Electrochemical measurement methods can be determined by an application you want to examine.

CV is the basic measurement skill for every electrochemical method.

If you want to use that material for use in energy storage material, you can do galvanostatic charge/discharge tests.

For more precise answer can be given if you Identify your target application

Both of elements have specific potential for the oxidation and reduction which will show their peaks on CV observation . As per your question, Fe is core and Au is shell. You did not mention about shell-thickness of element of nanoparticle. In this case, you may see only oxidation and reduction peaks of Au because CV is a surface-sensitive technique. The peak position of the surface element may be varied slightly due to electronic interaction/charge-transfer between two elements.

Cyclic Voltammetry is the most common and convenient method for making such analysis. You can also use the background electrolyte for measurements.

I do appreciate your kind advises!

For some detail based on TEM analysis, the coreshells turned out to be FeAu (~20nm core) FeO (~2nm shell) (but not clear it is mostly closed surface layer) and we are seeking whether this bimetallic hetero-structure could be useful for a direct methanol catalysis, oxidation rate study, or etc... However I am not that optimistic towards this direction due to the fact that Au-Fe layer seems less catalytic upon methanol oxidation, in contrast to reports elsewhere using other structures such as MgPd, PtPd...

As mentioned by others above, the first type of electrochemical characterization you want to perform is cyclic voltammetry... if you are looking at the material for oxidation reactions related to fuel cells, you are likely wanting to perform voltammetry in acidic conditions, possibly also do CO stripping to look at poisoning issues and both cyclic voltammetry and transient measurements in the fuel of choice (methanol, formic acid, etc.) The fact that you are using a very noble metal (Au) and one that isn't (Fe) might lead to changes in the structure as soon as you start your electrochemical tests (i.e. Fe can for example be dissolved in acidic conditions... there are studies in terms of for example PtFe nanoparticles which become Pt-skeleton structures, as Fe is leached out).

Dear Daniela,

As per your comment, would alkaline-based CV method be doable to achieve a feasible MFC performance against methanol oxidation?

Thanks for your kind comments!

Best,

Although alcohols as you say can be tested in alkaline solutions, I wonder how such conditions would affect the Fe? It might form oxides which might diminish reactivity? You can certainly try!