The problem is that the weight quantities sum exceeds 120% while all the standards (two different sets including pure elements and compounds such as LaB6, RbI, AgI, NaAlSi3O8) lay in the range 99.5-100.5. No signs of cathodoluminescence are visible on the spectra, no visible sample degradation or silver migration to or from the analysis points both in BSE or SE modes. The spectra acquisition area was about several tens of microns.
May it be caused by x-ray reabsorption-reemission in the substance? Can it be corrected or taken into account?
Dear Vladimir,
This problem is not frequent and, in fact, it has only happened to me once. We justified the problem by a software error, because it happened to us with different standards. What we did was shut down the system completely and restart it again. We reconnected the system and the failure recurred, so we repeated the process and reinstalled the software. After the reinstall we no longer had this problem.
I suppose that in your case you will have verified that this problem only occurs in certain samples but, if not, try with some standard because the same thing can happen to you as to us. These problems are very rare, but sometimes the software can be degraded and you need to reinstall it.
Best,
Fran
Thank you, Francisco Manuel Marquez ,
It seems that it's not our case because the standards measured along with the sample still give reasonable values.
However, thank you for your suggestion, I'd try to export data to another software and recalculate the compositions
Thanks, Marcella Bini,
We performed a single-crystal x-ray experiment. It is certainly a homogeneous compound with a defined structure, however, it still can be non-stoichiometric
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