研究目的
To assess the use of energy-dispersive X-ray fluorescence (EDXRF) spectrometry for elemental content evaluation in nanoparticle-containing agricultural samples, including seeds, suspension fertilizers, and plant leaves.
研究成果
EDXRF is a robust, fast, low-cost, and suitable technique for elemental quantification in nanoparticle-containing agricultural specimens. It demonstrated adequate performance for monitoring elements in seeds, suspension fertilizers, and plant leaves, with satisfactory LODs, repeatability, and trueness. The technique is recommended for multielemental analysis in such studies, though it has higher LODs than some other methods.
研究不足
EDXRF has higher limits of detection compared to techniques like ICP-MS or ICP-OES, which may not be suitable for very low concentration analyses. The method may not differentiate between different chemical species of the same element, and matrix effects can require correction methods. Sample preparation, such as dilution or ashing, is necessary and could introduce contamination or errors.
1：Experimental Design and Method Selection:
The study employed EDXRF spectrometry for qualitative and quantitative analyses of elements in agricultural samples containing nanoparticles. Methods included dry-ashing digestion for seedlings, thin-film preparation for suspension fertilizers, and direct analysis of powdered leaves using fundamental parameter (FP) and standard addition methods.
2：Sample Selection and Data Sources:
Samples included Phaseolus vulgaris (common bean) seedlings treated with ZnO, CuO, and Fe3O4 nanoparticles; submicron suspension fertilizers of MnCO3, ZnO, and CuO; and P. vulgaris leaves exposed to ZnO nanoparticles. Certified reference materials (NIST standards) were used for trueness evaluation.
3：List of Experimental Equipment and Materials:
Equipment included an EDXRF benchtop unit (EDX720, Shimadzu), muffle furnace (F-2, Fornitec), laboratory oven (515/4A, Fanem), tube shaker (Marconi MA 162), oscillating stirring table (TE-240/1, Tecnal), germination chamber (TE-4020, Tecnal), and various cuvettes and films (e.g., Spex Ind. Inc.). Materials included nanoparticles, acids, internal standards (e.g., Ga), and CRMs.
4：Experimental Procedures and Operational Workflow:
For seedlings, seeds were germinated, treated with NPs, dried, ashed, digested, and analyzed by EDXRF with internal standard. For suspension fertilizers, samples were diluted, homogenized, and analyzed as thin films. For leaves, samples were dried, ground, and analyzed directly or with standard addition.
5：Data Analysis Methods:
LODs were calculated using specific equations, and trueness was assessed through recovery percentages. Calibration curves were built, and statistical analyses (e.g., standard deviations) were performed.
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