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The possibility of the determination of mercury(II) with dithizone on the solid phase of a fibrous ion-exchange material filled with the AV-17 anion exchanger was studied. Mercury is adsorbed as an anionic complex. The sorption of mercury as chloride, iodide, sulfate, thiosulfate, nitrate, and EDTA complexes was studied. A procedure was proposed for the sorption–spectrometric determination of mercury with dithizone on a solid phase after sorption as the chloride complex. For improving the selectivity of the method, EDTA is added to the solution. The determination is affected only by Pd(II). The time of analysis is 15 min. The procedure was tested in the analysis of tap and river water and a solution modeling natural water.