Method for determining the quantitative composition of a powder sample
A method for automatic determination of the quantitative composition of a powder sample, comprises the following steps: (a) predetermining a list of phases; (b) calculating a theoretical diffraction diagram or theoretical energy-dispersive spectrum; (c) fitting the theoretical diffraction diagram or theoretical energy-dispersive spectrum. In step (a), a list is predetermined which is composed of phases that are actually contained in the powder sample and also phases that are possibly not contained in the powder sample, a threshold value for the phase content is predetermined for each phase, and the following further steps are carried out: (d) elimination of all phases, having phase contents which are below the threshold value, from the list in step (a); (e) repeating steps (b), (c) and (d) with the new list until all phase contents are above their predetermined threshold values; and (f) outputting the composition of the powder sample. This method permits automatic exclusion of amorphous or crystalline phases with phase contents below a user-definable threshold value in profile adjustment methods based on Rietveld or Pawley methods.
1. A method for automatic determination of a quantitative composition of a powder sample, having different phase contents of crystalline and/or amorphous phases, from a diffraction diagram recorded by diffractometry from the powder sample or from an energy-dispersive spectrum, the method comprising the steps of:
a) predetermining a list of phases which are to be allocated to the phase contents in the powder sample, the predetermined list comprising phases that are actually contained in the powder sample as well as phases that may not be contained in the powder sample, wherein a threshold phase content value is set for each phase;
b) calculating a theoretical diffraction diagram or theoretical energy-dispersive spectrum based on the phases predetermined in the list of step a);
c) fitting the theoretical diffraction diagram or theoretical energy-dispersive spectrum to that of a recorded powder sample by variation of the phase contents of the theoretical diffraction diagram or theoretical energy-dispersive spectrum;
d) eliminating all phases having phase contents which are below the threshold value from the list of step a), thereby generating a new list;
e) repeating steps b), c) and d) until all phase contents are above predetermined threshold values thereof; and
f) outputting the composition of the powder sample with remaining phases and associated phase contents thereof.
2. The method of claim 1 , wherein a same global threshold phase content value is set for each phase.
3. The method of claim 1 , wherein individual threshold phase content values are set for each phase.
4. The method of claim 3 , wherein the threshold phase content values are predetermined for each phase in dependence on a proof limit or noise threshold of a measuring method that is used.
5. The method of claim 1 , wherein a profile adjustment method based on individual reflexes is used in step c).
6. The method of claim 1 , wherein a profile adjustment method based on a Pawley method is used in step c).
7. The method of claim 1 , wherein a profile adjustment method based on a LeBail method is used in step c).
8. The method of claim 1 , wherein a profile adjustment method based on a Rietveld method is used in step c).
9. The method of claim 1 , wherein the diffraction diagram or energy-dispersive spectrum is recorded by means of X-ray, neutron or electron diffractometry.
10. Use of the method of claim 1 for quality control or for online quality control.