It depends on which sites you want to determine: NH3-TPD is used for determination of acidic sites and CO2-TPD for basic sites. Classical pulse-sorption experiments are performed using CO, H2 or N2O for titration of catalytic active metal sites - all depending upon the information you are looking for.

http://zeta-pa.de/pics/ZetA-tpd-info_e.pdf

thanks sir for providing such a useful links

Apart from TPD, n-butylamine titration is also used for  the acidity determination of solid samples. 

You can also use Pyridine Adsorption/Desorption followed by FTIR for acid sites caracterization, This tecnique also identifies Bronsted and Lewis acid sites. 

Good Luck