• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.564-573
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• 2022

Calcium carbonate (CaCO₃) exhibits three polymorphs: calcite with arhombohedral, vaterite with a spherical, and aragonite with a needle-like structure. Qualitative and quantitative analyses of the morphology of CaCO₃ are very important to investigate the synthesis of single-crystal vaterite and aragonite. In this work, the polymorphs of calcium carbonate were quantitatively analyzed using XRD. Pure vaterite and pure aragonite were synthesized and the peak distribution of a single phase was analyzed. The vaterite fraction of a mixture of calcite and vaterite was calculated based on the intensity of a specific diffraction peak, and compared to the results based on the peak area. The mean value of f_sV (the correction factor for the peak area of vaterite) was 0.654. The phase analysis of calcite-aragonite mixtures was performed, and the mean value of f_sA (the correction factor for the peak area of aragonite) was obtained as 0.6713. Using these factors, Eq. (24)~Eq. (32) for the quantitative analysis based on the total peak area of XRD were derived to calculate the phase contents of ternary phase CaCO₃. And three-component XRD section was defined considering overlapping sections.

• Proceedings of the Computational Structural Engineering Institute Conference
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• 2010.04a
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• pp.770-772
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• 2010

기존의 연구는 열화에 의한 물리적 평가 및 열화에 영향을 미치는 수화생성물의 존재여부에 대한 연구는 활발하게 이루어지고 있으나, 그에 따른 수화생성물의 정량화에 대한 연구는 미흡한 실정이다. 본 논문은 XRD 분석 기법을 이용하여 원전 콘크리트 구조물에 대해 열화요인 중 탄산화와 황산염에 대한 상대적 정량화에 대한 연구를 실시하였다. 두 열화인자는 콘크리트 내의 수산화칼슘과 반응하여 에트린가이트와 탄산칼슘을 생성하게 되는데, 본 연구에서 열화인자에 대한 노출기간이 증가할수록 열화에 영향을 미치는 수화 생성물이 증가하는 것을 확인 할 수 있었다. 그에 따른 수산화칼슘의 양이 감소하는 것도 확인 할 수 있었다.

• Journal of the Mineralogical Society of Korea
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• v.5 no.1
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• pp.32-41
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• 1992

An XRD quantitative analytical method using calculated XRD patterns was discussed in this study, Deep-seabed sediments commonly contain smectite, illite, chlorite, and kaolinite, and XRD pattern of each clay mineral of appropriate chemical composition was simulated by using an XRD pattern calculation method. Theoretical peak intensities of specific reflections of four clay minerals (the 001 reflections of smectite and illite, the 004 reflection of chlorite, and the 002 reflection of kaolinite) were measured from calculated patterns, and MIF(mineral intensity factor)value of each phase was determined from the intensities of calculated patterns. The peak intensities obtaine from experimental XRD patterns of sediments were corrected using the MIF values so that the calibrated intensity values for the specimens are linearly proportional to the weight fraction of each phase, which is normalized to 100 wt%. The MIF method can provide accurate quantitaive results without the necessity of correcting the factors by the mass absorption coefficient of each phase. This method excludes the necessity of standard specimens having compositions that are similar to those of clay minerals in the sediment samples. Therefore, quantitaive analysis using XRD calculation method can be utilized for the specimens, for which the standard specimens are very difficult or impossible to obtain. this quantitative method can provide rapid, routine analysis results for a large number of samples which occur in similar geological environments.

• Cement
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• s.126
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• pp.65-71
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• 1992

• Journal of the Korean Ceramic Society
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• v.40 no.5
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• pp.481-487
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• 2003

A technique for determination of proportions of char, coal ana coke is needed in order to monitor pulverized coal injection performance in operating blast furnace. Quantitative X-ray powder diffraction analysis can be applied to the problem providing that structural information on carbonaceous materials, coal, char, coke and their mixture are known. Chars were prepared from a coal at different temperatures (1000∼1400$^{\circ}C$) and were characterised by X-Ray powder Diffraction (XRD). The XRD result gave crystallite size (height Lc and diameter, La), aromaticity, number of (002) plane in carbon, and d-spacing. As a result, with increasing heat treat temperature of char, Lc$_{(002)}$, La$_{(10)}$ and number of (002) plane in carbon were increased, and d-spacing and FWHM(Full With Half Maximum) were decreased. Result of prediction of amount of char from the mixtures (char, coke and ore) based on the Lc$_{(002)}$ information of two mixtures (coke and char) showed very close values expected.

• Proceedings of the Korean Ceranic Society Conference
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• 2002.10a
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• pp.130.1-130
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• 2002

• Cement
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• s.158
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• pp.27-33
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• 2003

• Cement Symposium
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• no.20
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• pp.49-57
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• 1992

• Journal of the Mineralogical Society of Korea
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• v.7 no.1
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• pp.62-79
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• 1994

The quanttative and structural analysis of the binary standard mixtures of albite and quartz, and microcline and albite were carried out using the Rietveld refinement method in order to investigate the accuracy and precision of the method. The quantitative analysis using the Rietveld method results in a standard deviation of 4 wt % for the albite-quartz standard mixtures and 1 wt % for the microcline-albite standard mixtures, suggesting that its accuracy is far better than that of the conventional XRD method in which only a few selected peaks are utilized. Furthermore, the unit-cell parameters of component minerals in mixtures were also estimated accurately during the analysis. It was observed that the refined weight fractions deviate systematically from their measured values when the method is applied to the mixtures that contain minerals with different degrees of preferred orientation, such as albite-quartz mixtures. The preferred orientation parameters and R-values suggest that the systematic deviation is caused as a result of the preferred orientation effect of feldspar crystallites. It is evident that the preferred orientation corrections are of help for the accurate determination of unit-cell parameters, although they may not improve the result of quantitative analysis significantly. The refined weight fraction of the mineral with higher degree of preferred orientation in mixture is greater than the measured one. This is apparently caused by the effect of geometry of feldspar crystallites in the surface of the mounted sample. The Rietveld refinement method minimizes the problems inherent in the traditional XRD methods, such as the line overlap, primary extinction, and preferred orientation effect, by fitting every data point in a whole pattern explicitly. Furthermore, accurate unit-cell parameters as well as scale factors that can be obtained from the Rietveld refinement are used for the quqantification. The present stdudy demonstrates that the Rietveld method yields far more accurate analytical result than the conventional XRD quantitative analysis method does.

• Analytical Science and Technology
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• v.25 no.1
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• pp.33-38
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• 2012

Despite the importance of chloride binding, it is very difficult to measure the binding capacity, in particular, for the concrete body in an existing structure: in fact, the measurement procedure for chloride binding is much influenced by the environmental condition such as temperature, fineness of sample and pore water extraction techniques. The present study concerns the quantification of the binding capacity of chloride ions in concrete using the X-ray diffraction (XRD) technique. Once the binding isotherm of chlorides was determined by the Langmuir isotherm, as a function of the W/C, curing age and binder type, the generation of bound chlorides (i.e. Friedel's salt) was simultaneously ensured by the XRD technique. The amount of bound chloride was then determined by analyzing the peak intensity for the bound chlorides in the XRD curve. It was found that an increase in the curing age and a decrease in the W/C resulted in an increase in the binding capacity.