Coordination star polymers are a group of novel macromolecules with coordination metal-organic polyhedral (MOP) that make-up the core section. There is rare studies on the dynamic bonding of the coordination process and the further dynamic arm exchange process. Neutron scattering technologies are quite sensitive to hydrogen atoms, even compared to its isotopes. As we know that coordination star polymers are hydrogen enriched nano-scaled molecules (sizes from 2 to 10 nm), small angle neutron scattering (SANS) is an appropriate tool to characterize their solutions with high resolution and sensitivity. Two coordination star polymers with H-PS arms and D-PS arms were synthesized, respectively, for SANS studies of their possible dynamic arm exchange process. We propose to monitor the mixture solutions of H-star polymer and D-star polymer (molar ratio, 1:1) with SANS.