Accuracy in Rietveld quantitative phase analysis of Portland cements

Accuracy in Rietveld quantitative phase analysis of Portland cements
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DOI:
10.1107/s002188980301375x
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发表时间:
2003-10-01
影响因子:
6.1
通讯作者:
Aranda, MAG
Aranda, MAG
中科院分区:
材料科学3区
文献类型:
--
作者:
De la Torre, AG;Aranda, MAG

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合成了构成大多数硅酸盐水泥的多晶型:硅酸三钙、硅酸氢钙、铝酸盐、铁酸盐、石膏、钠长石和方解石。它们已被用于制备人工混合料,即白色波特兰熟料、灰色波特兰熟料和两种灰色波特兰水泥。用实验室X射线粉末衍射法(波长1.54埃)和Rietveld法获得了这些混合物的定量矿物学分析。为了评估这些分析的准确性,还研究了相同混合物的高能同步辐射X射线粉末数据(波长=0.40埃)。此外,还收集了多晶型和刚玉标准的二元混合物的同步辐射X射线粉末数据。这样做是为了确定合成样品中是否存在杂质晶相,并检查是否存在不可忽略的非晶相含量。同步加速器X射线分析的误差很低(通常小于1wt%)。在实验室X射线分析中,主相的相对误差约为2%,低含量组分的相对误差约为5%-10%。这些错误在工厂环境中是可以接受的,这种方法在水泥行业的常规应用正在实施中。
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 (lambda = 1.54 Angstrom) and the Rietveld method. To assess the accuracy of these analyses, high-energy synchrotron X-ray powder data (lambda = 0.40 Angstrom) 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.