Determination of amorphous matter in industrial minerals with X-ray diffraction using Rietveld refinement

A great variety of fine grained industrial rocks, which are valued by the industry contain variable amounts of amorphous or poorly crystalline matter, which is not easily detectable by the conventional mineralogical analysis methods based on X-ray diffraction (XRD). The quantification of amorphous matter in industrial rocks is a major task because it provides a thorough characterization of the raw materials and assists to interpret their reactivity. Among the most reliable methods used for quantification of amorphous matter, are those which are based on Rietveld refinement. In this study we prepared 1:1 mixtures of synthetic or natural calcite and quartz with 5-80% glass flour and added corundum (α-Al2O3) internal standard and applied the Autoquan2.80 © software based on the BGMN computer code to quantify the amorphous matter content. The mixtures with synthetic minerals yielded results with minimum absolute error due to the similar particle size of the minerals, the internal standard and the glass. By contrast, the mixtures with natural minerals displayed greater relative error due to the particle size difference between the minerals on the one hand and the internal standard and the glass on the other, due to the microabsorption effect. Moreover, preferred orientation was important in the case of natural calcite, due to perfect cleavage plane. Mixtures containing up to 25% amorphous matter did not display the characteristic hump at 20-30 °2θ, suggesting that the lack of the hump is not a safe criterion for the recognition of amorphous matter.