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Two methods are described in the literature with which the amorphous proportion of a sample can be determined with the help of XRD:

Internal standard
By adding a known amount of a standard substance, it is possible to calibrate the total amount of the crystalline substance and thereby determine the amorphous proportion.

by evaluating the background halo
The crystalline intensity component and the total intensity are determined by adapting the course of the background. The difference between the two sum intensities depends on the amount of amorphous phases in the sample.

The contribution is in German.

Róisín Murtagh, Editor for Wiley Analytical Science Magazine, interviews Dr. Alfred Wasserman,
Owner and CEO of RMSKempten