Evaluation of analytical method performance for determination of heavy metals in soils by energy dispersive X-ray fluorescence spectrometry based on inter-laboratory collaborative experiments
FAN Shuang1, GUO Chao1, ZHANG Bai-hui1, 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
In order to investigate the performance of analytical method for determination of heavy metals in soil and sediment by energy dispersive X-ray fluorescence spectrometry (ED-XRF), 14 testing laboratories were organized. Five soil and six sediment standard samples were provided uniformly. Quantitative tests on heavy metal elements including As, V, Cr, Mn, Ni, Pb, Cu, Zn, Co, and Mo were performed on spectrometers (desktop, floor-standing or portable) made by 6 domestic and foreign instrument manufacturers. The limit of detection of the method was calculated using the standard deviation data of repeated test results of samples with low content of heavy metals. The limit value was obtained using the treated results in each laboratory by robust statistical method to multiply by a coefficient of 1.6. Before performing statistical analysis of data, the measurement results were screened in advance based on the quality control requirements of conventional heavy metal analysis and Mandel test (h/k test method). The data adoption rate (%) of each element was listed as follows: Zn (93.3-97.0), Pb (95.2-96.4), Mn (92.3-96.2), Cu (89.4-93.2), As (90.1-92.3), Ni (86.5-88.9), Cr (84.6-88.3) and V (81.4-84.8). The adoption rate reflected the status of the accuracy of heavy metal test results for all laboratories involved. The main reason for the lower adoption rate of V and Cr was possibly related to the fact that the interference of overlapping peaks was not effectively deducted in some laboratories. The adoption rate of application program using spectrum fitting to obtain the intensity was better than that of interval integration method, and the and the relevant laboratories needed to further optimize and improve the application program. The measurement of heavy metals including As, Cr, Mn, Ni, Cu, Zn, Pb, and V in soil-sediment samples by ED-XRF in most laboratories could meet the requirements of quantitative analysis. Since the content range of Co in standard samples was relatively narrow, the precision and accuracy should be further evaluated. Only when the mass fraction of Mo in sample was higher than 1mg/kg, the requirements of quantitative analysis could be met.
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FAN Shuang, GUO Chao, ZHANG Bai-hui, DU Zhen-yu, YIN Hui-min, LI Yu-wu. Evaluation of analytical method performance for determination of heavy metals in soils by energy dispersive X-ray fluorescence spectrometry based on inter-laboratory collaborative experiments. , 2020, 40(8): 8-21.
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