Determination of inorganic elements in atmospheric particles by energy dispersive X-ray fluorescence spectrometry: establishment, evaluation and maintenance of the application program
GUO Chao1, ZHANG Bai-hui1, FAN Shuang1, DU Zhen-yu2,3,4 YIN Hui-min*2,3,4, LI Yu-wu1,2,3
1. Guohuan Oasis (Gu′an) Environmental Technology Co., Ltd., Langfang 065500, China; 2. Environmental Development Centre of the Ministry of Ecology and Environment, Beijing 100029, China; 3. National Research Center for Environmental Analysis and Measurements, Beijing 100029, China; 4. State Environmental Protection Key Laboratory for Dioxin Pollution Control, Beijing 100029, China
Abstract：During the determination of inorganic elements (Na, Mg, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Pb, Sr and Ba) in filtration membrane of atmospheric particles by energy dispersive X-ray fluorescence spectrometry (ED-XRF), the pretreatment of sample is not required. The analysis method is rapid and accurate, and the standard method has been issued and implemented. Based on many years of application experience, the following key points for the establishment of application program are included: (1) The overlapping spectral peaks should be analyzed by full spectrum fitting method when there is interference to deduct or reduce the influence of interference peaks and to obtain the characteristic peak intensity of the target element; (2) In order to ensure the spectral fitting of Na-K, Mg-K, Al-K and Si-K, the Lα lines with same or similar positions should be removed from the spectral lines which participate in the fitting; (3) Elements with interference or mutual interference, such as As-Pb, Fe-Co, Ti-V-Ba, Fe-Mn and Mn-Cr, must be determined simultaneously under the same grouping conditions; (4) The rational use of filters is helpful to improve the signal-to-noise ratio and reduce the background value. The accuracy of determination results is greatly affected by background subtraction especially for low content elements; (5) The setting of parameter intercept at 0 after regression of calibration curve can effectively avoid the influence of impurities on the support film of standard sample on the subsequent sample detection results; (6) When there is a lack of particulate filter standards in the market, the results of different analysis techniques, different instrument testing, and comparison between many laboratories for the same particulate samples in filter media can effectively find out the problems in application program. The experiences in many years indicate that, the study and commercial product of simulated particulate matter standard on filter media and recalibration samples for light element X-ray fluorescence intensity in domestic is of great significance for effectively monitoring the intensity fluctuations, ensuring the consistency of sample test results at the same instrument and the comparability of test results of the same samples between different laboratories.
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GUO Chao, ZHANG Bai-hui, FAN Shuang, DU Zhen-yu YIN Hui-min, LI Yu-wu. Determination of inorganic elements in atmospheric particles by energy dispersive X-ray fluorescence spectrometry: establishment, evaluation and maintenance of the application program. , 2020, 40(9): 1-9.
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