Results of investigations in energy dispersive X ray fluorescence analysis aimed at the develop ment of a high sensitivity method of microanalysis of solutions are presented. A combined scheme of analysis of one drop of solution of the volume several microliters is proposed and tested. The scheme includes a new preconcentration method based on the drop evaporation in the presence of a micrograin of a hydrophilic adsorbent followed by the microanalysis of the solid phase on the portable device with a polycapillary lens with a focal spot of 10 µm designed at the Institute of Physical Optics. Analytically meaningful X ray fluores cence spectra are obtained using DETATA (grain diameter about 100 µm) and SAC8 (50 µm) adsorbents and individual drops of model solutions containing Mn, Fe, Co, Ni, Cu, and Zn (0.2 mg/L and higher) and ana lytical characteristics of the proposed approach are demonstrated.