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Figure S1. 1H NMR spectra of different molecular weights of PS after sulfonation compared with polymerized styrene sulfonate.

Figure S2. UV/vis spectra of PSS obtained through polymerization and through sulfonation of PS.

Figure S3: 13C NMR inversion recovery experiments for PSS in D2O. Delays between 180 and 90° pulses are from bottom to top 0, 0.05, 0.5, 1, 2, 3, 6, 10, 16 s. 32 scans were performed for each delay with delay times between scans of 60 s.

Figure S4. 13C NMR spectra of poly(styrene sulfonate) for various conditions of sulfonation and compared to the polymerized styrene sulfonate.

Figure S5. SEC chromatograms, molar mass from multi angle light scattering and normalized light scattering intensity vs. time, for 16,000 g/mol PSS (red, right peak) and 108,000 g/mol PSS (blue, left peak). Both samples were 2.5 mg/mL in 60 % milliQ-water, 40 % acetonitrile containing 0.1 M NaNO3. Scattering is much more intense for larger molecules, so dimers would show up as shoulders on the left of the main peaks.

Figure S6. Correlation function (a) and hydrodynamic radius (b), obtained by dynamic light scattering, of PSS with Mw= 118,500 (Table 2) made by sulfonation of PS (polymer concentration was 1 mg/mL in 0.5 M NaCl, 25 oC).

Figure S7. UV-vis absorbance spectra of the progress of sulfonation of 280,000 g mol−1 PS in 96.7% H2SO4 at 90 oC.

Figure S8. 1H NMR of isotactic PS and atactic PS in CDCl3 (10 mg/mL)

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