• Title/Summary/Keyword: rietveld analysis

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In-situ Phase Transition Study of Minerals using Micro-focusing Rotating-anode X-ray and 2-Dimensional Area Detector (집속 회전형 X-선원과 이차원 검출기를 이용한 광물의 실시간 상전이 연구)

  • Seoung, Dong-Hoon;Lee, Yong-Moon;Lee, Yong-Jae
    • Economic and Environmental Geology
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    • v.45 no.2
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    • pp.79-88
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    • 2012
  • The increased brightness and focused X-ray beams now available from laboratory X-ray sources facilitates a variety of powder diffraction experiments not practical using conventional in-house sources. Furthermore, the increased availability of 2-dimensional area detectors, along with implementation of improved software and customized sample environmental cells, makes possible new classes of in-situ and time-resolved diffraction experiments. These include phase transitions under variable pressure- and temperature conditions and ion-exchange reactions. Examples of in-situ and time-resolved studies which are presented here include: (1) time-resolved data to evaluate the kinetics and mechanism of ion exchange in mineral natrolite; (2) in-situ dehydration and thermal expansion behaviors of ion-exchanged natrolite; and (3) observations of the phases forming under controlled hydrostatic pressure conditions in ion-exchanged natrolite. Both the quantity and quality of the in-situ diffraction data are such to allow evaluation of the reaction pathway and Rietveld analysis on selected dataset. These laboratory-based in-situ studies will increase the predictability of the follow-up experiments at more specialized beamlines at the synchrotron.

Effect of Low-grade Limestone on Raw Mill Grinding and Cement Clinker Sintering (저품위 석회석이 원료밀의 분쇄성과 시멘트 클링커 소성성에 미치는 영향)

  • Yoo, Dong-Woo;Park, Tae-Gyun;Choi, Sang-Min;Lee, Chang-Hyun
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.9 no.1
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    • pp.20-25
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    • 2021
  • The cement clinker, the main raw material of cement, is manufactured using limestone as the main material. Depending on the quality of limestone, the use of subsidiary materials changes, and has a great influence on the production of cement clinkers. In this study, the effect of CaO content of limestone, a cement clinker material, on Raw Mill grinding and sintering of cement clinker was investigated. The grinding time of the union materials changed in the content of limestone CaO was measured to identify the grinding properties. The raw material combination was cleaned within a range of 1,350-1,500℃. The sintering performance of cement clinker by Burnability index calculation was identified. The lower the grade of limestone, the lower the grinding quality of the raw material combination. The lower the CaO content of limestone, the greater the variation in F-CaO for sintering temperature. The lower the class of limestone, the higher B. I. value was calculated, indicating the lower cement clinker sintering. In addition, the mineral analysis results of cement clinker showed that if the F-CaO value was low due to the increase in sintering temperature, the Belite content decreased and the Alite content increased. In the case of Alite, the ratio of R-type decreased and that of M-type increased as the content of limestone CaO increased.

Applied-Mineralogical Characterization and Assessment of Some Domestic Bentonites (I): Mineral Composition and Characteristics, Cation Exchange Properties, and Their Relationships (국내산 벤토나이트에 대한 응용광물학적 특성 평가 (I): 광물 조성 및 특징과 양이온 교환특성과의 연계성)

  • 노진환
    • Journal of the Mineralogical Society of Korea
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    • v.15 no.4
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    • pp.329-344
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    • 2002
  • Mineralogical and chemical characterization of some domestic bentonites, such as quantitative XRD analysis, chemical leaching experiments, pH and CEC determinations, were done without any separation procedures to understand their relationships among mineral composition, characteristics, and cation exchange properties. XRD quantification results based on Rietveld method reveal that the bentonites contain totally more than 25 wt% of impurities, such as zeolites, opal-CT, and feldspars, in addition to montmorillonite ranging 30~75 wt%. Cation exchange properties of the zeolitic bentonites are deeply affected by the content of zeolites identified as clinoptilolite-heulandite series. Clinoptilolite is common in the silicic bentonites with lighter color. and occurs closely in association with opal-CT. Ca is mostly the dominant exchangeable cation, but some zeolitic bentonites have K as a major exchangeable cation, The values of cation exchange capacity (CEC) determined by Methylene Blue method are comparatively low and have roughly a linear relationship with the montmorillonite content of the bentonite, though the correlated data tend to be rather dispersed. Compared to this, the CEC determined by Ammonium Acetate method, i.e.‘Total CEC’, has much higher values (50~115 meq/100 g). The differences between those CEC values are much greater in zeolitic bentonites, which obviously indicates the CEC increase affected by zeolite. Other impurities such as opal-CT and feldspars seem to affect insignificantly on the CEC of bentonites. When dispersed in distilled water, the pH of bentonites roughly tends to increase up to 9.3 with increasing the alkali abundance, especially Na, in exchangeable cation composition. However, some bentonites exhibit lower pH (5~6) so as to regard as ‘acid clay’. This may be due to the presence of $H^{+}$ in part as an exchangeable cation in the layer site of montmorillonite. All the works of this study ultimately suggest that an assesment of domestic bentonites in grade and quality should be accomplished through the quantitative XRD analysis and the ‘Total CEC’measurement.

Characterization of Synthesized Carbonate and Sulfate Green Rusts: Formation Mechanisms and Physicochemical Properties (합성된 탄산염 및 황산염 그린 러스트의 형성 메커니즘과 이화학적 특성 규명)

  • Lee, Seon Yong;Choi, Su-Yeon;Chang, Bongsu;Lee, Young Jae
    • Korean Journal of Mineralogy and Petrology
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    • v.35 no.2
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    • pp.111-123
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    • 2022
  • Carbonate green rust (CGR) and sulfate green rust (SGR) commonly occur in nature. In this study, CGR and SGR were synthesized through co-precipitation, and their formation mechanisms and physicochemical properties were investigated. X-ray diffraction (XRD) and Rietveld refinement showed both CGR and SGR with layered double hydroxide structure were successfully synthesized without any secondary phases under each synthetic condition. Refined structural parameters (unit cell) for two green rusts were a (=b) = 3.17 Å and c = 22.52 Å for CGR and a (=b) = 5.50 Å and c = 10.97 Å for SGR with the crystallite size 57.8 nm in diameter from (003) reflection and 40.1 nm from (001) reflections, respectively. Scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) results showed that both CGR and SGR had typical hexagonal plate-like crystal morphologies but their chemical composition is different in the content of C and S. In addition, Fourier transform infrared (FT-IR) spectroscopy analysis revealed that carbonate (CO32-) and sulfate (SO42-) molecules were occupied as interlayer anions of CGR and SGR, respectively. These SEM/EDS and FT-IR results were in good agreement with XRD results. Changes in the solution chemistry (i.e., pH, Eh and residual iron concentrations (Fe(II):Fe(III)) of the mixed solution) were observed as a function of the injection time of hydroxyl ion (OH-) into the iron solution. Three different stages were observed in the formation of both CGR and SGR; precursor, intermediator, and green rust in the formation of both CGR and SGR. This study provides co-precipitation methods for CGR and SGR in a way of the stable synthesis. In addition, our findings for the formation mechanisms of the two green rusts and their physicochemical properties will provide crucial information with researches and industrials in utilizing green rust.