I am currently working on determining the elemental composition of shells of sea urchins. Most of the samples show relatively similar results but in some cases it is obvious that something is wrong (e.g. no calcium is shown).Since it is my first time using a SEM i dont really know what settings I need to use to get an EDS analysis as accurate as possible. All help is welcome,thank you in advance.
It seems that you have not feed the possible elements present in your sample while doing your eds study. Some times one should put the manes of the elements that are possibly be there.
WD for EDS you can find in a manual of your EDS system. It can be a bit different depending on configuration of your SEM/EDS (usually 10-15 mm). While WD does affect intensity of obtained spectra it usually not critical for qualitative/semiqualitative analysis when trace elements are of no interest.
Accelerating votage of 15kV should work for your specimens.
If you show us results of your analysis with and without Ca it would be easier to help you. Bear in mind that absence of Ca peak on otherwise normal spectrum means that there is no Ca, not some failure in settings.
My pattern is around 3 times the energy of the peak of interest, Large Probe Current and WD = 10 mm. You can't forget to turn off the IR!!!
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