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2 results for “Rietveld analysis”
Rietveld quantitative phase analysis of Oil Well Cement: in situ hydration study at 150 bars and 150ºC
<p>Raw data for: Rietveld Quantitative Phase Analysis of Oil Well Cement: In Situ Hydration Study at 150 Bars and 150 °C;</p> <p>doi: <a href="https://doi.org/10.3390/ma12121897">https://doi.org/10.3390/ma12121897</a></p> <p>Oil well cements are multimineral materials that hydrate under high pressure and temperature. Its overall reactivity at early ages is studied by a number of techniques including the consistometer. However, for a proper understanding of the performances of these cements in the field, the reactivity of every component, at the field conditions, must be analysed. So far, <em>in situ</em> high energy synchrotron powder diffraction studies of hydrating oil well cement pastes have been carried out but the quality of the data was not appropriated for Rietveld quantitative phase analyses. Therefore, the phase reactivities were followed by the inspection of the evolution of non-overlapped diffraction peaks. Very recently, we have developed a new cell specially designed to rotate under high pressure and temperature. Here, this spinning capillary cell is used to <em>in situ</em> study the hydration of a commercial oil well cement paste at 150 bars and 150 ºC. The powder diffraction data have been analysed by the Rietveld method to quantitatively determine the reactivities of each component phase. The reaction degree of alite was 90% after 7 hours and that of belite was 42% at 14 hours. These analyses are accurate as the <em>in situ</em> measured crystalline portlandite content at the end of the experiment, 12.9 wt%, compares relatively well with the value determined <em>ex situ</em> by thermal analysis, 14.0 wt%. The crystalline calcium silicates forming at 150 bars and 150 ºC are also discussed.</p>
Accuracy in Rietveld quantitative phase analysis with Mo and Cu strictly monochromatic radiations
<p><strong>Abstract </strong>This chapter is mainly based in the article entitled “Accuracy in Rietveld quantitative phase analysis: A comparative study of Mo and Cu strictly monochromatic radiations” by León-Reina et al., Journal of Applied Crystallography (2016). It reports Rietveld quantitative phase analyses using laboratory based Mo and Cu radiations where synchrotron powder diffraction (λ = 0.77439(2) Å) has been used to validate the most challenging analyses. From the results for three series with increasing contents of an analyte (inorganic crystalline phases, organic crystalline phases and a glass), it is inferred that Rietveld analyses from high-energy Mo-Kα<sub>1</sub> patterns have slightly better accuracies than those obtained from Cu-Kα<sub>1</sub> diffraction data. 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. We explain this outcome, in spite of the lower diffraction power for Mo-radiation when compared to Cu-radiation, due to the larger volume (and hence a larger number of crystallites) tested with Mo and also because higher energy allows the recording of patterns with fewer systematic errors. Limits of detection (LoD) and limits of quantification (LoQ) have also been established for the studied series. For similar recording times, LoDs in Cu-patterns, ~0.2 wt%, are slightly lower than those derived from Mo-patterns, ~0.3 wt%. LoQ for a well crystallised inorganic phase using laboratory powder diffraction was established close to 0.10 wt%, as stable fits were obtained. However, the accuracy of these analyses was very poor, with relative errors close to 100%. Only contents higher than 1.0 wt% yielded analyses with relative errors lower than 20%.</p>
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