Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis
Energy-dispersive X-ray fluorescence spectrometry (EDXRF) is a rapid and inexpensive method for soil analysis; however, analytical results are influenced by particle size effects and spectral interferences. The objective of this study was to optimise sample preparation and calibrations to improve th...
| Main Authors: | , , , , , |
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| Format: | Article |
| Language: | English |
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MDPI AG
2020-09-01
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| Series: | Agronomy |
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| Online Access: | https://www.mdpi.com/2073-4395/10/9/1309 |
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| author | Maame E. T. Croffie Paul N. Williams Owen Fenton Anna Fenelon Konrad Metzger Karen Daly |
| author_facet | Maame E. T. Croffie Paul N. Williams Owen Fenton Anna Fenelon Konrad Metzger Karen Daly |
| author_sort | Maame E. T. Croffie |
| collection | DOAJ |
| description | Energy-dispersive X-ray fluorescence spectrometry (EDXRF) is a rapid and inexpensive method for soil analysis; however, analytical results are influenced by particle size effects and spectral interferences. The objective of this study was to optimise sample preparation and calibrations to improve the accuracy of EDXRF for soil tests. Methods of sample preparation were compared by calculating the recoveries of 13 elements in four International Soil-Analytical Exchange (ISE) standards prepared as loose powder (LP), pressed pellet (PP), and pressed pellet with wax binder (PPB). A matching library (ML) was created and evaluated against the fundamental parameters (FP) calibration using 20 ISE standards. Additionally, EDXRF results of 41 tillage soils were compared with Inductively coupled plasma optical emission spectrometry (ICP-OES) results. The PPB had most recoveries within the acceptable range of 80–120%; conversely, PP yielded the poorest element recoveries. For the calibration, the ML provided better recoveries of Ni, Pb, Cu, Mg, S, P, and Cr; however, for Zn, and Mn, it had the opposite effect. Furthermore, EDXRF results compared with ICP-OES separated by soil texture class for Al, K, Mn, and Fe. In conclusion, the EDXRF is suitable for quantifying both trace elements and macronutrients in contaminated soils and has the potential to provide screening or prediction of soil texture in agriculture. |
| first_indexed | 2024-03-10T16:36:42Z |
| format | Article |
| id | doaj.art-4b9cd64d26f547c79bd6d20898c809d1 |
| institution | Directory Open Access Journal |
| issn | 2073-4395 |
| language | English |
| last_indexed | 2024-03-10T16:36:42Z |
| publishDate | 2020-09-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Agronomy |
| spelling | doaj.art-4b9cd64d26f547c79bd6d20898c809d12023-11-20T12:22:10ZengMDPI AGAgronomy2073-43952020-09-01109130910.3390/agronomy10091309Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil AnalysisMaame E. T. Croffie0Paul N. Williams1Owen Fenton2Anna Fenelon3Konrad Metzger4Karen Daly5Institute for Global Food Security, School of Biological Sciences, Queen’s University Belfast, Belfast BT9 5DL, UKInstitute for Global Food Security, School of Biological Sciences, Queen’s University Belfast, Belfast BT9 5DL, UKEnvironment, Soils and Land Use Department, Teagasc Johnstown Castle Research Centre, Y35 TC97 Wexford, IrelandEnvironment, Soils and Land Use Department, Teagasc Johnstown Castle Research Centre, Y35 TC97 Wexford, IrelandEnvironment, Soils and Land Use Department, Teagasc Johnstown Castle Research Centre, Y35 TC97 Wexford, IrelandEnvironment, Soils and Land Use Department, Teagasc Johnstown Castle Research Centre, Y35 TC97 Wexford, IrelandEnergy-dispersive X-ray fluorescence spectrometry (EDXRF) is a rapid and inexpensive method for soil analysis; however, analytical results are influenced by particle size effects and spectral interferences. The objective of this study was to optimise sample preparation and calibrations to improve the accuracy of EDXRF for soil tests. Methods of sample preparation were compared by calculating the recoveries of 13 elements in four International Soil-Analytical Exchange (ISE) standards prepared as loose powder (LP), pressed pellet (PP), and pressed pellet with wax binder (PPB). A matching library (ML) was created and evaluated against the fundamental parameters (FP) calibration using 20 ISE standards. Additionally, EDXRF results of 41 tillage soils were compared with Inductively coupled plasma optical emission spectrometry (ICP-OES) results. The PPB had most recoveries within the acceptable range of 80–120%; conversely, PP yielded the poorest element recoveries. For the calibration, the ML provided better recoveries of Ni, Pb, Cu, Mg, S, P, and Cr; however, for Zn, and Mn, it had the opposite effect. Furthermore, EDXRF results compared with ICP-OES separated by soil texture class for Al, K, Mn, and Fe. In conclusion, the EDXRF is suitable for quantifying both trace elements and macronutrients in contaminated soils and has the potential to provide screening or prediction of soil texture in agriculture.https://www.mdpi.com/2073-4395/10/9/1309calibrationelemental analysissoilspectrometryX-Ray fluorescence |
| spellingShingle | Maame E. T. Croffie Paul N. Williams Owen Fenton Anna Fenelon Konrad Metzger Karen Daly Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis Agronomy calibration elemental analysis soil spectrometry X-Ray fluorescence |
| title | Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis |
| title_full | Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis |
| title_fullStr | Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis |
| title_full_unstemmed | Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis |
| title_short | Optimising Sample Preparation and Calibrations in EDXRF for Quantitative Soil Analysis |
| title_sort | optimising sample preparation and calibrations in edxrf for quantitative soil analysis |
| topic | calibration elemental analysis soil spectrometry X-Ray fluorescence |
| url | https://www.mdpi.com/2073-4395/10/9/1309 |
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