To my opinion there will be always some residual H(OH) groups left after exchange or an attachment reaction due to inaccessible spots (gaps) on the surface. Instead of looking for an analysis method I would rather go for a proper end-capping, which offers you a practical solution (by blocking these groups), especially when you don't have attrition, i.e. your material is used in a fix bed.
If you are explicitly looking for surface analysis methods please check https://www.google.hu/url?sa=t&rct=j&q=&esrc=s&source=web&cd=2&cad=rja&uact=8&ved=0CDgQFjAB&url=http%3A%2F%2Fwww.chem.qmul.ac.uk%2Fsurfaces%2Fscc%2Fscat5.htm&ei=YzSpU6zOH7P20gWSkIGgDA&usg=AFQjCNGFgWCUcOxYJ4yVebXZ_pggBLQEgA&sig2=VeCiorr7_IjUYKDYnQnU1Q
I agree that a complete exchange is unlikely, but you can increase the amount of exchanged surface protons by increasing the pH far above the PZC (for example for SiO2 (PZC= 2-4) at pH=10-11. This is called "strong Electrostatic Adsorption"). For the characterization, you could try determining the initial density of surface hydroxyls (before exchange with cations) by eg. temperature programmed desorption and compare it to the amount of adsorbed cations (determined by elemental analysis)
When working at high pH, you should always think about hydrolysis of the metal. Such Hydrolysis might cause precipitation rather than adsorption.
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