Scanning electron microscopy and X-ray diffraction in the determination of macroelements in soil and plants

Sample preparation is a crucial stage in obtaining correct results for micro- and macro-elements in soil and plants. The current study is a part of systematic research on the methods for soil and plant sample preparation for analysis of the most important macro-elements. The purpose is to determine the limits of the application of the most widely spread standardized and non-standardized methods for sample preparation and to shed more light on the possibilities of using scanning electron microscopy/energy dispersive spectroscopy (SEM-EDS) and X-ray Diffraction (XRD) in soil and plant analysis. The most common methods for extracting macro- elements in soil and plants (dry ashing, acid digestion, and microwave digestion in different variants) were compared using three certified soil samples and the Polish reference material CTR-VTL-2 (Virginia tobacco leaves). Three macro-elements (K, Ca and Mg) in the digest were analyzed using flame AAS and the insoluble fraction after digestion were analysed using XRD and SEM-EDS. It is concluded, that the degree of extraction of the elements from soil and plant materials is highly dependent on the mineralisation method. The X-ray investigation showed the formation of KClO4 when HClO4 was used as a part of the acids mixture. The use of HF at Ca and Mg determination led to the formation of CaF2 and MgF2. The result was verified by SEM-EDS.