X-ray photoelectron spectroscopy (XPS) or Energy Dispersive X-Ray Spectroscopy (EDX)

Dear Dr Hirbod, I think it is better to you do the bellow.

1- You must dissolve your composite in mixture of HCl/HNO3 or other strong acids to fully disolving of the your solids

2- in this step you can analyze your mixture by ICP or atomic absorption.

XPS has limitation like it scans only upto 10nm on the surface,so not a best method to analyze the amount of metal impregnated.As suggested by Dr.Sadegh,deliberate leaching with HNO3 followed by ICP analysis would give the amount.You can also do a AAS as well.

If you want to find the active Cu in Surface...Means accessible to at least gas molecules, then use N2O decomposition reaction method or CO or H2 TPD. good luck

Thanks everyone.

I might be a little late, but would like to add a small comment as well. X-ray fluorescence is a quite easy way to determine metal quantities in your samples as you do not need vacuum or any chemical preparation/treatment of your samples. And the data analysis is straightforward as well ... Best regards to everyone, Dirk

Atomic absorption is good for determination of total amount of element in the sample. But if you need amount of metallic atoms on the surface (for calculating catalytic activity) H2 adsorption would be better method. Not for Palladium!

The best way is using chemisorbsion technique (if you know of a good specialist and methodology) or using ICP ( good universal method for your task)

Well, to my opinion, XPS and chemisorption are probably the most adapted techniques. Other techniques have their own limitations : ICP or XRF are intrinsically "massic" methods and do not provide interesting data at the interface. EDX could be interested, but most of the analysis used for the deposition of the sample metallic grids... in copper !!! So that means that you won't be able to quantify Cu atome of your materials. XPS remains probably the most interesting for you, providing that you will be able to produce "clean" samples at the XPS scale.

Really depends on Cu amount and where do you want to see. For bulk analysis and to know the total amount of Cu in your material, below than 10wt% you may use AAS, at higher loading XRF is more valuable. While, XPS and EDX are very statistic (you should sample at different points of the material) and represent only what is on the surface, due to the detection limits of these methods.

To determine the %of metal content ICP-AES or AAS is the best method. But for determining the surface metal content, Chemisorption method is suitable

From ICP-AES or AAS, you can total amount of metal (surface as well as bulk) present on the surface of support. XPS and chemisorption gives only surface metal amount only, these can't give total metal amount.