Accuracy in Rietveld quantitative phase analysis of Portland cements

Abstract

The polymorphs that constitute most Portland cements have been synthesized: tricalcium silicate, dicalcium silicate, aluminate, ferrite, gypsum, bassanite and calcite. They have been used to prepare artificial mixtures,i.e.white Portland clinker, grey Portland clinker and two types of grey Portland cements. Quantitative mineralogical analyses of these mixtures have been obtained by laboratory X-ray powder diffraction (λ = 1.54 Å) and the Rietveld method. To assess the accuracy of these analyses, high-energy synchrotron X-ray powder data (λ = 0.40 Å) for the same mixtures have also been studied. Furthermore, synchrotron X-ray powder data were collected for binary mixtures of the polymorphs and a corundum standard. This was done to determine the presence of impurity crystalline phases in the synthesized samples and to check the presence of non-negligible amorphous phase contents. The errors in the synchrotron X-ray analyses are quite low (usually smaller than 1 wt%). The relative errors in the laboratory X-ray analyses are of the order of 2% for the main phases and increase to approximately 5–10% for the low-content components. These errors are acceptable in the factory environment and the routine application of this methodology in the cement industry is being implemented.