Heavy metals rank high among the environmental pollutants nowadays. The rare-earth elements (REE) emissions in the environment have also increased due to the growth of hightech production. Therefore, the development of materials for effective removal of heavy and REE for the purpose of future reuse is relevant. We obtained diethylenetriaminefunctionalized polysilsesquioxane with phenylene bridges, thoroughly characterized it and compared its sorption properties towards different heavy and REE metal ions (Fig.1). Figure 1. Synthesis, characterisation, and sorption properties of diethylenetriamine-silica Typically for the phenylene-bridged materials [1], the bulk of the sample is comprised by very small particles (<50 nm in size) forming a well-developed three-dimensional mesoporous structure (as witnessed by N2 adsorption-desorption isotherms). Qualitatively the incorporation of diethylenetriamine groups was confirmed by characteristic adsorption bands in the infrared spectra, while analysis on CHNS elements indicates the quantitative content of groups at the level of 1.5 mmol/g. Comparing the sorption of different metal ions in mmol/g, the uptake of Ni2+ is the highest, while the uptake of the attested REE is similar: 0.97 (Ni2+) > 0.65 (Cu2+) > 0.4 (Eu3+, Er3+, or Tb3+). Thus, samples of this type have potential for use in sorption to remove metal ions from water