Nanoparticles (NPs) are of considerable interest, owing to their enhanced catalytic activity and optical properties. Ionic liquids (ILs) are employed as a medium to prepare small (<20 nm in diameter) and relatively low dispersity (typically, ±1–2 nm) NPs. While ensemble techniques (e. g., UV/Vis) can provide a great deal of information, increasingly, single‐entity electrochemistry (SEE) has been used to provide physical insight into individual NP catalysis and dynamics. Herein, Pt NP impact current spikes for particles prepared in the IL phase and based on electrocatalytic amplification (ECA) of the borohydride oxidation reaction (BOR) were recorded during i‐t measurements. Additionally, direct oxidative LiBH4 nanocrystal (NC) impact signals were observed herein for the first time. By quantifying the charge transferred during the stochastic collision events, the radius of the NCs (rNC) was calculated (∼5.5 nm) and compares favorably with TEM images. Critically, small additions (1 % v/v) of a molecular, polar organic solvent (tetrahydrofuran, THF) disrupt the ILs supramolecular fluidic nature, which enhances NC impact frequency and the aggregation of Pt NPs.