Accuracy and Precision of Energy Dispersive X-Ray Fluorescence (EDXRF) Analysis of Trace and Major Elements in Rock Standard Reference Materials Using Fine Powder
In this work the performance of a screening analytical method for Energy Dispersive
X-Ray Fluorescence (EDXRF) analysis in terms of accuracy and precision was evaluated
through analysis of rock standard reference materials. The method allowed the division
of elements into four groups taking into account the excitation energies and measurement
conditions of the sample. Two standard reference materials were used
and 15 sample replicates were prepared and analyzed, then statistics were applied
to assess the precision and accuracy of analytical results. The obtained results
show that major compounds or elements (SiO2, P2O5,
K2O, CaO, Fe2O3, Ti) can be determined in fine
powder sample with a deviation lower than 15%, and a relative standard deviation
in the range (1 - 10)%. The deviation was found to be lower than 5% for major compounds
such as K2O, and CaO, which suggest that the EDXRF is accurate in evaluating
major elemental concentrations in rock samples. It was also found that the method
seems to be more accurate and precise for major elements than for trace element
investigation. This screening analytical method can be used for routine analysis
with acceptable results, even though the method should be optimized to increase
its precision and accuracy.
References
[1]
Akbulut, S., Cevik, U., Van, A. A., De Wael, K., & Van Grieken, R. (2014). Precision and Accuracy of ST-EDXRF Performance for As Determination Comparing with ICP-MS and Evaluation of As Deviation in the Soil Media. Chemosphere, 96, 16-22. https://doi.org/10.1016/j.chemosphere.2013.06.086
[2]
Croffie, M. E. T., Williams, P. N., Fenton, O., Fenelon, A., Metzger, K., & Daly, K. (2020). Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis. Agronomy, 10, Article No. 1309. https://doi.org/10.3390/agronomy10091309
[3]
Duchesne, J. C., & Bologne, G. (2009). XRF Major and Trace Element Determination in Fe-Ti Oxide Minerals. Geologica Belgica, 12, 205-212.
[4]
Enzweiler, J., & Webb, P. C. (1996). Determination of Trace Elements in Silicate Rocks by X-Ray Fluorescence Spectrometry on 1:5 Glass Discs: Comparison of Accuracy and Precision with Pressed Powder Pellet Analysis. Chemical Geology, 130, 195-202. https://doi.org/10.1016/0009-2541(96)00022-8
[5]
Guembou, J. C. S., Moyo Ndontchueng, M., Mekongtso Nguelem, J. E., Chene, G., Motapon, O., Kayo, S. A., & Strivay, D. (2019). Determination of the Natural Radioactivity, Elemental Composition and Geological Provenance of Sands from Douala in the Littoral Region of Cameroon Using X-Ray and γ-Ray Spectrometry. Applied Earth Science, 128, 167-180. https://doi.org/10.1080/25726838.2019.1637656
[6]
Injuk, J., & Van Grieken, R. E. (1993). Sample Preparation for XRF. In Handbook of X-Ray Spectrometry Methods and Techniques (p. 658). Marcel Dekker, Inc.
[7]
Kimura, J., & Yamada, Y. (1996). Evaluation of Major and Trace Element XRF Analyses Using a Flux to Sample Ratio of Two to One Glass Beads. Journal of Mineralogy, Petrology and Economic Geology, 91, 62-72. https://doi.org/10.2465/ganko.91.62
[8]
Krishna, A. K., Khanna, T. C., & Mohan, K. R. (2016). Rapid Quantitative Determination of Major and Trace Elements in Silicate Rocks and Soils Employing Fused Glass Discs Using Wavelength Dispersive X-Ray Fluorescence Spectrometry. Spectrochimica Acta Part B: Atomic Spectroscopy, 122, 165-171. https://doi.org/10.1016/j.sab.2016.07.004
[9]
Lundblad, S. P., Mills, P. R., & Hon, K. (2008). Analysing Archaeological Basalt Using Non-Destructive Energy-Dispersive X-Ray Fluorescence (EDXRF): Effects of Post-Depositional Chemical Weathering and Sample Size on Analytical Precision. Archaeometry, 50, 1-11.
[10]
Lutz, J., & Pernicka, E. (1996). Energy Dispersive X-Ray Fluorescence Analysis of Ancient Copper Alloys: Empirical Values for Precision and Accuracy. Archaeometry, 38, 313-323. https://doi.org/10.1111/j.1475-4754.1996.tb00779.x
[11]
Nakayama, K., & Nakamura, T. (2005). X-Ray Fluorescence Analysis of Rare Earth Elements in Rocks Using Low Dilution Glass Beads. Analytical Sciences, 21, 815-822. https://doi.org/10.2116/analsci.21.815
[12]
Orihashi, Y., & Hirata, T. (2003). Rapid Quantitative Analysis of Y and REE Abundances in XRF Glass Bead for Selected GSJ Reference Rock Standards Using Nd-YAG 266 nm UV Laser Ablation ICP-MS. Geochemical Journal, 37, 401-412. https://doi.org/10.2343/geochemj.37.401
[13]
Remya, D. P. S., Trupti, A. C., Nicy, A., Dalvi, A. A., Swain, K. K., Wagh, D. N., & Verma, R. (2015). Evaluation of Uncertainty in the Energy Dispersive X-Ray Fluorescence Determination of Platinum in Alumina. Analytical Methods, 7, 5345-5351. https://doi.org/10.1039/C5AY00547G
[14]
Rousseau, R. M. (2001). Detection Limit and Estimate of Uncertainty of Analytical Results. The RIGAKU Journal, 18, 33-47.
[15]
Saini, N. K., Mukherjee, P. K., Rathi, M. S., & Khanna, P. P. (2000). Evaluation of Energy-Dispersive X-Ray Fluorescence Spectrometry in the Rapid Analysis of Silicate Rocks Using Pressed Powder Pellets. X-Ray Spectrum, 29, 166-172. https://doi.org/10.1002/(SICI)1097-4539(200003/04)29:2<166::AID-XRS411>3.0.CO;2-L
[16]
Saini, N. K., Mukherjee, P. K., Rathi, M. S., Khanna, P. P., & Purohit, K. K. (2002). Trace Element Estimation in Soils: An Appraisal of ED-XRF Technique Using Group Analysis Scheme. Journal of Trace and Microprobe Techniques, 20, 539-551. https://doi.org/10.1081/TMA-120015615
[17]
Xue, D. S., Tian, H. C., Zhang, D. P., Liu, Y. H., Sun, J. F., Wu, S. T., Liu, S. K., Guo, S., & Wan, B. (2022). Quantitative Verification of 1:35 Diluted Fused Glass Disks with 10 mg Sample Sizes for the Wavelength-Dispersive X-Ray Fluorescence Analysis of the Whole-Rock Major Elements of Precious Geological Specimens. Spectrochimica Acta Part B: Atomic Spectroscopy, 193, Article ID: 106433. https://doi.org/10.1016/j.sab.2022.106433