Dynamic light scattering was used to gain insight into pH-dependent solution behaviour of the star-shaped block copolymers. Sample preparation was carried out by dissolution at pH = 13 at 0.2 mg/mL or 0.4 mg/mL respectively in case of pH = 3 and pH = 5, followed by titration (see below). Please note that comparably large aggregates were formed at pH = 3 after titration, thus measurements had to be conducted directly after titration and a 5 µm filter had to be used to account for large aggregates. . Moreover, we also examined the aggregates formed by [PEG27-b-PtBAMA6]4 aggregates by AFM. The films of the copolymer solutions at pH= 3 and pH= 13 at a concentration of 0.2 mg/mL were deposited on silicon wafers by spin coating. Figure shows representative AFM images of aggregates formed at pH= 3 (Figure ) and pH= 13 (Figure ). At pH 3, the lateral sizes of the aggregates is distinctly larger (≈ 800 nm -1.7 µm) compared to pH 13 (≈ 40 nm -200 nm), which is in agreement with the results obtained from DLS experiments. The overall sizes are slightly lower, presumably due to drying. With further increase of the solution concentration to 1 mg mL -1 , larger aggregates were observed (Figure ). Additionally, the size of aggregates increases if the PDha block lengths is increased in case of [PEG27-b-PDha41]4(Figure ).