I am investigating all the different characterization techniques that enables to determine the Fe2+/Fe3+ ratio in slags. If possible with a quick routine analysis for process control.
Will the ion milling for TEM sample preparation alter the original oxidation of iron ?
If you have access to it, Mößbauer spectroscopy is probably the best method to analyze iron charge states. It is even possible to do it as spectromicroscopy:
Article Exploration of synchrotron Mössbauer microscopy with microme...
EELS also works, but it's certainly more expensive when talking about the plain spectroscopy.
Article A STEM/EELS method for mapping iron valence ratios in oxide minerals
If you need spectromicroscopy, the cost aspect might probably revert itself because TEM/EELS setups are more abundant.
I would consider XPS, but I should check with my colleague. It is a surface technique and the surface may not be the same as the bulk.
I am surprised to hear mention of TEM as a method for process control. I would think it makes for a rather slow cycle. It may also have the surface problem.
I had forgotten about Mossbauer. That is a good recommendation.
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