is proposed to use both ICP-OES based on the acid digestion system and XRF by direct measurement to determine the element content in film samples, which is verified with the determination of rare earth elements in thin film samples. The feasibility of the acid digestion system and ICP-OES analysis method was explored with the coating solid powder material. The target element recovery rate is 93.3%～99.7%. The experimental results show that the WD-XRF calibration curve established based on the digestion-ICP-OES measurement results has a good linear relationship (i.e. the correlation coefficient of each element is 0.9978～1.000). The measurement result of the WD-XRF can meet the requirements of metrological traceability, as expected. Based on the precision of the fluorescence intensity data of the same batch of coated samples, the uniformity of the coating process was investigated. The relative standard deviation of intensity was from 0.16% to 1.5%. The evaluation data of uncertainty of measurement results show that the fitting model errors of ICP-OES are the main components of uncertainty of measurement results for low content filter membrane samples. The experimental results laid the foundation for the subsequent collaborative analysis of standards for film samples of other series of elements. |
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