Let's assume that the PEEK is a triphenyl repeating unit and that sulfonation occurs only on one of the phenyl rings. The extent of the sulfonation (DS %) can be estimated from the NMR by singling out the lonely signal around 7.5 ppm, which corresponds to the hydrogen ortho to the sulfonate. In a 100% sulfonation (i.e., DS = 100%), the ratio of this signal to the rest of the aromatic hydrogens (r) should be 1/11. Similarly, at DS values of 75%, 50%, and 25%, the corresponding r values should be 1/15, 1/23, and 1/47, respectively. Thus, the DS value (in %) is relatable to the r value using the equation DS = 1076.8r + 2.65. So, from your proton nmr, determine the r value and plug into the equation.
Sajid Hussain, using this method, even it is possible to calculate the degree of substitution in a different substituted position in the molecule. Please, give my best regards to Dr. Afsar Khan from COMSATS!