i intend to characterize and quantify total active sites on the surface of iron oxide nanoparticles during the catalytic study on aqueous based pollutants. if the reaction is on gas system model, you might use chemisorption method etc. however, since the pollutant is in liquid form, how we could quantify total active sites on the surface of nanoparticles? kindly advice. thank you.
Maybe use some molecules, also dissolved in the liquid phase, which show significant changes to their vibrational characteristics when adsorbed on the particles. Could be as "simple" as using CO, if suitable. The vibrational spectra could then be taken using IR spectroscopy.
I remember an older colleague (B. Chaudret) who mentioned to me having made inverstigations of this kind with bimetallic nanoparticles. At the time I think they looked into surface modifications of these particles. I don't have the reference at hand, though, will come back to mention if in case I find it.
Some of that is being mentioned in the book linked below, Chapter 2.1.1, page 238
https://books.google.de/books?id=E_03zJyPdZsC&pg=PA238&lpg=PA238&dq=B%3DChaudret+and+particles+and+CO&source=bl&ots=GfvJSn8OeR&sig=T1SyWYzXGf62du2eYLWexh-FvGo&hl=de&sa=X&ved=0ahUKEwix6-iJtJzMAhUsIcAKHVpkDG0Q6AEIKjAB#v=onepage&q=B%3DChaudret%20and%20particles%20and%20CO&f=false
Here comes what I found. Hope it is instructive (didn't read in detail!). Concerning quantification of active sites on your samples - this is something I regard as a highliy non-trivial issue. good luck.
Surface Chemistry on Colloidal Metals. Reversible Adsorbate-Induced Surface Composition Changes in Colloidal Palladium-Copper Alloys
John S. Bradley, Ernestine W. Hill, Bruno Chaudret, Anne Duteil
Langmuir, 1995, 11 (3), pp 693–695
DOI: 10.1021/la00003a002
Synthesis of monodispersed bimetallic palladium-copper nanoscale colloids
John S. Bradley, Ernestine W. Hill, Carl Klein, Bruno Chaudret, Anne Duteil
Chem. Mater., 1993, 5 (3), pp 254–256
DOI: 10.1021/cm00027a005
Publication Date: March 1993
Preparation and characterization of organosols of monodispersed nanoscale palladium. Particle size effects in the binding geometry of adsorbed carbon monoxide
J. S. Bradley, E. W. Hill, S. Behal, C. Klein, A. Duteil, B. Chaudret
Chem. Mater., 1992, 4 (6), pp 1234–1239
DOI: 10.1021/cm00024a023
Publication Date: November 1992
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