XPS can be okay but it still has its limitations. It is a surface senstive technique and may provide slightly different composition than the bulk material.
Mössbauer spectroscopy definitely works. However, this techniques needs a gamma-radiation source and is not available in many labs.
"- Clay, solid sample (solid crystalline powders), can be swollen by water."
What do you mean? This is a statement not a question.
Tamás Szabó Thank you very much Dr. Szabo. Your ideas are definately my plans (my PhD supervisor also recommend me to use Mössbauer spectroscopy and we have it), but still I will think about a way to reduce the strutural Fe(III) to Fe(II) in clay materals (no damage to the clay nanosheets at the same time). If you have any idea, please educate me without hesitation. Xiong
Dear Xiong, I do not have any idea at the moment but I recommend you to check early literature on clays. I think it is s challenging task...structural ion is strongly bound and it may be difficult to reduce these without completely disintegrating the silicate structure.