Accuracy in Rietveld quantitative phase analysis: a comparative study of strictly monochromatic Mo and Cu radiations.

This study reports 78 Rietveld quantitative phase analyses using Cu Kα1, Mo Kα1 and synchrotron radiations. Synchrotron powder diffraction has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (an inorganic crystalline phase, an organic crystalline phase and a glass), it is inferred that Rietveld analyses from high-energy Mo Kα1 radiation have slightly better accuracies than those obtained from Cu Kα1 radiation. This behaviour has been established from the results of the calibration graphics obtained through the spiking method and also from Kullback-Leibler distance statistic studies. This outcome is explained, in spite of the lower diffraction power for Mo radiation when compared to Cu radiation, as arising because of the larger volume tested with Mo and also because higher energy allows one to record patterns with fewer systematic errors. The limit of detection (LoD) and limit of quantification (LoQ) have also been established for the studied series. For similar recording times, the LoDs in Cu patterns, ∼0.2 wt%, are slightly lower than those derived from Mo patterns, ∼0.3 wt%. The LoQ for a well crystallized inorganic phase using laboratory powder diffraction was established to be close to 0.10 wt% in stable fits with good precision. However, the accuracy of these analyses was poor with relative errors near to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.

Active iron-rich belite sulfoaluminate cements: clinkering and hydration.

Ordinary Portland cement (OPC) is an environmentally contentious material, as for every ton of OPC produced, on average, 0.97 tons of CO2 are released. Conversely, belite sulfoaluminate (BSA) cements are promising eco-friendly building materials, as their production may deplete CO2 emissions up to 35% (compared to OPC). However, the hydration rate of belite is slow. Here, we report the clinkering of iron-rich BSA materials, their activation with B2O3, and establishing a methodology to measure their improved reactivities. Nonactivated BSA clinker contained only beta belite phase, 52 wt %. Meanwhile, BSA clinkers activated with 1 and 2 wt % of B2O3 contained 28 wt % of beta and 25 wt % of alpha'H; and 54 wt % of alpha'H phase, respectively. Therefore, activation of BSA has been proved as alpha'H-belite is stabilized. The hydration of the cements has been studied by laboratory and synchrotron X-ray powder diffraction (using Rietveld method and chemical constraints), calorimetry, and environmental scanning electron microscopy. Cement pastes have different hydration rates. For nonactivated BSA cement, 20 and 48% of the belite reacted after one and three months, respectively. Conversely, 37-49% after one month and 52-62% after three months of overall belite reactivities have been measured for BSA cements activated with B2O3.