• Korean Chemical Engineering Research
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• v.50 no.2
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• pp.251-256
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• 2012

Etherification of n-butanol to di-n-Butyl Ether was carried out over Keggin $H_{3+x}PW_{12-x}Nb_xO_{40}$ (x=0, 1, 2, 3) and $H_{6+x}P_2W_{18-x}Nb_xO_{62}$ (x=0, 1, 2, 3) Wells-Dawson heteropolyacid catalysts. Niobium-substituted Keggin and Wells-Dawson heteropolyacid catalysts with different niobium content were prepared. Successful preparation of the catalysts was confirmed by FT-IR, ICP-AES, and $^{31}P$ NMR analyses. Their acid properties were determined by $NH_3$-TPD (Temperature-Programmed Desorption) measurements. Heteropolyacid catalysts showed different acid properties depending on niobium content in both series. The correlation between acid properties of heteropolyacid catalysts and catalytic activity was then established. Acidity of Keggin and Wells-Dawson heteropolyacid catalysts decreased with increasing niobium content, and conversion of n-butanol and yield for di-n-butyl ether increased with increasing acidity of the catalysts, regardless of the identity of heteropolyacid catalysts (without heteropolyacid structural sensitivity). Thus, acidity of heteropolyacid catalysts served as an important factor determining the catalytic performance in the etherification of n-butanol to di-n-Butyl Ether.

• The Journal of the Petrological Society of Korea
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• v.20 no.3
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• pp.161-172
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• 2011

Open beaker digestion method is routinely used as the sample preparation technique for trace element determination of rock samples by inductively coupled plasma mass spectrometry, With this method, however, dissolution of Zr and Hf is not always guaranteed especially when the samples contain refractory minerals. In this study, glass bead digestion technique was compared with conventional open beaker digestion technique for the sample preparation of three USGS rock standards such as AGV-2, BHVO-2, and G-3. Thirty trace elements including rare earth elements were analysed by ICP-MS and ICP-AES. There were no clear differences in analytical results for the AGV-2 and BHVO-2 standards between the two techniques, but Zr, Hf, Y, and middle- to heavy- rare earth element concentrations of the G-3 standard prepared by open beaker digestion technique were significantly lower than the recommended values. This can be attributed to the presence of refractory mineral zircon. On the contrary, all the analytical results of the G-3 standard prepared by glass bead digestion technique were in good agreement with the recommended values, indicating complete dissolution of zircon. The analytical results show that the volatile elements such as Pb and Zn were not lost during the preparation of glass bead. Low dilution glass bead digestion technique described here will be very helpful to enhance precision and accuracy of trace element analysis for geological samples containing refractory minerals.

• Food Science and Preservation
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• v.24 no.8
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• pp.1094-1102
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• 2017

Hazardous metals leaching experiment was carried out in accordance with various usage environments for camping cooking utensils distributed in the market. There was a significant difference in the degree of migration for lead, arsenic, cadmium and nickel defending on the solvent and how to use, although they were all appropriate for criteria. In general, the migrated amount of aluminum was increased in acidic condition, and the migrated amount of arsenic was increased in salty condition. Physical scratches increased the overall release of hazardous metals from the portable pots and pans for camping in all solvents. Especially, in 0.5% citric acid solution, cadmium was migrated by physical scratch in stainless steel and hard aluminum pots and pans. The longer the leaching time, the higher the migration of aluminum in acid condition and arsenic in basic condition. From these results, it is desirable to use the cooking utensil for camping without being exposed to strong acidic or basic solution and scratches in order to reduce the migration of hazardous metals from them.

• The Journal of the Petrological Society of Korea
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• v.22 no.2
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• pp.137-151
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• 2013

This study is focused on element behaviors and mineral compositions of the fault rock developed in Yongdang-ri, Yangbuk-myeon, Gyeongju City, Korea, using XRF, ICP, XRD, and EPMA/BSE in order to better understand the chemical variations in fault rocks during the fault activity, with emphasis on dependence of chemical mobility on mineralogy across the fault zone. As one of the main components of the fault rocks, $SiO_2$ shows the highest content which ranges from 61.6 to 71.0%, and $Al_2O_3$ is also high as having the 10.8~15.8% range. Alkali elements such as $Na_2O$ and $K_2O$ are in the range of 0.22~4.63% and 2.02~4.89%, respectively, and $Fe_2O_3$ is 3.80~12.5%, indicating that there are significant variations within the fault rock. Based on the chemical characteristics in the fault rocks, it is evident that the fault gouge zone is depleted in $Na_2O$, $Al_2O_3$, $K_2O$, $SiO_2$, CaO, Ba and Sr, whereas enriched in $Fe_2O_3$, MgO, MnO, Zr, Hf and Rb relative to the fault breccia zone. Such chemical behaviors are closely related to the difference in the mineral compositions between breccia and gouge zones because the breccia zone consists of the rock-forming minerals including quartz and feldspar, whereas the gouge zone consists of abundant clay minerals such as illite and chlorite. The alteration of the primary minerals leading to the formation of the clay minerals in the fault zone was affected by the hydrothermal fluids involved in fault activity. Taking into account the fact that major, trace and rare earth elements were leached out from the precursor minerals, it is assumed that the element mobility was high during the first stage of the fault activity because the fracture zone is interpreted to have acted as a path of hydrothermal fluids. Moving toward the later stage of fault activity, the center of the fracture zone was transformed into the gouge zone during which the permeability in the fault zone gradually decreased with the formation of clay minerals. Consequently, elements were effectively constrained in the gouge zone mostly filled with authigenic minerals including clay minerals, characterized by the low element mobility.

• Korean Journal of Food Science and Technology
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• v.44 no.1
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• pp.21-27
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• 2012

This research was carried out as a survey on the contents of lead, cadmium, and arsenic in processed foods (milk, vegetable oil, and margarine) in Korea. The limits of quantification (LOQs) were Pb 0.3 ${\mu}g/kg$, Cd 0.15 ${\mu}g/kg$, and As 0.45 ${\mu}g/kg$ for milk and Pb 0.61 ${\mu}g/kg$, Cd 0.31 ${\mu}g/kg$, and As 0.91 ${\mu}g/kg$ for vegetable oil and margarine. The recoveries were 92.6-98.0% for Pb, 91.2-98.9% for Cd, and 97.9-104.7% for As. The average levels of Pb were 2.395 ${\mu}g/kg$ for milk, and 7.656 ${\mu}g/kg$ for vegetable oil. The average levels of Cd were 0.483 ${\mu}g/kg$ for milk, and 0.380 ${\mu}g/kg$ for vegetable oil, and levels of As were 0.781 ${\mu}g/kg$ for milk, and 1.241 ${\mu}g/kg$ for vegetable oil. The results of this study showed that Pb, Cd, and As contents in the whole samples were less than the maximum residual levels in the processed foods that were specified by the Codex standard.

• Journal of Korean Society of Environmental Engineers
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• v.31 no.1
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• pp.42-50
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• 2009

Samples of subway dust were collected by the air filter system of 30 subway stations on Daegu subway line 1 in January 2008. Samples were sieved below 100 ${\mu}m$, and 14 elements were analyzed using ICP after acid extraction. Results obtained from the source assessment of trace elements using enrichment factor showed that Ca, Fe, K, Mg, Mn, Na, V were influenced by natural sources such as weathered rock and resuspended soil, while Cd, Cr, Cu, Ni, Pb and Zn were influenced by anthropogenic sources such as fuel combustion and waste incineration. Concentrations were remarkably higher in components from natural sources than in components from anthropogenic sources. Anthropogenic sources were significantly affected by indoor dusts than outdoor dusts. Results of pollution indices of heavy metals indicated that indoor dusts were more contaminated with heavy metal ions than outdoor dusts. The correlation analysis among trace elements indicated that components were much correlated in the order of natural sources-anthropogenic sources, anthropogenic sources-anthropogenic sources, natural sources-natural sources in both indoor and outdoor dusts. Trace element components of outdoor dusts were largely correlated than those of indoor dusts. In addition, indoor dusts were significantly affected by outdoor dusts rather than depth from the surface or the average daily number of subway passengers.

• Economic and Environmental Geology
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• v.49 no.1
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• pp.13-22
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• 2016

The objectives of this study were to recover silica and iron oxides and $CO_2$ sequestration using serpentine via various acid dissolution and pH swing processes. Serpentine collected from Guhang-myeon in S. Korea were mainly composed of antigorite and magnetite consisting of $SiO_2$ (45.3 wt.%), MgO (41.3 wt.%), $Fe_2O_3$ (12.2 wt.%). Serpentine pulverized ($${\leq_-}75{\mu}m$$) and then dissolved in 3 different acids, HCl, $H_2SO_4$, $HNO_3$. Residues treated with acidic solution were recovered from the solution (step 1). And then the residual solution containing dissolved serpentine was titrated using $NH_4OH$. And pH of the solution increased up to pH=8.6 to obtain reddish precipitates (step 2). After recovery of the precipitates, the residual solution reacted with $CO_2$ and then pH increased up to pH=9.5 to precipitate white materials (step 3). The mineralogical characteristics of the original sample and harvested precipitates were examined by XRD, and TEM-EDS analyses. ICP-AES analysis was also used to investigate solution chemistry. The dissolved ions were Mg, Si, and Fe. The antigorite became noncrystralline silica after acid treatment (step 1). The precipitate at pH=8.6 was mainly amorphous iron oxide, of which size ranged from 2 to 10 nm and mainly consisting of Fe, O, and Si (step 2). At pH=9.5, nesquehonite [$Mg(HCO_3)(OH){\cdot}2(H_2O)$] and lasfordite [$MgCO_3{\cdot}H_2O$] were formed after reaction with $CO_2$ (step 3). The size of carbonated minerals was ranged from 1 to $6{\mu}m$. These results indicated that the acid treatment of serpentine and pH swing processes for the serpentine can be used for synthesis of other materials such as silica, iron oxides and magnesium carbonate. Also, This process may be useful for the precursor synthesis and $CO_2$ sequestration via mineral carbonation.

• Analytical Science and Technology
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• v.29 no.4
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• pp.170-178
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• 2016

Accuracy and precision of ID methods for different spike isotopes of ⁷⁶Se, ⁷⁷Se, and ⁷⁸Se were compared for the analysis of Selenium using quadrupole ICP/MS equipped with Octopole reaction cell. From the analysis of Se inorganic standard solution, all of three spikes showed less than 1 % error and 1 % RSD for both short-term (a day) and long-term (several months) periods. They showed similar results with each other and ⁷⁸Se showed was a bit better than ⁷⁶Se and ⁷⁷Se. However, different spikes showed different results when NIST SRM 1568a and SRM 2967 were analyzed because of the several interferences on the m/z measured and calculated. Interferences due to the generation of SeH from ORC was considered as well as As and Br in matrix. The results showed similar accuracy and precisions against SRM 1568a, which has a simple background matrix, for all three spikes and the recovery rate was about 80% with steadiness. The %RSD was a bit higher than inorganic standard (1.8 %, 8.6 %, and 6.3 % for ⁷⁸Se, ⁷⁶Se and ⁷⁷Se, respectively) but low enough to conclude that this experiment is reliable. However, mussel tissue has a complex matrix showed inaccurate results in case of ⁷⁸Se isotope spike (over 100 % RSD). ⁷⁶Se and ⁷⁷Se showd relatively good results of around 98.6 % and 104.2 % recovery rate. The errors were less than 5 % but the precision was a bit higher value of 15 % RSD. This clearly shows that Br interferences are so large that a simple mathematical calibration is not enough for a complex-matrixed sample. In conclusion, all three spikes show similar results when matrix is simple. However, ⁷⁸Se should be avoided when large amount of Br exists in matrix. Either ⁷⁶Se or ⁷⁷Se would provide accurate results.

• Journal of the Korean Wood Science and Technology
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• v.35 no.1
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• pp.73-80
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• 2007

This study was carried out to separate the heavy toxic metals in eco-building materials by low-temperature pyrolysis, especially arsenic (As) compounds in CCA wood preservative as a solid in char. The pyrolysis was carried out to heat the CCA-treated Hemlock at $280^{\circ}C$, $300^{\circ}C$, $320^{\circ}C$, and $340^{\circ}C$ for 60 mins. Laboratory scale pyrolyzer composed of [preheater$\rightarrow$pyrolyzer$\rightarrow$1st water scrubber$\rightarrow$2nd bubbling flask with 1% $HNO_3$ solution$\rightarrow$vent], and was operated to absorb the volatile metal compound particulates at the primary water scrubber and the secondary nitric acid bubbling flask with cooling condenser of $4^{\circ}C$ under nitrogen stream of 20 mL/min flow rate. And the contents of copper, chromium and arsenic compounds in its pyrolysis such as carbonized CCA treated wood, 1st washing and 2nd washing liquors as well as its raw materials, were determined using ICP-AES. The results are as follows : 1. The yield of char in low-temperature pyrolysis reached about 50 percentage similar to the result of common pyrolytic process. 2. The higher the pyrolytic temperature was, the more the volatiles of CCA, and in particular, the arsenic compounds were to be further more volatile above $320^{\circ}C$, even though the more repetitive and sequential monitorings were necessary. 3. More than 85 percentage of CCA in CCA-treated wood was left in char in such low-temperature pyrolytic condition at $300^{\circ}C$. 4. Washing system for absorption of volatile CCA in this experiment required much more contacting time between volatile gases and water to prevent the loss of CCA compounds, especially the loss of arsenic compound. 5. Therefore, more complete recovery of CCA components in CCA-treated wood required the lower temperature than $320^{\circ}C$, and the longer contacting time of volatile gases and water needed the special washing and recovery system to separate the toxic and volatile arsenic compounds in vent gases.

• Journal of the Mineralogical Society of Korea
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• v.20 no.4
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• pp.357-366
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• 2007

Microorganisms participate in a variety of geochemical processes such as weathering and formation of minerals, leaching of precious metals from minerals, and cycling of organic matter The objective of this study was to investigate biogeochemical processes of iron leaching from magnetite ore by iron-reducing bacteria isolated from intertidal flat sediments, southwestern part of Korea. Microbial iron leaching experiments were performed using magnetite ore, Shinyemi magnetite ore, in well-defined media with and without bacteria at room temperature for a month. Water soluble Fe and Mn during the leaching experiments were determined by ICP analysis of bioleached samples, and the resulting precipitated solids were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The extent of iron leaching from magnetite in the aerobic conditions (Fe = 15 mg/L and Mn = 3.41 mg/L) was lower than that in the anaerobic environments (Fe = 32.8 mg/L and Mn = 5.23 mg/L). The medium pH typically decreased from 8.3 to 7.2 during a month incubation. The Eh of the initial medium decreased from +144.9 mV to -331.7 mV in aerobic environments and from -2.3 mV to -494.6 mV in anaerobic environments upon incubation with the metal reducing microorganisms. The decrease in pH is due to glucose fermentation producing organic acids and $CO_2$. The ability of bacteria to leach soluble iron from crystalline magnetite could have significant implications for biogeochemical processes in sediments where Fe(III) in magnetite represents the largest pool of electron acceptor as well as to use as a novel biotechnology for leaching precious and heavy metals from raw materials.