• Journal of Environmental Science International
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• v.29 no.12
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• pp.1261-1274
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• 2020

The characteristics of ammonia-nitrogen (NH4+-N) adsorption by a zeolitic material synthesized from Jeju scoria using the fusion and hydrothermal method was studied. The synthetic zeolitic material (Z-SA) was identified as a Na-A zeolite by X-ray diffraction, X-ray fluorescence analysis and scanning electron microscopy images. The adsorption of NH4+-N using Jeju scoria and different types of zeolite such as the Z-SA, natural zeolite, and commercial pure zeolite (Na-A zeolite, Z-CS) was compared. The equilibrium of NH4+-N adsorption was reached within 30 min for Z-SA and Z-CS, and after 60 min for Jeju scoria and natural zeolite. The adsorption capacity of NH4+-N increased with approaching to neutral when pH was in the range of 3-7, but decreased above 7. The removal efficiency of NH4+-N increased with increasing Z-SA dosage, however, its adsorption capacity decreased. For initial NH4+-N concentrations of 10-200 mg/L at pH 7, the adsorption rate of NH4+-N was well described by the pseudo second-order kinetic model than the pseudo first-order kinetic model. The adsorption isotherm was well fitted by the Langmuir model. The maximum uptake of NH4+-N obtained from the Langmuir model decreased in the order of Z-CS (46.8 mg/g) > Z-SA (31.3 mg/g) > natural zeolite (5.6 mg/g) > Jeju scoria (0.2 mg/g).

• Economic and Environmental Geology
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• v.52 no.6
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• pp.509-517
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• 2019

The birnessite (7Å manganate, δ-MnO₂) which is a manganese oxide and comprises manganese nodules, is a major manganese mineral on the earth surface and a precursor in the synthesis of todorokite. In this study birnessite was synthesized by three different methods: Feng et al. (2004) and Luo et al. (1998) based on redox reaction and Ma et al. (1999) based on reduction reaction. 12 birnessite samples were synthesized by different combinations of Na⁺ and K⁺ cations based on the base (OH^-) and permanganate (MnO₄^-) reagents in the synthesis. The mineral compositions of synthesized birnessite were identified by XRD, and the two cation ratio in the mineral was measured by ICP. The products obtained after hydrothermal treatment of Mg-buserite, by the precursor of birnessite, was examined by XRD, and then phase transition to todorokite and their characteristics were compared. Our results show that the byproducts and the characteristics of phase transition by each synthetic method have different trends. Hausmannite (γ-Mn₃O₄) and feitknechtite (β-MnOOH) were formed by both methods in the redox reaction mechanism. By Feng et al. (2004)'s method, manganite (γ-MnOOH) phase only appeared when cation was predominantly Na⁺. Two birnessite samples synthesized by redox reaction mechanism showed phase transition to todorokite (10Å manganate, OMS-1) when both NaOH and KMnO₄ were used together. However, single-phase birnessite was formed by Ma et al. (1999)'s method, and phase transition was confirmed only for the sample when the cation was only composed of Na⁺.

• Journal of the Mineralogical Society of Korea
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• v.19 no.1 s.47
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• pp.15-29
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• 2006

Synthetic Mn-tourmalines (tsilaisite) were obtained by hydrothermal synthesis under the condition of 2 Kbar, $375{\sim}700^{\circ}C$, and 50 day-run-time with complete substitution of Mg in dravite by Mn (Mn%=0, 25, 50, 75, and 100%). They are all 6 samples containing Mn-tourmaline with some amounts of albite, spessartine, rhodocrosite, phlogopite etc, showing different synthetic condition of temperature and Mn composition. Synthetic Mn-tourmalines are of site deficiency in X-site ($0.53{\sim}0.68$) more than that of natural ones (approx. $0.2{\sim}0.3$) and show Mn cations occupying Y-site less than expected with initial experiments, leading to failure in synthesis of end-member tsilaisite. Rietveld structural refinements reveal that $R_{wp}$ ($R_{p}/R_{exp}$) is in the range of 13.35 and 18.62%, $R_{B}$ and S (CofF) are $4.85{\sim}6.25%$ (S-18: 8.57%), $1.31{\sim}1.59$ (S-18: 1.81), respectively. Unit cell parameters (space group R3m, z=3) are ${\alpha}=15.8994\;{\AA}$ and $c=7.1846\;{\AA}$ in average (S-18: ${\alpha}=15.9491\;{\AA},\;c=7.1773\;{\AA}$). Average bond lengths of and are $2.67{\sim}2.69\;{\AA}$ (S-18: $2.65\;{\AA}$) and $2.00{\sim}2.02\;{\AA}$ (S-18: $1.96\;{\AA}$), respectively. Ditrigonality (${\delta}$) are in the range of 0.022 and 0.031 (S-18: 0.061), indicating degrading symmetry with increase of Mn content.

• Journal of the Mineralogical Society of Korea
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• v.22 no.3
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• pp.241-248
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• 2009

Kaolinite was synthesized from amorphous $SiO_2$ and $Al(OH)_3{\cdot}xH_{2}O$ as starting materials by hydrothermal reaction conducted at $250^{\circ}C$ and $30\;kg/cm^2$. The acidity of the solution was adjusted at pH 2. The synthesized kaolinite was characterized by XRD, IR, NMR, FE-SEM, TEM and EDS to clarify the formational process according to the reaction time from 2 to 36 hours. X-ray diffraction patterns showed after 2 h of reaction time, the starting material amorphous $Al(OH)_3{\cdot}xH_{2}O$ transformed to boehmite (AlOOH) and after the reaction time 5 h, the peaks of boehmite were observed to be absent thereby indicating the crystal structure is partially destructed. Kaolinite formation was identified in the product obtained after 10 h of reaction and the peak intensity of kaolinite increased further with reaction time. The results of TGA and DTA revealed that the principal feature of kaolinite trace are well resolved. TGA results showed 13 wt% amount of weight loss and DTA analysis showed that exothermic peak of boehmite observed at $258^{\circ}C$ was decreased gradually and after 10 h of reaction time, it was disappeared. After 5 h of the reaction time, the exothermicpeak of transformation to spinel phase was observed and the peak intensiy increased with reaction time. The results of FT-IR suggested a highly ordered kaolinite was obtained after 36 hours of reaction. It was identified by the characteristic hydroxide group bands positioned at 3,696, 3670, 3653 and $3620\;cm^{-1}$. The development of the hydroxyl stretching between 3696 and $3620\;cm^{-1}$, depends on the degree of order and crystalline perfection. TEM results showed that after 15 h reaction time, curved platy kaolinite was observed as growing of (001) plane and after 36 h, the morphology of synthetic kaolinite exhibited platy crystal with partial polygonal outlines.

• The Journal of the Petrological Society of Korea
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• v.6 no.2
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• pp.123-132
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• 1997

In the system $MgO-SiO_2-H_2O$, Talc[$Mg_3Si_4O_{10}(OH)_2$] has been synthesized hydrothermally at 200 MPa, $600^{\circ}C$ from the oxide mixture of the bulk composition of talc. The oxide mixture of the bulk composition of anthophyllite$[Mg_7Si_8O_{22}(OH)2]$ converted to talc, enstatite $(MgSiO_3)$, quartz at 200 MPa, $750^{\circ}C$ with excess of $H_2O$. In low to medium pressure metramorphism, enstatite-talc assemblage is metastable relative to anthophyllite with the reaction talc + 4 enstatite=anthophyllite (Greenwood, 1963). The high temperature stability of talc is bounded with the dehydration reaction to anthophyllite rather than that to enstatite(Greenwood, 1963; Chernosky et al., 1985). Therefore our experiment result assemblage, enstatite-talc-quatz at 200 MPa, $750^{\circ}C$ from oxide mixture of bulk compostion of anthophyllite is metastable assemblage. The hydrothermal experiment performed at 41 to 243 MPa, 680 to $760^{\circ}C$ with the starting material composed of synthetic talc, enstatite and quartz. Talc or enstatite grows during the runs and no extra phases including anthophyllite nucleated. Based on the increase or decrease of the each phase from run products, one of the possible reactions is talc=3 enstatite+quartz+H_2O$. The reversal bracket of the reaction is 699 to $700^{\circ}C$ at 100 MPa. Talc is stable up to $740^{\circ}C$ at 200 MPa and enstatite grow at $680^{\circ}C$, 40 MPa and at $760^{\circ}C$, 250 MPa. Though the high temperature limit of talc around 200 MPa is bounded thermodynamically by the reaction, 7 talc=3 anthophyllite+4 quartz+4 H_2O$, talc persisted throughout the previous reaction up to the reaction, talc=3 enstatite+quartz+$H_2O$.

• Journal of the Mineralogical Society of Korea
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• v.21 no.4
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• pp.341-347
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• 2008

The feasibility of commercializing the hydrothermal synthesis of Na-A type zeolite from siliceous mudstone has been conducted using a 50-liter bench-scale autoclave and the application of the zeolite as an environmental remediation agent. Siliceous mudstone, which is widely distributed around the Pohang area, was adopted as a precursor. The siliceous mudstone is favorable for the synthesis of zeolite because it contains 70.7% $SiO_2$ and 10.0% $Al_2O_3$, which are major ingredient of zeolite formation. The synthesis of zeolite was carried out under the following conditions that had been obtained from the previous laboratory-scale tests: 10hr reaction time, $80^{\circ}C$ reaction temperature, $Na_2O/SiO_2$ ratio = 0.6, $SiO_2/Al_2O_3$ ratio = 2.0 and $H_2O/Na_2O$ ratio= 98.6. The crystallinity and morphology of the zeolite formed were similar to those obtained from the laboratory-scale tests. The recovery and cation exchange ion capacity were 95% and 215 cmol/kg, respectively, which are slightly higher than those obtained in laboratory scale tests. To examine the feasibility of the zeolite as an environmental remediation agent, experiments for heavy metal adsorption to zeolite were conducted. Its removal efficiencies of heavy metals in simulated waste solutions decreased in the following sequences: Pb > Cd > Cu = Zn > Mn. In a solution of 1500 mg/L total impurity metals, the removal efficiencies for these impurity metals were near completion (> 99%) except for Mn whose efficiency was 98%. Therefore, the synthetic Na-A type zeolite was proven to be a strong absorbent effective for removing heavy metals.

• Clean Technology
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• v.25 no.4
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• pp.331-335
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• 2019

Interest in environmental pollution is increasing all over the world, and technology development to solve it is actively carried out. In areas where heat is used, especially, combustion is causing countless pollutants in the air environment. Combustion catalyst is a technology that reduces NOx and CO by lowering combustion temperature and enabling complete combustion. Traditional combustion catalysts are expensive and complex in the synthesis process using precious metal catalyst. In this study, hexaaluminate, a high-temperature combustion catalyst, was manufactured using urea, and the properties were investigated according to the synthesis time. The combustion performance and characteristics were evaluated using this catalyst. As the temperature increased, the changing methane conversion rate was shown in two patterns. The conversion rates for 1 hour, 9 hours, and 12 hours were similar, while the conversion rates for 3 hours and 6 hours showed similar patterns. Methane combustion performance increased rapidly as the synthesis time increased from 6 hours to 9 hours, whereas the temperature at T50 was approximately 745 ℃. The performance of the synthesized combustion catalyst for 9 hours was optimum as the NOx emission of this combustion catalyst was not present and the maximum emission of CO was 72 ppm.

• Journal of the Mineralogical Society of Korea
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• v.21 no.3
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• pp.283-287
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• 2008

The imogolite synthesis wore performed by using tetraethoxysilane (TEOS) and aluminium-sec-butoxide (ASB) at < $100^{\circ}C$. A mixure of TEOS and ASB in a molar ratio of 1:2 was prepared under vigorous stirring and the experiments were performed under the hydrothemal refluxing condition. When the concentration of TEOS and ASB in solution was 0.5 M, a well-crystallized imogolite was synthesized, and the reflections wore shown at d = 22.4, $9.5\;\AA$ etc., after XRD analysis. DTA analysis shows 2 exothemal peaks at 68 and $249^{\circ}C$, suggesting the dehydration and the dehyroxylation reaction, respectively. The result of TG indicates 41% weight loss. And the weak and unsymmetrical peaks by the Si-O-Al stretching vibrations at 953 and $993cm^{-1}$ and by O-Si-O bending vibration at $562cm^{-1}$ were observed after IR analysis. The synthetic imogolite was fibrous and shows a spiders web like network structure.

• Journal of the Korean Chemical Society
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• v.46 no.6
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• pp.515-522
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• 2002

Solid beta-dicalcium silicate hydrate $(\beta-C_2SH)$ synthesized under hydrothermal conditions at $240^{\circ}C$ and Ca/Si=2 molar ratio shows cation exchange properties towards divalent metal cations such as Fe, Cu, Zn, Cd, or Pb. The ability of metal cation uptake by the solid was found to be in the order: $Fe^{2+}$〉$Cu^{2+}$〉$Zn^{2+}$〉$Cd^{2+}$ = $Pb^{2+}$. Cesium selectivity of the solid was demonstrated in the presence of univalent cation such as $Li^+$, $Na^+$ and $K^+$ and divalent cations such as $Ca^{2+}$, $Mg^{2+}$ and $Ba^{2+}$, which are one hundred times more concentrated than the $Cs^+$. The uptake of $Cs^+$ is maximum in the presence of $Mg^{2+}$ whereas it is minimum in the presence of $K^+$. The different affinities of ${\beta}-C_2SH$ towards divalent metal cations can be used for the separation of those ions. Due to its selectivity for cesium it can be used in partitioning of radioactive Cs+ from nuclear wastes containing numerous cations. The mechanism of the metal cation exchange and cesium selectivity reactions by the solid is studied.

• Journal of the Mineralogical Society of Korea
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• v.2 no.2
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• pp.90-99
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• 1989

Manganese deposits ar the Dongnam mine occur as vein in the Pungchon limestone of Ordovician age. Manganese ore veins consist of the hydrothermal manganese carbonate ores in the deeper part and the supergene manganese oxide ores in the shallow part. Manganese carbonate ores consist mainly of rhodochrosite, with minor amount of proxmangite, garnet, calcite, quartz, pyrite, galena and sphalerite. Manganese oxide ores consist of rancieite, buserite, birnessite, vernadite, todorokite, pydrolusite, nsutite, hydrohetaerosite and goethite. Manganese oxide minerals were formed in the following sequences; 1) rhodochrosite ${\rightarrow}$ vernadite ${\rightarrow}$ birnessite ${\rightarrow}$ nsutite ${\rightarrow}$ pyrolusite, 2) pyroxmangite ${\rightarrow}$ birnessite, 3) Buserite ${\rightarrow}$ ransieite. Todorokite, buserite and hydrohetaerolite were precipitated from solution in the later stage. The natural analogue of synthetic buserite has been discovered from the mine. It has been disclosed that buserite transforms to rancicite by dehydration, and that distinction between buserite and todorokite is possible by X-ray diffraction studies combined with dehydration experiment. Minerals identified from the mine have been characterized using various methods including polarizing microscopy, X-ray diffraction, thermal analysis, infrared spectroscopy, X-ray diffraction, thermal analysis, infrared spectroscopy, elecrton microscopy and dehydration experiment.