Roos, A. H., et al. Soft Matter, 2021, DOI:https://doi.org/10.1039/D1SM00582K
We characterize temperature-dependent macroscopic and nanoscopic phase transitions and nanoscopic pre-transitions of water-soluble single chain nanoparticles (SCNPs). We analyze the temperature-dependent phase transitions of spin-labeled SCNPs by rigorous spectral simulations of a series of multicomponent EPR-spectra that derive from the nanoinhomogeneities (1) that are due to the single-chain compartmentation in SCNPs and (2) the transformation upon temperature change due to the LCST behavior. These transitions of the SCNPs and their respective polymer precursors can be monitored and understood on the nanoscale by following EPR-spectroscopic parameters like hyperfine couplings that depend on the surrounding solvent molecules or Heisenberg spin exchange.