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Analytical Method for Dioxin and Organo-Chlorinated Compounds: (Ⅱ) Comparison and Extraction Methods of Dioxins from XAD-2 Adsorbent

  • 양정수;이성광;박영훈;이대운
    • Bulletin of the Korean Chemical Society
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    • v.20 no.6
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    • pp.689-695
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    • 1999
  • Supercritical fluid extraction (SFE), ultrasonic extraction (USE), and accelerated solvent extraction (ASE) were compared with the well known Soxhlet extraction for the extraction of polychlorinated biphenyls (PCBs) and polychlorinated dibenzo-p-dioxins(PCDDs) from the XAD-2 resin which was used to adsorb PCDDs in the atmosphere. XAD-2 resin spiked with five PCDDs was chosen as a sample. The optimum conditions for the extraction of PCDDs by SFE were turned out to be the use of CO2 modified with 10% toluene at 100 ℃ and 350 atm, with 5 min static extraction followed by 20 min dynamic extraction. SFE gave a good extraction rate with good reproducibility for PCDDs ranging from 68 to 98%. The ultrasonic extraction of PCDDs from XAD-2 was investigated and compared with other extractions. A probe type method was compared with a bath type. Two extraction solvents, toluene and acetone were compared with their mixture. The use of their mixture in probe type, with 9 minutes of extraction time, was found to be the optimum condition. The average recovery of the five PCDDs for USE was 82-93%. Accelerated solvent extraction (ASE) with a liquid solvent, a new technique for sample preparation, was performed under elevated temperatures and pressures. The effect of tem-perature on the efficiency of ASE was investigated. The extraction time for a 10 g sample was less than 15 min, when the organic solvent was n-hexaneacetone mixture (1 : 1, v/v). Using ASE, the average recoveries of five PCDDs ranged from 90 to 103%. SFE, USE, and ASE were faster and less laborious than Soxhlet extraction. The former three methods required less solvent than Soxhlet extraction. SFE required no concentration of the solvent extracts. SFE and ASE failed to perform simultaneous parallel extractions because of instrumental limitations.

Effect of additives on the hydrothermal synthesis of manganese ferrite nanoparticles

  • Kurtinaitiene, Marija;Mazeika, Kestutis;Ramanavicius, Simonas;Pakstas, Vidas;Jagminas, Arunas
    • Advances in nano research
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    • v.4 no.1
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    • pp.1-14
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    • 2016
  • Superparamagnetic iron oxide nanoparticles (Nps), composed of magnetite, $Fe_3O_4$, or maghemite, ${\gamma}-Fe_2O_3$, core and biocompatible polymer shell, such as dextran or chitozan, have recently found wide applications in magnetic resonance imaging, contrast enhancement and hyperthermia therapy. For different diagnostic and therapeutic applications, current attempt is focusing on the synthesis and biomedical applications of various ferrite Nps, such as $CoFe_2O_4$ and $MnFe_2O_4$, differing from iron oxide Nps in charge, surface chemistry and magnetic properties. This study is focused on the synthesis of manganese ferrite, $MnFe_2O_4$, Nps by most commonly used chemical way pursuing better control of their size, purity and magnetic properties. Co-precipitation syntheses were performed using aqueous alkaline solutions of Mn(II) and Fe(III) salts and NaOH within a wide pH range using various hydrothermal treatment regimes. Different additives, such as citric acid, cysteine, glicine, polyetylene glycol, triethanolamine, chitosan, etc., were tested on purpose to obtain good yield of pure phase and monodispersed Nps with average size of ${\leq}20nm$. Transmission electron microscopy (TEM), X-ray diffraction, energy dispersive X-ray spectroscopy (EDX), $M\ddot{o}ssbauer$ spectroscopy down to cryogenic temperatures, magnetic measurements and inductively coupled plasma mass spectrometry were employed in this study.

Preparation and Evaluation of Microcapsule/Emulsions via the Electroatatic Interations of Polysaccharide and Protein (식물 유래 다당류/단백질 기반 마이크로캡슐/에멀젼 제조 및 평가)

  • Choi, Yu Ri;Lim, Hyung Jun;Lee, John Hwan;Oh, Seong Geun
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.41 no.4
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    • pp.295-302
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    • 2015
  • A novel microcapsule/emulsions for cosmetics was studied. Our present studies demonstrate that the biopolymer-stabilized microemulsion composed of polysaccharide and protein can encapsulate and stabilize remarkably coenzyme-Q10 (Q10). Polysaccharide and protein complex were incorporated in the microcapsule in order to reinforce the physical strength of the microspheres. We compared the long-term stability of the activity of Q10 in biopolymer-stabilized microemulsion. There was no noticeable negative effect on the activity of Q10. Optical microscope (OM) and transmission electron microscope (TEM) showed that microcapsules were spherical and had a smooth surface. Consequently, the polysaccharide/protein emulsion produced in this study may be beneficial in improving the emulsion stability and the protection capability of labile substances.

Green Synthesis of Multifunctional Carbon Nanodots and Their Applications as a Smart Nanothermometer and Cr(VI) Ions Sensor

  • Li, Lu;Shao, Congying;Wu, Qian;Wang, Yunjian;Liu, Mingzhu
    • Nano
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    • v.13 no.12
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    • pp.1850147.1-1850147.14
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    • 2018
  • In this work, water-soluble and blue-emitting carbon nanodots (CDs) were synthesized from apple peels for the first time via one-step hydrothermal method. The synthetic route is facile, green, economical and viable. The as-prepared CDs were characterized thoroughly by transmission electron microscopy (TEM), X-ray diffraction (XRD), Raman, Fourier transform infrared (FT-IR), X-ray photoelectron (XPS), fluorescence and UV-Vis absorption spectroscopy in terms of their morphology, surface functional groups and optical properties. The results show that these CDs possessed ultrasmall size, good dispersivity, and high tolerance to pH, ionic strength and continuous UV irradiation. Significantly, the CDs had fast and reversible response towards temperature, and the accurate linear relationship between fluorescence intensity and temperature was used to design a novel nanothermometer in a broad temperature range from 5 to $65^{\circ}C$ facilely. In addition, the fluorescence intensity of CDs was observed to be quenched immediately by Cr(VI) ions based on the inner filter effect. A low-cost Cr(VI) ions sensor was proposed employing CDs as fluorescent probe, and it displayed a wide linear range from 0.5 to $200{\mu}M$ with a detection limit of $0.73{\mu}M$. The practicability of the developed Cr(VI) sensor for real water sample assay was also validated with satisfactory recoveries.

Fabrication and Characterization of Spherical Carbon-Coated Li3V2(PO4)3 Cathode Material by Hydrothermal Method with Reducing Agent

  • Moon, Jung-In;Song, Jeong-Hwan
    • Korean Journal of Materials Research
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    • v.29 no.9
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    • pp.519-524
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    • 2019
  • Spherical $Li_3V_2(PO_4)_3$ (LVP) and carbon-coated LVP with a monoclinic phase for the cathode materials are synthesized by a hydrothermal method using $N_2H_4$ as the reducing agent and saccharose as the carbon source. The results show that single phase monoclinic LVP without impurity phases such as $LiV(P_2O_7)$, $Li(VO)(PO_4)$ and $Li_3(PO_4)$ can be obtained after calcination at $800^{\circ}C$ for 4 h. SEM and TEM images show that the particle sizes are $0.5{\sim}2{\mu}m$ and the thickness of the amorphous carbon layer is approximately 3~4 nm. CV curves for the test cell are recorded in the potential ranges of 3.0~4.3 V and 3.0~4.8 V at a scan rate of $0.01mV\;s^{-1}$ and at room temperature. At potentials between 3.0 and 4.8 V, the third $Li^+$ ions from the carbon-coated LVP can be completely extracted, at voltages close to 4.51 V. The carbon-coated LVP exhibits an initial specific discharge capacity of $118mAh\;g^{-1}$ in the voltage region of 3.0 to 4.3 V at a current rate of 0.2 C. The results indicate that the reducing agent and carbon source can affect the crystal structure and electrochemical properties of the cathode materials.

Study on Optical Characteristics of Nano Hollow Silica with TiO2 Shell Formation

  • Roh, Gi-Yeon;Sung, Hyeong-Seok;Lee, Yeong-Cheol;Lee, Seong-Eui
    • Journal of the Korean Ceramic Society
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    • v.56 no.1
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    • pp.98-103
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    • 2019
  • Optical filters to control light wavelength of displays or cameras are fabricated by multi-layer stacking process of low and high index thin films. The process of multi-layer stacking of thin films has received much attention as an optimal process for effective manufacturing in the optical filter industry. However, multi-layer processing has disadvantages of complicated thin film process, and difficulty of precise control of film morphology and material selection, all of which are critical for transmittance and coloring effect on filters. In this study, the composite $TiO_2$, which can be used to control of UV absorption, coated on nano hollow silica sol, was synthesized as a coating material for optical filters. Furthermore, systematic analysis of the process parameters during the chemical reaction, and of the structural properties of the coating solutions was performed using SEM, TEM, XRD and photo spectrometry. From the structural analysis, we found that the 85 nm nano hollow silica with 2.5 nm $TiO_2$ shell formation was successfully synthesized at proper pH control and titanium butoxide content. Photo luminescence characteristics, excited by UV irradiation, show that stable absorption of 350 nm-light, correlated with a 3.54 eV band gap, existed for the $TiO_2$ shell-nano hollow silica reacted with 8.8 mole titanium butoxide solution. Transmittance observed on substrate of the $TiO_2$ shell-nano hollow silica showed effective absorption of 200-300 nm UV light without deterioration of visible light transparency.

The Reduction Properties of Nitrate in Water with Palladium and Indium on Aluminum Pillared Montmorillonite Catalyst (팔라디움과 인디움을 담지한 Al 층간가교 몬모릴로나이트 촉매의 수중 질산성질소 환원 특성)

  • Jeong, Sangjo
    • Journal of Korean Society on Water Environment
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    • v.34 no.6
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    • pp.621-631
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    • 2018
  • In this study, catalyst was made through incipient wetness method using palladium (Pd) as noble metal, indium (In) as secondary metal, and montmorillonite (MK10) and Al pillared montmorillonite (Al-MK10) as supporters. The nitrate reduction rate of the catalysts was measured by batch experiments where H2 gas was used as reducing agent and formic acid as pH controller. Transmission electron microscopy (TEM) equipped with energy dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were all used to determine the elemental distribution of Pd, In, Al, and Si on catalysts. It was observed that Al pillaring increased the Al/Si elemental composition ratio and point of zero charge of MK10, but decreased its BET specific surface area and pore volume. The nitrate reduction rate of Al-MK10 Pd/In was 2.0 ~ 2.5 times higher than that of MK10 Pd/In using artificial groundwater (GW) in ambient temperature and pressure. Nitrate reduction rates in GW were 1.2 ~ 1.7 times lower than those in distilled deionized water (DDW). Nitrate reduction rates in acidic conditions were higher than those in neutral condition in both GW and DDW. The amount of produced NH3-N over degraded NO3- at acid conditions was lower than that of neutral condition. Even though the leaching of Pd after reaction was measured in DDW it was not detected when both Al-MK10 Pd/In and MK10 Pd/In were used in GW. The modification of montmorillonite as a supporter significantly increased the reductive catalytic activities of nitrates. However, the ratio of producing ammonia by-products to degraded nitrates in ambient temperature and pressure was similar.

Ni Nanoparticle-Graphene Oxide Composites for Speedy and Efficient Removal of Cr(VI) from Wastewater

  • Wang, Wan-Xia;Zhao, Dong-Lin;Wu, Chang-Nian;Chen, Yan;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.31 no.6
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    • pp.345-352
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    • 2021
  • In this study, Ni nanoparticle supported by graphene oxide (GO) (Ni-GO) is successfully synthesized through hydrothermal synthesis and calcination, and Cr(VI) is extracted from aqueous solution. The morphology and structure of Ni-GO composites are characterized by scanning electron microscopy (SEM), trans mission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). High-resolution transmission electron microscopy (HRTEM) and XRD confirms the high dispersion of Ni nanoparticle after support by GO. Loading Ni on GO can obviously enhance the stability of Ni-GO composites. It can be calculated from TGA that the mass percentage of Ni is about 60.67 %. The effects of initial pH and reaction time on Cr(VI) removal ability of Ni-GO are investigated. The results indicate that the removal efficiency of Cr(VI) is greater than that of bared GO. Ni-GO shows fast removal capacity for Cr(VI) (<25 min) with high removal efficiency. Dynamic experiments show that the removal process conforms to the quasi-second order model of adsorption, which indicates that the rate control step of the removal process is chemical adsorption. The removal capacity increases with the increase of temperature, indicating that the reaction of Cr(VI) on Ni-GO composites is endothermic and spontaneous. Combined with tests and characterization, the mechanism of Cr(VI) removal by rapidly adsorption on the surface of Ni-GO and reduction by Ni nanoparticle is investigated. The above results show that Ni-GO can be used as a potential remediation agent for Cr(VI)-contaminated groundwater.

Ag2Se Modified TiO2 Heterojunction with Enhanced Visible-Light Photocatalytic Performance

  • Zhu, Lei;Tang, Jia-Yao;Fan, Jia-Yi;Sun, Chen;Oh, Won-Chun
    • Korean Journal of Materials Research
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    • v.31 no.12
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    • pp.657-664
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    • 2021
  • To build a highly active photocatalytic system with high efficiency and low cast of TiO2, we report a facile hydrothermal technique to synthesize Ag2Se-nanoparticle-modified TiO2 composites. The physical characteristics of these samples are analyzed by X-ray diffraction, scanning electron microscopy with energy dispersive X-ray analysis, transmission electron microscopy and BET analysis. The XRD and TEM results show us that TiO2 is coupled with small sized Ag2Se nanoplate, which has an average grain size of about 30 nm in diameter. The agglomeration of Ag2Se nanoparticles is improved by the hydrothermal process, with dispersion improvement of the Ag2Se@TiO2 nanocomposite. Texbrite BA-L is selected as a simulated dye to study the photodegradation behavior of as-prepared samples under visible light radiation. A significant enhancement of about two times the photodegradation rate is observed for the Ag2Se@TiO2 nanocomposite compared with the control sample P25 and as-prepared TiO2. Long-term stability of Ag2Se@TiO2 is observed via ten iterations of recycling experiments under visible light irradiation.

Analysis of the characteristics of the environment and fish community in the Gwanggyo Lake Park area using the environmental DNA technique (환경 DNA 기법을 활용한 광교호수공원 일대의 시기 및 수환경 특성별 어류상 분석)

  • Won, Su-Yeon;Kang, Yu-Jin;Song, Young-Keun
    • Journal of the Korean Society of Environmental Restoration Technology
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    • v.25 no.5
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    • pp.77-88
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    • 2022
  • This study aims to understand the relationship between the distribution of fish species in the two water ecosystems and the habitat factors according to the survey period targeting Gwanggyo Lake Park in the city. There are studies on the appearance and distribution of species by applying eDNA to freshwater ecosystems. However, in the domestic, streams are the target, and studies on the relationship between species distribution and habitat environment in two water environments are lacking. We conducted to analyze the species list and relationship with habitat factors using eDNA research in May and October at 21 points in Gwanggyo Lake Park, Suwon City, which were connected to lakes and streams. As a result, there was no species difference in the water environment according to the survey period. However, the total number of reads during the spawning season(May) was 3,126,482, which was more than double that after the spawning season(October). Tolerant species appeared in Woncheon Lake with a slow or stagnant flow, but there was no significant correlation between species and habitat factors depending on the survey period. On the other hand, intermediate and sensitive species appeared in the Woncheon stream with high flow. There was a significant correlation between the low temperature during the spawning season and the high dissolved oxygen content after the spawning season(P<0.001, Tem.: 20.7±2.6℃, DO: 8.6±1.7). It is expected that environmental DNA will be used to survey species and suggest monitoring methods according to the survey period.