I have measured the ECSA value of commercially available 20 wt% Pd/C, from the Pd-O reduction region, in 0.5 M KOH. I am getting it to be 10.92 cm2. which is around 52 m2/gPd. Is it possible?
the value sounds not too unrealistic to me. To which positive inversion potential have you recorded your CVs? Estimating ECSA from the oxide reduction charge is quite unprecise because the higher you scan the more charge you will get.
I would calculate the ECSA as well from the H-UPD charge averaged from the cathodic and anodic scan of the CV. For a particle size around 3 nm I would expect roughly 100 m²/gPd.
Procedures are well-described in the attached publications.
All the best!
Philipp
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For the deposit of uniform spherical particles, their ESCA is related to the size of particles as follows:
ESCA=6/(rho*d),
Here ESCA - specific surface area (in cm2/g), rho - material density (12 g/cm3 for Pd), and d - particles size (in cm). So, for 52 m2/g, the mass-average size of your particles is 9.6 nm. Does it sound reasonable for you?