I am fitting a W4d orbital where the 5/2 peak height appears to be smaller than the 3/2. I have tried with multiple curve fittings but the FWHMs are very high, between 4 and 6 eV. When using smaller FWHM, the peaks go too high and the resulting curve fluctuates too much in comparison to the raw data.
4-6eV is indeed a lot, with a modern setup the expectation would be somewhere in the 1-2eV range. Are you allowed to share a spectrum so we can see whether it looks maybe like multiple components convolutiong into one thing?
As far as I remember, the FWHM should be determined by each individual device, and agree with Jurgen, it should be within 1-2 eV. The easiest would be to measure few reference samples containing (surely) peaks with single components, from this you can find what FWHM values are typical for the device and use those for fitting.
Would be useful to see this spectrum. It's impossible for the 5/2 to be smaller than the 3/2, so I would assume that there is another element present or you have a really strange background to the spectrum.
I would point out that there is certainly nothing wrong with the W4d peaks being 4 eV or so in FWHM as these will have different relaxation times and will be broader. I would have a concern if you were quoting the 4f peaks with those widths however!
For example, in WS2, I find that W4f peaks are ~ 0.7 eV, with the corresponding W4d peaks ~ 4 eV.
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