<p>In contrast to colloidal Prussian blue, dispersed analogs of transition cyanobimetals are underrepresented in fundamental research, despite their significant practical potential and the growing interest in their applications. A recent study has reported the synthesis and characterization of zinc hexacyanoferrate colloidal particles with an overall surface charge ranging from negative to neutral. Building on this progress, the present work focuses on the pilot approach for the creation and characterization of positively charged particles prepared by cation adsorption on the negatively charged nanosample, investigates the affinity of transition metals for cyano-bridging, and examines the influence of <i>t</i>-butanol on cyano-bridge formation. The nexus of the investigation is the characterization and coagulation behavior of hydrosols, which provides valuable insights for applied researchers and offers a data set that advances the development of new materials with unique properties. The quantitative analysis using Dynamic Light Scattering, Laser Doppler Velocimetry, and Infrared Spectroscopy supported the research. The combination of these techniques—each probing different sample phenomena—yields complementary data that enable comprehensive analysis and robust conclusions.</p> Graphical abstract <p></p>