• Korean Journal of Mineralogy and Petrology
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• v.35 no.4
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• pp.431-445
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• 2022

A quantitative phase analysis method of X-ray powder diffraction was studied to determine the mineral content of clay-rich rocks practically as well as effectively. For quantitative X-ray powder diffraction analysis of the clay-rich rocks, it is necessary to prepare whole-rock powder samples with a random orientation by side mounting method. In addition, for the identification of the clay minerals in the rock, it is required to prepare an oriented mount specimen with a clay particle size of 2 ㎛ or less, ethylene glycol treatment, and heat treatment. RIR (reference intensity ratio) and Rietveld method were used for the quantitative analysis of the clay-rich rocks. It was possible to obtain the total clay and the non-clay minerals contents from the whole-rock X-ray diffraction profiles using the RIR values. In addition, it was possible to calculate the relative content of each clay mineral from the oriented X-ray diffraction profiles of the clay particle size and assign it to the total clay. In the Rietveld method of whole-rock X-ray diffraction, effective quantitative values were obtained from the Rietveld diffraction patterns excluded the region of less than 10 degrees (2θ). Similar quantitative values were shown in not only the RIR but the Rietveld methods. Therefore, the analysis results indicate a possibility of a routine quantitative analysis of clay-rich rocks in the laboratory. However, quantitative analysis of clay minerals is still a challenge because there are numerous varieties of clay minerals with different chemical and structural characteristics.

• Korean Journal of Mineralogy and Petrology
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• v.34 no.4
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• pp.227-239
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• 2021

A practical and effective method of X-ray powder diffraction analysis was investigated for quantitative analysis of the mineral content of natural samples. Sample mounting experiments were conducted to select the best randomly oriented powder sample mount. A comparative experiment was also made between a reference intensity ratio (RIR) method, which compares a single peak intensity with standard material, and the Rietveld method, which calculates a full X-ray diffraction pattern, to search for the effective method of mineral quantification. In addition, samples containing amorphous minerals were quantitatively analyzed by the Rietveld method and the efficiency was reviewed. As a result of the study, the optimal random orientation could be reached by the side mounting method. The Rietveld method using the full pattern of X-ray diffraction was more suitable for mineral quantitative analysis, rather than the RIR method using a specific peak. However, either method could depend on the analyst's experience in addition to analytical technique. Moreover, amorphous minerals can be quantitatively analyzed by the Rietveld method, and the analysis results make the geological analysis possible.

• Economic and Environmental Geology
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• v.49 no.5
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• pp.349-360
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• 2016

This study determined mineralogical characteristics and discussed the meaning of mineralogical changes of the lower Choseon Supergrouop in the Weondong area based on the field geological investigation and the drilling core description using X-ray diffraction (XRD) mineral quantification and Scanning Electron Microscopy (SEM) observation. 100 samples with depth were collected from the core (250 m long) at a site in the study area. Especially, to investigate the changes from the upper Daegi Formation to the lower Hwajeol Formation, the samples were collected closely with the interval of about 0.3 m at this section. All samples were made into power using mortar for XRD. Mineral quantitative analysis was executed using Relative Intensity Ratio (RIR) method with corundum as an internal standard phase. Calcite, $2M_1$ illite and quartz are main constituents in most of samples. Dolomite and siderite are significantly observed in the Sesong Formation. As the results of quantitative analysis for the major minerals, the upper Daegi Formation is dominated by calcite with over 80%. The Sesong Formation includes high percentage of dolomite and siderite with the intercalation of thin layers containing high calcite and $2M_1$ illite contents. Hwajeol Formation is characterized by the alternation between thin layers of $2M_1$ illite and quartz-dominated layer (IQDL) and calcite-dominated layer (CDL). IQDL is more frequent in the lower part, whereas CDL is more common in the upper part. The boundary between Daegi Formation and the Sesong Formation is distinct, whereas the boundary between the Sesong Formation and the Hwajeol Formation tends to be changed gradually in mineralogy. The result of SEM observation shows that quartz and $2M_1$ illite are detrital, and a significant amount of calcite also shows detrital form with some recrystallized one, indicating that the repeated influx of terrestrial materials had changed the mineralogy of the shallow sea depositional environment in the early Paleozoic era.