• Applied Chemistry for Engineering
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• v.30 no.6
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• pp.749-756
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• 2019

Na-X and Na-A zeolites that give high adsorption capacity for heavy metals in an aqueous system were synthesized from the coal fly ash obtained from a thermoelectric power plant using a fusion method. The characteristics and Cu(II) adsorption capacity of the synthetic zeolites were also compared to those of using a commercial zeolite. For the selection of optimum conditions of zeolite synthesis, the effects of major parameters in the fusion method such as a dosage ratio of NaOH, aging time, hydrothermal reaction time, and also the dosage ratio of NaAlO₂ (Na-A) on the characteristics and Cu(II) adsorption capacity of the synthetic zeolites were studied. For the analysis of characteristics of the synthetic zeolites, X-ray diffraction (XRD), cation exchange capacity (CEC), Brunaue-Emmett-Teller (BET) and scanning electron microscopy (SEM) were used. The optimum conditions for the synthesis of zeolites with a high adsorption capacity for cationic heavy metals including Cu(II) were the aging time of 6 h, hydrothermal reaction time of 6 h and NaOH and NaAlO₂ dosage ratio of 1.5 and 0.5 (Na-A), respectively. According to the Langmuir isotherm test, maximum Cu(II) adsorption capacities of the synthetic and commercial Na-X and Na-A zeolites were found to be 90.1, 105.26, 102.05, and 109.89 mg/g, respectively. This indicates that the adsorption capacity of synthetic zeolites was comparable to commercial ones. The results of this study also suggest that the coal fly ash can be potentially used as a raw material for the zeolite synthesis.

• Journal of the Mineralogical Society of Korea
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• v.22 no.2
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• pp.139-151
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• 2009

Mineralogical characteristics of secondary precipitate formed at some mineral water springs in Gyeongbuk Province, Korea were studied in relation to water chemistry. The chemical water types of mineral water springs are mostly classified as $Ca-HCO_3$ type, but $Na(Ca)-HCO_3$ and $Ca-SO_4$ types are also recognized. Ca, Fe, and $HCO_3\;^-$ are the most abundant components in the water. The pH values of most springs lie in 5.76${\sim}$6.81, except Hwangsu spring having pH 2.8. Saturation indices show that all springs are supersaturated with respect to iron minerals and oxyhydroxides such as hematite and goethite. The result of particle size analysis shows that the precipitate is composed of the composite with various sizes, indicating the presence of iron minerals susceptible to a phase transition at varying water chemistry or the mixtures consisting of various mineral species. The particle size of the reddish precipitate is larger than that of the yellow brown precipitate. Based on XRD and SEM analyses, the precipitate is mostly composed of ferrihydrite (two-line type), goethite, schwertmannite, and calcite, with lesser silicates and manganese minerals. The most abundant mineral fanned at springs is ferrihydrite whose crystals are $0.1{\sim}2\;{\mu}m$ with an average of $0.5\;{\mu}m$ in size, characterized by a spherical form. It should be interestingly noted that schwertmannite forms at Hwangsu spring whose pH is very low. At Shinchon spring, Gallionella ferruginea, one of the iron bacteria, is commonly found as an indicator of the important microbial activity ascribed to the formation of iron minerals because very fine iron oxides with a spherical form are closely distributed on surfaces of the bacteria. A genetic relationship between the water chemistry and the formation of the secondary precipitate from mineral water springs was discussed.

• Economic and Environmental Geology
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• v.49 no.2
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• pp.77-88
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• 2016

Chrysotile is a 1:1 sheet silicate mineral belonging to serpentine group. It has been highlighted studies because of uses, shapes and structural characteristics of the fibrous chrysotile. However, it was designated as Class 1 carcinogen, so high attentions were being placed on detoxification studies of chrysotile. The objectives of this study were to investigate changes of mineralogical characteristics of chrysotile and to suggest detoxification mechanism of chrysotile by thermal decomposition. Samples for this study were obtained from LAB Chrysotile mine in Canada. The samples were heated in air in the range of 600 to $1,300^{\circ}C$. Changes of mineralogical characteristics such as crystal structure, shape, and chemical composition of the chrysotile fibers were examined by TG-DTA, XRD, FT-IR, TEM-EDS and SEM-EDS analyses. As a result of thermal decomposition, the fibrous chrysotile having hollow tube structure was dehydroxylated at $600-650^{\circ}C$ and transformed to disordered chrysotile by removal of OH at the octahedral sheet (MgOH) (Dehydroxylation 1). Upon increasing temperature, it was transformed to forsterite ($Mg_2SiO_4$) at $820^{\circ}C$ by rearrangement of Mg, Si and O (Dehydroxylation 2). In addition, crystal structure of forsterite had begun to transform at $800^{\circ}C$, and gradually grown 3-dimensionally to enstatite ($MgSiO_3$) by recrystallization after the heating above $1,100^{\circ}C$. And then finally transformed to spherical minerals. This study showed chrysotile structure was collapsed about $600-700^{\circ}C$ by dehydroxylation. And then the fibrous chrysotile was transformed to forsterite and enstatite, as non-hazardous minerals. Therefore, this study indicates heat treatment can be used to detoxification of chrysotile.

• Journal of the Mineralogical Society of Korea
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• v.16 no.4
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• pp.307-320
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• 2003

Garnet has been considered as a possible matrix for the immobilization of radioactive actinides. It is expected that Fe­based garnet be able to have the high substitution ability of actinide elements because ionic radius of Fe in tetrahedral site is larger than that of Si of Si­based garnet. Accordingly, we synthesized Fe­garnet with the batch composition of $Ca_{2,5}$C $e_{0.5}$Z $r_2$F $e_3$ $O_{12}$ and $Ca_2$CeZrFeF $e_3$ $O_{12}$ and studied their phase relations and properties. Mixed samples were fabricated in pellet forms under the pressure of 400 kg/$\textrm{cm}^2$ and were sintered in the temperature range of 1100∼140$0^{\circ}C$ in atmospheric conditions. Phase identification and chemical composition of synthesized samples were analyzed by XRD and SEM/EDS. In results, where the compounds were sintered at 130$0^{\circ}C$, we optimally obtained Fe­garnets as the main phase, even though some minor phases like perovskite were included. The compositions of Fe­garnets synthesized from the batch compositions of $Ca_{2,5}$C $e_{0.5}$Z $r_2$F $e_3$ $O_{12}$ and $Ca_2$CeZrFeF $e_3$ $O_{12}$, are $Ca_{2.5­3.2}$C $e_{0.3­0.7}$Z $r_{1.8­2.8}$F $e_{1.9­3.2}$ $O_{12}$ and $Ca_{2.2­2.5}$C $e_{0.8­1.0}$Z $r_{1.3­1.6}$ F $e_{0.4­.07}$ F $e_{3­3.2}$ $O_{12}$, respectively. Ca contents were exceeded and Ce contents were exceeded or depleted in 8­coodinated site, comparing to the initial batch composition. These results were caused by the compensation of the difference of ionic radius between Ca and Ce.

• Economic and Environmental Geology
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• v.43 no.4
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• pp.305-314
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• 2010

The stabilization process using limestone ($CaCO_3$) and steel making slag as the immobilization amendments was investigated for As contaminated farmland soils around Chonam abandoned mine, Korea. Batch and continuous column experiments were performed to quantify As-immobilization efficiency in soil and the analyses using XRD and SEM/EDS for secondary minerals precipitated in soil were also conducted to understand the mechanism of Asimmobilization by the amendments. For the batch experiment, with 3% of limestone and steel making slag, leaching concentration of As from the contaminated soil decreased by 62% and 52% respectively, compared to that without the amendment. When the mixed amendment (2% of limestone and 1% of steel making slag) was used, As concentration in the effluent solution decreased by 72%, showing that the mixed of limestone and steel making slag has a great capability to immobilize As in the soil. For the continuous column experiments without the amendment, As concentration from the effluent of the column ranged from 50 to $80\;{\mu}g/L$. However, with 2% limestone and 1% steel making slag, more than 80% diminution of As leaching concentration occurred within 1 year and maintained mostly below $10\;{\mu}g/L$. Results from XRD and SEM/EDS analysis for the secondary minerals created from the reaction of the amendments with $As^{+3}$ (arsenite) investigated that portlandite ($Ca(OH)_2$), calcium-arsenite (Ca-As-O) and calcite ($CaCO_3$) were main secondary minerals and the distinct As peaks in the EDS spectra of the secondary minerals can be observed. These findings suggest that the co-precipitation might be the major mechanisms to immobilize As in the soil medium with limestone and steel making slag.

• Journal of the Korean Chemical Society
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• v.33 no.5
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• pp.558-567
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• 1989

The synthesis of methanol from carbon dioxide and hydrogen was studied for various compositions of Cu/ZnO catalyst system. Effect of the composition ratio of CuO and ZnO on the catalytic activity in the above reaction and the relationship between the activity and the characteristics of the catalysts were explained from the result of surface area measurements, SEM, XRD, and XPS. The major products of the reaction were methanol and carbon monoxide. The selectivity to methanol increased with increase of the copper oxide content in the catalyst up to CuO: ZnO = 30:70 weight ratio, and decreased rapidly when the content is above 70%. SEM and BET measurements, indicate that this point corresponds to the increasing point of the catalyst crystallite size and the decreasing point of the surface area. As to the Cu/Cu + Zn atomic ratio, the surface concentration of copper measured by XPS decreased remarkably when the copper oxide content in catalyst was higher than 50%. All the unreduced catalysts had almost same binding energy of Cu(2P3) level, but the binding energy for $Cu(2P^3)$ level of reduced catalysts was lowered than that of calcined catalysts. The surface copper species which was in the maximum amount when the CuO:ZnO composition in the catalyst was 30:70, existed as zero valent copper. This result agreed with the experimental result that the highest rate of methanol formation was observed when the CuO content in the catalyst was 30%. It was postulated that these reduced catalysts performed with a relatively strong basicity because the formation rate of acetone was higher than that of propylene in isopropanol decomposition as measured in a pulse type reactor.

• Korean Chemical Engineering Research
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• v.50 no.2
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• pp.229-237
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• 2012

Phosphorus was incorporated into Co/$Al_2O_3$ catalyst for FTS by impregnating an acidic precursor, phosphoric acid, in ${\gamma}-Al_2O_3$ support to improve the mechanical strength, the hydrothermal stability of the catalyst particle, and the catalytic performance as well. Surface characterization techniques such as FT-IR revealed that $AlPO_4$ phase was generated on the surface of the P-modified catalyst. The addition of phosphorus was found to alleviate the interaction between cobalt and alumina surface, and to increase reducibility of catalyst. The catalytic activity such as $C_{5+}$ productivity and turnover frequency (TOF) was calculated to evaluate catalytic performance. The influence of calcination temperature of the $Al_2O_3$ containing 2 wt.% P on the catalytic performance was also investigated. Through hydrothermal stability test and XRD analysis, the P-modified catalyst had strong resistant to the pressurized and hot $H_2O$. The mechanical strength of the P-modified catalyst was also examined through an in-house fluidized-bed vessel, and it was found that the catalyst fragmentation could be successfully suppressed with P. Taken as a whole, the best performance was shown to be at 1~2 wt.% P in alumina and at the calcination temperature of $500^{\circ}C$.

• Journal of the Korean Magnetics Society
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• v.18 no.3
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• pp.109-114
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• 2008

The samples were synthesized by using a solid state reaction. The X-ray diffraction pattern for $Ti_{0.96}Co_{0.02}Fe_{0.02}O_2$ showed a pure rutile phase with tetragonal structure, Mixtures of the proper proportions of the elements sealed in evacuated quartz ampoule were heated at $870{\sim}930^{\circ}C$ for one day and then slowly cooled down to room temperature at a rate of $10^{\circ}C$/h. In order to obtain single phase material, it was necessary to grind the sample after the first firing and to press the powders into pellets before annealing them for a second time in evacuated and sealed quartz ampoule. Magnetic properties have been investigated using the vibrating sample magnetometer (VSM). Room temperature magnetic hysteresis (M-H) curve showed an obvious ferromagnetic behavior and the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $1.5\;{\mu}_B$/CoFe. But the magnetic moment per Fe atom under the applied of 0.8 T was estimated to be about $0.02\;{\mu}_B$/CoFe without Ti-getter. Size of particles is about $1\;{\mu}m$ using the transmission electron microscope (TEM). The ingredients of sample are distributed irregular in particles. Only Fe get shown on the surface of particles.

• Clean Technology
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• v.24 no.1
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• pp.77-84
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• 2018

In this study, $Li_4Ti_5O_{12}$ anode materials for lithium ion battery were synthesized by dry ball-mill method. Polyvinyl chloride (PVC) as a carbon source was added to improve electrochemical properties. When the PVC was added after $Li_4Ti_5O_{12}$ formation, the spinel structure was well synthesized and it was confirmed by X-ray diffraction (XRD) experiments. When the carbon material was added before the synthesis and the heat treatment was performed, it was confirmed that a material having a different crystal structure was synthesized even when a small amount of carbon material was added. In the case of $Li_4Ti_5O_{12}$ without the carbon material, the electrical conductivity value was about $10{\mu}S\;m^{-1}$, which was very small and similar to that of the nonconductor. As the carbon was added, the electrical conductivity was greatly improved and increased up to 10,000 times. Electrochemical impedance spectroscopy (EIS) analysis showed that the size of semicircle corresponding to the resistance decreased with the carbon addition. This indicates that the resistance inside the electrode is reduced. According to the Cyclic voltammetry (CV) analysis, the potential difference between the oxidation peak and the reduction peak was reduced with carbon addition. This means that the rate of lithium ion insertion and deinsertion was increased. $Li_4Ti_5O_{12}$ with 9.5 wt% PVC added sample showed the best properties in rate capabilities of $180mA\;h\;g^{-1}$ at 0.2 C-rate, $165mA\;h\;g^{-1}$ at 0.5 C-rate, and $95.8mA\;h\;g^{-1}$ at 5 C-rate.

• Journal of Korean Society of Environmental Engineers
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• v.33 no.11
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• pp.812-820
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• 2011

This study was conducted to characterize $CO_2$ biomineralization on several minerals (i.e., CaO, MgO, $SiO_2$) by bottle test in an aqueous solution and solidified sludge using different aerobic bacterial strains like Bacillus megaterium and Bacillus pasteurii by batch test. These bacteria promote the formation of microenvironments that facilitate the precipitation of mineral phases that were unsaturated in the bulk solution. For one type of mineral solely amended, the $CO_2$ was reduced at the highest of 4.0 mmol for MgO while it was not that much lower for CaO and $SiO_2$ showing 1.1 and 0.3 mmol $CO_2$2, respectively. For two types of minerals simultaneously amended, the $CO_2$ was reduced at the greater extent for both Ca + Mg and Mg + Si showing 2.7 and 2.3 mmol, respectively whereas it was less for Ca + Si at 1.8 mmol. For solidified sludge, the $CO_2$ reduction rate changed depending on the volume of solidified sludge placed in the medium and the input $CO_2$ concentration.. The reduction rate of $CO_2$ was increased with increasing the volume of solidified sludge. Results of XRD analysis indicate that $CaCO_3$ (Calcite) was dominantly formed among others (e.g., Aragonite, Dolomite). SEM analysis showed that the sample with Bacillus pasteurii, could more form minerals rather than control. As demonstrated in this study, $CO_2$ would be effectively sequestered in biomineralization process.